CN108751956B - Method for preparing alumina-based amorphous and solid solution ceramic micron powder mixture by aluminum oxide combustion synthesis quenching method - Google Patents
Method for preparing alumina-based amorphous and solid solution ceramic micron powder mixture by aluminum oxide combustion synthesis quenching method Download PDFInfo
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- CN108751956B CN108751956B CN201810751719.7A CN201810751719A CN108751956B CN 108751956 B CN108751956 B CN 108751956B CN 201810751719 A CN201810751719 A CN 201810751719A CN 108751956 B CN108751956 B CN 108751956B
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- 238000000034 method Methods 0.000 title claims abstract description 151
- 239000006104 solid solution Substances 0.000 title claims abstract description 107
- 239000000919 ceramic Substances 0.000 title claims abstract description 91
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 90
- 239000000203 mixture Substances 0.000 title claims abstract description 80
- 239000000843 powder Substances 0.000 title claims abstract description 75
- 238000005049 combustion synthesis Methods 0.000 title claims abstract description 52
- 238000010791 quenching Methods 0.000 title claims abstract description 49
- 230000000171 quenching effect Effects 0.000 title claims abstract description 49
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 title claims description 48
- 229910052751 metal Inorganic materials 0.000 claims abstract description 111
- 239000002184 metal Substances 0.000 claims abstract description 111
- 238000001816 cooling Methods 0.000 claims abstract description 91
- 239000011812 mixed powder Substances 0.000 claims abstract description 82
- 239000002131 composite material Substances 0.000 claims abstract description 77
- 238000006243 chemical reaction Methods 0.000 claims abstract description 29
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 24
- CQBLUJRVOKGWCF-UHFFFAOYSA-N [O].[AlH3] Chemical compound [O].[AlH3] CQBLUJRVOKGWCF-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 168
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 102
- 238000002156 mixing Methods 0.000 claims description 43
- 239000007789 gas Substances 0.000 claims description 29
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 28
- 230000001590 oxidative effect Effects 0.000 claims description 24
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000003085 diluting agent Substances 0.000 claims description 18
- 239000000395 magnesium oxide Substances 0.000 claims description 17
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 11
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 10
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 claims description 10
- 239000000292 calcium oxide Substances 0.000 claims description 10
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(iii) oxide Chemical compound O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 claims description 10
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 10
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 claims description 10
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Chemical compound [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 claims description 10
- ZIKATJAYWZUJPY-UHFFFAOYSA-N thulium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Tm+3].[Tm+3] ZIKATJAYWZUJPY-UHFFFAOYSA-N 0.000 claims description 10
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 8
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 7
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 6
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 6
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 6
- HYXGAEYDKFCVMU-UHFFFAOYSA-N scandium oxide Chemical compound O=[Sc]O[Sc]=O HYXGAEYDKFCVMU-UHFFFAOYSA-N 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 5
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 claims description 5
- 229910000423 chromium oxide Inorganic materials 0.000 claims description 5
- 229910000428 cobalt oxide Inorganic materials 0.000 claims description 5
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims description 5
- 229910003440 dysprosium oxide Inorganic materials 0.000 claims description 5
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(iii) oxide Chemical compound O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 claims description 5
- 229910001940 europium oxide Inorganic materials 0.000 claims description 5
- 229940075616 europium oxide Drugs 0.000 claims description 5
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 claims description 5
- 229910001938 gadolinium oxide Inorganic materials 0.000 claims description 5
- 229940075613 gadolinium oxide Drugs 0.000 claims description 5
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 claims description 5
- 229910000449 hafnium oxide Inorganic materials 0.000 claims description 5
- WIHZLLGSGQNAGK-UHFFFAOYSA-N hafnium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Hf+4] WIHZLLGSGQNAGK-UHFFFAOYSA-N 0.000 claims description 5
- JYTUFVYWTIKZGR-UHFFFAOYSA-N holmium oxide Inorganic materials [O][Ho]O[Ho][O] JYTUFVYWTIKZGR-UHFFFAOYSA-N 0.000 claims description 5
- OWCYYNSBGXMRQN-UHFFFAOYSA-N holmium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ho+3].[Ho+3] OWCYYNSBGXMRQN-UHFFFAOYSA-N 0.000 claims description 5
- 229910003443 lutetium oxide Inorganic materials 0.000 claims description 5
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 5
- 229910000476 molybdenum oxide Inorganic materials 0.000 claims description 5
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 5
- 229910000484 niobium oxide Inorganic materials 0.000 claims description 5
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims description 5
- MPARYNQUYZOBJM-UHFFFAOYSA-N oxo(oxolutetiooxy)lutetium Chemical compound O=[Lu]O[Lu]=O MPARYNQUYZOBJM-UHFFFAOYSA-N 0.000 claims description 5
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 claims description 5
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 5
- MMKQUGHLEMYQSG-UHFFFAOYSA-N oxygen(2-);praseodymium(3+) Chemical compound [O-2].[O-2].[O-2].[Pr+3].[Pr+3] MMKQUGHLEMYQSG-UHFFFAOYSA-N 0.000 claims description 5
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 claims description 5
- UZLYXNNZYFBAQO-UHFFFAOYSA-N oxygen(2-);ytterbium(3+) Chemical compound [O-2].[O-2].[O-2].[Yb+3].[Yb+3] UZLYXNNZYFBAQO-UHFFFAOYSA-N 0.000 claims description 5
- 229910003447 praseodymium oxide Inorganic materials 0.000 claims description 5
- 229910001954 samarium oxide Inorganic materials 0.000 claims description 5
- 229940075630 samarium oxide Drugs 0.000 claims description 5
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 claims description 5
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 5
- 229910001936 tantalum oxide Inorganic materials 0.000 claims description 5
- 229910003451 terbium oxide Inorganic materials 0.000 claims description 5
- SCRZPWWVSXWCMC-UHFFFAOYSA-N terbium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Tb+3].[Tb+3] SCRZPWWVSXWCMC-UHFFFAOYSA-N 0.000 claims description 5
- 229910001935 vanadium oxide Inorganic materials 0.000 claims description 5
- 229910003454 ytterbium oxide Inorganic materials 0.000 claims description 5
- 229940075624 ytterbium oxide Drugs 0.000 claims description 5
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 238000001125 extrusion Methods 0.000 claims description 2
- 229910010413 TiO 2 Inorganic materials 0.000 claims 1
- 239000007921 spray Substances 0.000 claims 1
- 229910052727 yttrium Inorganic materials 0.000 claims 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims 1
- 238000000498 ball milling Methods 0.000 abstract description 58
- 238000002360 preparation method Methods 0.000 abstract description 19
- 230000008569 process Effects 0.000 abstract description 12
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000004321 preservation Methods 0.000 abstract description 2
- 230000000977 initiatory effect Effects 0.000 abstract 1
- 229910052760 oxygen Inorganic materials 0.000 abstract 1
- 239000001301 oxygen Substances 0.000 abstract 1
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 238000005507 spraying Methods 0.000 description 85
- 229910052593 corundum Inorganic materials 0.000 description 80
- 229910001845 yogo sapphire Inorganic materials 0.000 description 80
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 44
- 238000001035 drying Methods 0.000 description 42
- 239000000463 material Substances 0.000 description 42
- 238000007873 sieving Methods 0.000 description 36
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 25
- 229910052802 copper Inorganic materials 0.000 description 25
- 239000010949 copper Substances 0.000 description 25
- 229910000831 Steel Inorganic materials 0.000 description 22
- 229910052742 iron Inorganic materials 0.000 description 22
- 239000010959 steel Substances 0.000 description 22
- 238000004140 cleaning Methods 0.000 description 18
- 238000007711 solidification Methods 0.000 description 18
- 238000001291 vacuum drying Methods 0.000 description 18
- 238000007789 sealing Methods 0.000 description 15
- 230000001276 controlling effect Effects 0.000 description 14
- 230000036316 preload Effects 0.000 description 14
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 13
- 239000000155 melt Substances 0.000 description 13
- 238000003825 pressing Methods 0.000 description 11
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 9
- 230000008023 solidification Effects 0.000 description 8
- 239000003381 stabilizer Substances 0.000 description 7
- 238000002485 combustion reaction Methods 0.000 description 6
- CJNBYAVZURUTKZ-UHFFFAOYSA-N hafnium(IV) oxide Inorganic materials O=[Hf]=O CJNBYAVZURUTKZ-UHFFFAOYSA-N 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 239000005300 metallic glass Substances 0.000 description 5
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 5
- 238000005245 sintering Methods 0.000 description 5
- 239000004567 concrete Substances 0.000 description 4
- 238000000280 densification Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
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- 238000003780 insertion Methods 0.000 description 4
- 230000037431 insertion Effects 0.000 description 4
- 239000002114 nanocomposite Substances 0.000 description 4
- 238000007712 rapid solidification Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000010891 electric arc Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000009776 industrial production Methods 0.000 description 3
- 238000013001 point bending Methods 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000001241 arc-discharge method Methods 0.000 description 2
- 238000000889 atomisation Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 230000003628 erosive effect Effects 0.000 description 2
- 230000005496 eutectics Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910001338 liquidmetal Inorganic materials 0.000 description 2
- 238000005551 mechanical alloying Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 239000011226 reinforced ceramic Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910018516 Al—O Inorganic materials 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910009474 Y2O3—ZrO2 Inorganic materials 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910000808 amorphous metal alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000007578 melt-quenching technique Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910001960 metal nitrate Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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Abstract
一种铝氧燃烧合成急冷法制备氧化铝基非晶和固溶体陶瓷微米粉混合物的方法，本发明涉及一种复合陶瓷粉体的制备方法领域，具体涉及一种铝氧燃烧合成高温熔体结合旋转金属盘或轧辊设备急冷的方法。本发明要解决现有制备方法存在成本高、效率低、时间长、产量低，只能小批量生产的技术问题。方法：一、制备混合粉体；二、引发合成反应，保温，在旋转金属盘或轧辊设备的对辊中冷却，然后粉碎，球磨。本方法的工艺过程简单，反应迅速，制备周期短，产量大，纯度高，可控制，是一种低成本、高效率、高性能的亚稳态微米粉的制备工艺方法。本发明用于制备Al2O3基非晶和固溶体陶瓷微米粉混合物。
A method for preparing a mixture of alumina-based amorphous and solid solution ceramic micro-powders by an aluminum-oxygen combustion synthesis and rapid cooling method. The invention relates to the field of preparation methods for composite ceramic powders, and in particular relates to an alumina-oxygen combustion synthesis of high-temperature melt combined with rotating A method of quenching metal disk or roll equipment. The invention aims to solve the technical problems of high cost, low efficiency, long time and low output in the existing preparation method, and can only be produced in small batches. Methods: 1. Preparation of mixed powder; 2. Initiating synthesis reaction, heat preservation, cooling in rotating metal disc or counter roll of roller equipment, then pulverizing and ball milling. The method has the advantages of simple technological process, rapid reaction, short preparation period, large output, high purity and controllability, and is a low-cost, high-efficiency and high-performance preparation technology for metastable micron powder. The present invention is used for preparing Al 2 O 3 -based amorphous and solid solution ceramic micro-powder mixtures.
Description
Technical Field
The invention relates to the field of a preparation method of composite ceramic powder, in particular to a method for rapidly cooling a high-temperature melt synthesized by aluminum oxide combustion in combination with a rotating metal disc or a roller device.
Background
Combustion synthesis (synthesis), also known as self-propagating high temperature synthesis (SHS). The method does not need an external heat source, and is a technology for synthesizing the inorganic refractory material by means of heat generated during the reaction of the raw materials. The method has the advantages that: low cost, low energy consumption, high reaction temperature and high production efficiency.
In the field of amorphous material preparation, the main research focuses on the preparation of metal amorphous, and the industrial production is realized; the introduction of the preparation of the ceramic amorphous is less, the preparation of the high-temperature resistant ceramic amorphous is basically not available, and the existing preparation method of the ceramic amorphous has the advantages of low ceramic conversion rate, high cost and unsuitability for industrial production.
The common preparation methods of the amorphous materials (amorphous metal and amorphous ceramic) mainly comprise the following steps: melt quenching, chemical reduction, mechanical alloying, sol-gel, precursor pyrolysis, and arc discharge. Among them, the quenching method is the earliest method for producing an amorphous alloy, and its principle is to try to increase the specific surface area of an alloy sample and to reduce the interfacial thermal resistance of a melt and a cooling medium in order to achieve a high cooling rate. Atomization and single roll are the two most commonly used methods. The atomization method is mainly used for preparing amorphous state and crystalline state powder. The principle is that the metal liquid flow is impacted by high-speed gas flow to be dispersed into tiny liquid drops, so that the rapid solidification is realized. The method has simple equipment, convenient operation and easy industrialized production. The single-roll method is to use a fast-rotating copper roll to quickly solidify the liquid metal sprayed on the copper roll and then throw the liquid metal off the surface of the copper roll to form amorphous and microcrystalline strips with the thickness of several to dozens of microns. This process can yield 106The cooling rate of K/s is one of the common methods, and the method is mainly used for preparing amorphous metal.
For the arc discharge method, the method is mainly applied to the preparation of amorphous metal; and for amorphous ceramic preparation, the method is also suitable. The current report of preparing amorphous material by arc discharge is about A12O3-Y2O3-ZrO2And (5) amorphous preparation. A12O3，Y2O3，ZrO2The three raw materials are weighed according to a certain proportion, are made into a rod-shaped material after ball milling and mixing, the top end is melted through arc discharge, small drops are dripped on a roller, and the amorphous plate-shaped material is extruded by the roller. By adopting the method, the melt of the composite ceramic system is obtained, then the non-equilibrium amorphous is obtained by a rapid solidification method, the nanocrystalline precipitation is realized in the material after sintering or heat treatment, and the high-density fine and uniform nano structure can be obtained. However, the current research mainly focuses on mechanism research, and practical technologies suitable for large-scale production are still lacking.
In summary, in the commonly used preparation methods of amorphous metal materials, the chemical reduction method cannot be used to prepare amorphous ceramics; the powder produced by the mechanical alloying method has poor sphericity, is easy to mix with impurities in the crushing process and has low efficiency. The common preparation method of the amorphous ceramic material has long time required by the sol-gel method, has a large number of micropores, can escape a plurality of gases and organic matters in the drying process and generates shrinkage; a large amount of pores and cracks are generated in the cracking process of the polymer in the precursor pyrolysis method, the integrity of the material is damaged, and the performance of the material is finally influenced; the arc discharge method does not achieve large-scale production.
Disclosure of Invention
The invention aims to solve the technical problems of high cost, low purity, low efficiency, long time and low yield of amorphous metal materials prepared by the existing method and can only be produced in small batches, and provides a quenching method for preparing Al by aluminum oxide combustion synthesis2O3A method for preparing a mixture of amorphous and solid solution ceramic micropowder.
Method for preparing Al by aluminum oxide combustion synthesis quenching method2O3The method for preparing the mixture of the amorphous ceramic micron powder and the solid solution ceramic micron powder comprises the following steps:
drying and uniformly mixing aluminum powder and a diluent to obtain mixed powder;
secondly, the mixed powder obtained in the step one is put into a pressure-resistant reactor with a nozzle at the lower end, oxidizing gas is introduced, the mixed powder is ignited to initiate a synthesis reaction, the temperature is kept, then the nozzle of the pressure-resistant reactor is opened, the composite melt in the pressure-resistant reactor is sprayed into a pair of rollers of a rotating metal disc or a roller device to be cooled, and then the aluminum alloy is crushed and ball-milled to obtain the Al2O3Based on the mixture of amorphous and solid solution ceramic micron powder, the aluminum oxide combustion synthesis quenching method is completed for preparing Al2O3A method for preparing a mixture of amorphous and solid solution ceramic micropowder.
If the composite melt is sprayed into a rotating metal disc, the radius of the rotating metal disc is 50-200 cm, and the rotating speed is 60-150 r/min; spraying Al on one side of rotating metal disc2O3/ZrO2Spraying high-pressure and high-speed water flow to the other side of the composite melt for auxiliary cooling, wherein the water amount is 20-30L/minThe pressure is 0.1-0.5 MPa, and Al is formed on the surface of the rotating metal disc by solidification2O3/ZrO2Amorphous and solid solution films;
if the composite melt is sprayed into a pair roller of a roller device, the double roller device is adopted, the roller pressure is 30-70 MPa, and the roller rotating speed is 100-4000 rpm; spraying Al between the pair of rollers2O3/ZrO2Spraying high-pressure and high-speed water flow on two sides of the composite melt to assist in cooling the double rollers, wherein the water amount is 20-30L/min, the water pressure is 0.1-0.5 MPa, and extruding to form Al2O3/ZrO2Amorphous and solid solution ribbons.
The invention adopts the exothermic combustion reaction of the aluminum oxygen (see chemical equation (1)), does not adopt the exothermic combustion reaction of metal Al and various metal nitrates, and further increases A12O3The purity of the powder removes the influence of residual metal salt and impurity compound. Simultaneously, the exothermic reaction of the combustion of the aluminum oxygen is utilized, the system exothermic reaction is utilized to generate high temperature and high pressure, so that the raw material in a molten state is injected onto a rapidly rotating iron, copper and steel disc (shown in an attached figure 1) or a roller device (shown in an attached figure 2) at a high speed, water cooling is assisted, the cooling speed of the molten body is accelerated, and Al is obtained2O3/ZrO2Amorphous and solid solution mixed films or ribbons. The method belongs to a rapid solidification process far away from an equilibrium state, so that amorphous and high-solid-solubility powder which is difficult to obtain in the equilibrium state can be obtained; when the micron powder is used for preparing eutectic ceramics in the later period, nanocrystalline can be separated out, the effect of nano-composite reinforced ceramics is achieved, and the performance of the ceramics is greatly improved.
In the process of the present invention, Al-O is the most important2The exothermic reaction of combustion (see chemical equation (1)) between them, and instantly generates high temperature and high pressure to melt Al2O3、ZrO2Diluent and high temperature Al2O3/ZrO2And (3) a melt rapid solidification process. The basic principle of combustion synthesis is as follows2Or O2And N2Mixed gas and high reducing Al powder as raw material, ZrO is used2Powder and Al2O3The powder is diluent (or other oxide diluent is added), and phase change stabilizer (yttrium oxide, cerium oxide) is addedOxides of magnesium, calcium oxide, titanium oxide, etc.) to control tetragonal phase ZrO in the product2The content of (a). Wherein N is added2Is aimed at in Al-O2After the preferential reaction, a small amount of ZrN is formed by the reaction with Al powder (see equation (2)), increasing the conductivity and hardness of the ceramic. Meanwhile, other gases are added to reduce the concentration of the oxidizing gas, so that the reaction rate is reduced, and the safety factor of production is improved.
4Al+3O2→2Al2O3 (1)
8Al+3N2+6ZrO2→4Al2O3+6ZrN (2)
The reaction has extremely high theoretical temperature (2100-4000 ℃), and inert alumina and zirconia are added as diluents, so that the stability of combustion synthesis can be improved, and the regulation and control of the ZrO product are facilitated2/Al2O3In different proportions to obtain ZrO of different proportions2/Al2O3Compounding micron powder. The temperature and the speed of the melt during spraying are influenced by the pressure and the temperature in the combustion reaction container, the spraying speed is higher when the pressure is higher, and the cooling speed of the melt is relatively higher; when the pressure is low, the ejection speed is low, and the cooling speed is relatively slow. The ejection speed is not only related to the pressure, but also related to the diameter of the nozzle, and when the nozzle is smaller, the ejection speed is higher, and when the nozzle is larger, the ejection speed is lower. Therefore, the melt is sprayed out after heat preservation (1-60 s) by controlling the high temperature (2100-4000 ℃) and the high pressure (5-50 MPa).
The invention can adjust the theoretical adiabatic temperature and reaction pressure of the combustion synthesis reaction by designing the proportion of the reactants. The pressure is controlled mainly by three ways: 1) adjusting the gas pressure in the container after reaction by changing the raw material ratio and the atmosphere pressure; 2) the pressure is regulated by the temperature generated by the reaction; 3) after the reaction, the system was reduced to the set pressure by reducing the pressure. And finally, controlling the pressure range in the system to be 5-50 MPa.
An electric heating body is arranged in the reactor, and the raw material powder is heated to 25-300 ℃, so that ZrO can be improved2Content of (2), reduction of Al2O3So as to improve and regulate the performance of the prepared nano composite reinforced ceramic.
The above process diluents have a wide range of applicability and include, but are not limited to, one or a combination of barium oxide, iron oxide, vanadium oxide, molybdenum oxide, aluminum oxide, zirconium oxide, magnesium oxide, calcium oxide, strontium oxide, scandium oxide, titanium oxide, chromium oxide, cobalt oxide, nickel oxide, yttrium oxide, niobium oxide, hafnium oxide, tantalum oxide, lanthanum oxide, cerium oxide, praseodymium oxide, neodymium oxide, samarium oxide, europium oxide, gadolinium oxide, terbium oxide, dysprosium oxide, holmium oxide, erbium oxide, thulium oxide, ytterbium oxide, lutetium oxide, and silicon oxide. Such as Al production2O3/MgO、Al2O3/TiO2、Al2O3/Y2O3、Al2O3/ZrO2/Y2O3And the like.
For the cooling process, the invention adopts a rotating iron, copper, steel disc (determined according to the temperature and pressure of the sprayed melt) or a roller device to Al2O3/ZrO2The melt is quenched to obtain Al2O3/ZrO2A mixture of amorphous and solid solution films or ribbons. For high temperature Al2O3/ZrO2The melt is rapidly cooled, and a rotating disc or a roller device is required to have excellent heat-conducting property; ag. Metals such as Al have good thermal conductivity but have a low melting point, and Al2O3/ZrO2The melt temperature is too high to cause great erosion effect on cooling metal, so the selected rotating disc or roller equipment is high-temperature resistant iron, copper or steel and assists water cooling to accelerate the cooling rate. Wherein, for the equipment of rotating iron, copper and steel discs, one side of the disc is sprayed with high-temperature Al2O3/ZrO2The melt is sprayed with high-pressure and high-speed water flow on the other side to assist cooling and reduce the temperature of the rotating iron, copper and steel discs (see figure 1). And for the roller equipment, high-temperature Al is sprayed between the rollers2O3/ZrO2The melt is sprayed with high-pressure and high-speed water flow on two sides to assist in cooling the double rollers (see figure 2). Generally, the faster the metal disc and counter-roller rotate, the Al2O3/ZrO2Melt body temperatureThe lower the degree, Al2O3/ZrO2The lower the solidification point of the melt (different molar ratios of Al)2O3、ZrO2Different freezing points) the higher the cooling rate.
Because the rotary iron, copper and steel discs are adopted for cooling, the cooling rate of the melt close to one side of the discs is high, and the melt is an amorphous structure; because of the low thermal conductivity of ceramics, supersaturated solid solutions can form on the outer layer away from the cooling surface of the metal plate when the melt is cooled at a relatively slow rate. Similarly, for the roller equipment, the strip close to the two circular rollers is of an amorphous structure, and the middle of the strip is of a supersaturated solid solution.
The pressure-resistant reaction vessel comprises a reactor 1, a tabletting 4, a nozzle 5, a nozzle support 6, a sealing preload piece 8, an upper slide plate 10, a lower slide plate 11 and a dragging device 9, wherein two-stage stepped circular holes are formed along the thickness direction of the bottom of the reactor 1, a first stepped circular hole 2 is positioned at the upper part of a second stepped circular hole 3, and the diameter of the first stepped circular hole 2 is larger than that of the second stepped circular hole 3;
the nozzle support 6 is of a coaxial integrated structure formed by a circular plate-shaped support body part 6-1 and a cylindrical part 6-2, an insertion hole 6-3 is formed along the central axis of the nozzle support 6, a circular ring groove 6-4 is formed in the end face of the cylindrical part 6-2, the nozzle support 6 is inserted and embedded into a two-stage stepped circular hole, the cylindrical part 6-2 is matched with a second stepped circular hole 3, the circular plate-shaped support body part 6-1 is matched with a first stepped circular hole 2, the lower surface of the circular plate-shaped support body part 6-1 is lapped on the stepped surface of the two-stage stepped circular hole, and a sealing preload piece 8 is embedded in the circular ring groove 6-4;
the pressing sheet 4 is arranged on the upper surface of the circular plate-shaped frame body 6-1, the pressing sheet 4 is in threaded connection with the first stepped round hole 2, and a pressing sheet through hole is formed in the center of the pressing sheet 4;
the nozzle 5 is arranged in a tabletting through hole of the tabletting 4 and an insertion hole 6-3 of the nozzle support 6, a graphite core is arranged in the nozzle 5, the bottom surface of the nozzle 5 is abutted against the upper surface of the sealing preload piece 8, the upper plate surface of the upper sliding plate 10 is contacted with the outer surface of the bottom of the reactor 1, the lower sliding plate 11 is contacted and arranged below the upper sliding plate 10, sliding plate through holes are respectively formed in the upper sliding plate 10 and the lower sliding plate 11, the sealing preload piece 8 is ensured to pass through the sliding plate through holes, the sliding plate through holes in the lower sliding plate 11 are directly opposite to the sealing preload piece 8, the upper sliding plate 10 is driven by the dragging device 9 to move horizontally, and the nozzle size of the nozzle is phi 1-20 mm.
The invention has the beneficial effects that:
the method has the advantages of simple process, rapid reaction (several seconds to several minutes), short preparation period, large yield (1-30 kg), high purity and controllability, and is a novel preparation process method of the metastable state micro-rice flour with low cost, high efficiency and high performance.
In the invention, Al is mainly mixed2O3/ZrO2The melt is rapidly quenched to obtain Al2O3/ZrO2The amorphous and solid solution powder mixture has extremely high heat dissipation requirements. Generally, the cooling rate is higher than 106K/s will have amorphous, it is necessary to require good heat conductivity of the rotating disc or roll equipment, good heat conductivity of Ag, Al and other metals, but low melting point, Al2O3/ZrO2The melt temperature is too high to cause great erosion effect on cooling metal, so the selected rotating disc or roller equipment is high-temperature resistant iron, copper or steel and assists water cooling to accelerate the cooling rate. Simultaneously increasing the ejection speed of the melt, reducing the temperature of the melt and lowering the solidification point of Al2O3/ZrO2The molar ratio is such that the cooling rate is increased, and the higher the cooling rate is, the more amorphous structure is formed.
Generally, the resulting amorphous and solid solution films are 5 μm to 30 μm thick. The powder prepared by ball milling is crushed and sintered by a high-temperature densification process, and the uniform and fine nano composite alumina/zirconia ceramic can be obtained. At present, the nano composite alumina/zirconia eutectic ceramic can be obtained by adopting the method for hot pressing and sintering.
When the content of zirconia is lower (20 wt% -40 wt%), the strength can reach 1000MPa, and the toughness can reach 12 MPa.m1/2(ii) a When the content of zirconia is medium (40 wt% -60 wt%), the strength can reach 1100MPa, and the toughness can reach 13 MPa.m1/2(ii) a When the content of zirconia is higher (60 wt% -80 wt%), the strength can reach 1200MPa, and the toughness can reach 15 MPa.m1/2。
The diluents of the process of the present invention have a wide range of applicability and includeBut are not limited to, barium oxide, iron oxide, vanadium oxide, molybdenum oxide, aluminum oxide, zirconium oxide, magnesium oxide, calcium oxide, strontium oxide, scandium oxide, titanium oxide, chromium oxide, cobalt oxide, nickel oxide, yttrium oxide, niobium oxide, hafnium oxide, tantalum oxide, lanthanum oxide, cerium oxide, praseodymium oxide, neodymium oxide, samarium oxide, europium oxide, gadolinium oxide, terbium oxide, dysprosium oxide, holmium oxide, erbium oxide, thulium oxide, ytterbium oxide, lutetium oxide, and silicon oxide, among others, and combinations thereof. Such as Al production2O3/MgO、Al2O3/TiO2、Al2O3/Y2O3、Al2O3/ZrO2/Y2O3And the like.
Drawings
FIG. 1 is a schematic illustration of the cooling of a rotating metal disk according to the present invention;
FIG. 2 is a schematic view of the cooling of a pair of rolls according to the present invention;
FIG. 3 is a schematic view of the structure of a pressure-resistant reactor according to the present invention;
FIG. 4 is a schematic view showing the structure of a nozzle holder in the pressure-resistant reactor of the present invention;
FIG. 5 is a surface microscopic SEM photograph of the milled, ball-milled micropowder of the example.
Detailed Description
The technical solution of the present invention is not limited to the specific embodiments listed below, and includes any combination of the specific embodiments.
The first embodiment is as follows: the embodiment of the invention relates to a quenching method for preparing Al by aluminum oxide combustion synthesis2O3The method for preparing the mixture of the amorphous ceramic micron powder and the solid solution ceramic micron powder comprises the following steps:
drying and uniformly mixing aluminum powder and a diluent to obtain mixed powder; 10-40 parts of aluminum powder and 60-90 parts of diluent by mass;
secondly, the mixed powder obtained in the step one is put into a pressure-resistant reactor with a nozzle at the lower end, oxidizing gas is introduced, the mixed powder is ignited to initiate a synthesis reaction, the temperature is kept, then the nozzle of the pressure-resistant reactor is opened, and the pressure-resistant reaction is carried outSpraying the composite melt in the reactor to the pair rollers of a rotating metal disc or roller device for cooling, then crushing and ball milling to obtain Al2O3Based on the mixture of amorphous and solid solution ceramic micron powder, the aluminum oxide combustion synthesis quenching method is completed for preparing Al2O3A method for preparing a mixture of amorphous and solid solution ceramic micropowder.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: in the first step, the diluent is one or a mixture of more of barium oxide, iron oxide, vanadium oxide, molybdenum oxide, aluminum oxide, zirconium oxide, magnesium oxide, calcium oxide, strontium oxide, scandium oxide, titanium oxide, chromium oxide, cobalt oxide, nickel oxide, yttrium oxide, niobium oxide, hafnium oxide, tantalum oxide, lanthanum oxide, cerium oxide, praseodymium oxide, neodymium oxide, samarium oxide, europium oxide, gadolinium oxide, terbium oxide, dysprosium oxide, holmium oxide, erbium oxide, thulium oxide, ytterbium oxide, lutetium oxide and silicon oxide. The rest is the same as the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: when Al is present2O3When the base amorphous and solid solution ceramic micron powder mixture contains zirconium oxide, Y2O3And ZrO2The molar ratio of (0-15) to 100; CeO (CeO)2And ZrO2The molar ratio of (0-30) to 100; MgO and ZrO2The molar ratio of (0-28) to 100; CaO and ZrO2The molar ratio of (0-33.45) to 100; TiO 22And ZrO2The molar ratio of (0-44.41) to 100; sc (Sc)2O3And ZrO2The molar ratio of (0-20) to 100. The other is the same as in the first or second embodiment.
Y in the present embodiment2O3，CeO2，MgO，CaO，TiO2，Sc2O3Act as phase change stabilizers.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: introducing oxidizing gas O in the second step2Or the oxidizing gas is O2Mixed with air, or with an oxidizing gas of O2And N2Or the oxidizing gas is O2Air and N2And (3) mixing. The others are the same as in one of the first to third embodiments.
In the present embodiment, the pressure of the oxidizing gas is 5 to 50MPa, wherein O is2The partial pressure is more than or equal to 5 MPa.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: if the composite melt is sprayed into a rotating metal disc in the second step, the radius of the rotating metal disc is 50-200 cm, and the rotating speed is 60-150 r/min; spraying Al on one side of rotating metal disc2O3/ZrO2Spraying high-pressure and high-speed water flow to the other side of the composite melt for auxiliary cooling, wherein the water amount is 20-30L/min, the water pressure is 0.1-0.5 MPa, and Al is formed by solidification on the surface of the rotating metal disc2O3/ZrO2Amorphous and solid solution films;
if the composite melt is sprayed into a pair roller of a roller device, the double roller device is adopted, the roller pressure is 30-70 MPa, and the roller rotating speed is 100-4000 rpm; spraying Al between the pair of rollers2O3/ZrO2Spraying high-pressure and high-speed water flow on two sides of the composite melt to assist in cooling the double rollers, wherein the water amount is 20-30L/min, the water pressure is 0.1-0.5 MPa, and extruding to form Al2O3/ZrO2Amorphous and solid solution ribbons.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is: method for preparing Al by aluminum oxide combustion synthesis quenching method2O3The method for preparing the amorphous and solid solution ceramic micron powder mixture specifically comprises the following steps:
firstly, mixing Al and Al2O3And ZrO2Drying in a vacuum drying oven at 60-120 ℃ for 8-16 h and 0.05-0.09 MPa, ball-milling by a planetary ball mill at a ball-material mass ratio of 3:1 for 2-8 h, sieving with a 40-200 mesh sieve, and mixing uniformly to obtain mixed powder;
secondly, the mixed powder obtained in the first step is put into a pressure-resistant reactor with a nozzle at the lower end, the nozzle size of the nozzle is phi 1-20mm,introducing oxidizing gas with the pressure of 5-50 MPa, wherein the oxidizing gas is O2Or O2Then the pressure-resistant reactor is arranged in a circulating water cooling device, the theoretical temperature is set to be 2100-4000 ℃, the reaction pressure is set to be 5-50 MPa, resistance wires ignite the mixed powder to initiate synthesis reaction, then the temperature is kept for 1-60 s, then a nozzle of the pressure-resistant reactor is opened, and Al in the pressure-resistant reactor2O3/ZrO2Spraying the composite melt to a rotating metal disc for cooling, then cleaning, drying, crushing by a crusher, then ball-milling by a planetary ball mill, controlling the ball-material mass ratio to be 3:1 and the ball-milling time to be 3-6 h, and sieving to obtain Al2O3/ZrO2The mixture of amorphous and solid solution ceramic micron powder is used for preparing Al by an aluminum oxide combustion synthesis quenching method2O3A method for preparing a mixture of amorphous and solid solution ceramic micropowder; wherein the rotating metal disc is an iron disc, a copper disc or a steel disc;
spraying the composite melt into a rotating metal disc, wherein the radius of the rotating metal disc is 50-200 cm, and the rotating speed is 60-150 r/min; spraying Al on one side of rotating metal disc2O3/ZrO2Spraying high-pressure and high-speed water flow to the other side of the composite melt for auxiliary cooling, wherein the water amount is 20-30L/min, the water pressure is 0.1-0.5 MPa, and Al is formed by solidification on the surface of the rotating metal disc2O3/ZrO2Amorphous and solid solution films.
The seventh embodiment: method for preparing Al by aluminum oxide combustion synthesis quenching method2O3The method for preparing the amorphous and solid solution ceramic micron powder mixture specifically comprises the following steps:
firstly, mixing Al and Al2O3And ZrO2Drying in a vacuum drying oven at 60-120 ℃ for 8-16 h and 0.05-0.09 MPa, ball-milling by a planetary ball mill at a ball-material mass ratio of 3:1 for 2-8 h, sieving with a 40-200 mesh sieve, and mixing uniformly to obtain mixed powder;
secondly, the mixed powder obtained in the first step is filled into a pressure-resistant reactor with a nozzle at the lower end, and the nozzle size of the nozzle is phi 1-20mm, introducing oxidizing gas with the pressure of 5-50 MPa, wherein the oxidizing gas is O2Or O2The pressure-resistant reactor is arranged in a circulating water cooling device, the theoretical temperature is set to be 2100-4000 ℃, the reaction pressure is set to be 5-50 MPa, the reaction time is 10-600 s, the resistance wire ignites the mixed powder to initiate the synthetic reaction, then the temperature is kept for 1-60 s, the nozzle of the pressure-resistant reactor is opened, and Al in the pressure-resistant reactor2O3/ZrO2Spraying the composite melt into a pair of rollers of a roller device for cooling, then cleaning, drying, crushing by a crusher, ball-milling and sieving to obtain Al2O3/ZrO2The mixture of amorphous and solid solution ceramic micron powder is used for preparing Al by an aluminum oxide combustion synthesis quenching method2O3A method for preparing a mixture of amorphous and solid solution ceramic micropowder;
spraying the composite melt into a pair roller of a roller device, wherein the roller pressure is 30-70 MPa, and the roller rotating speed is 100-4000 rpm by adopting a double-roller device; spraying Al between the pair of rollers2O3/ZrO2Spraying high-pressure and high-speed water flow on two sides of the composite melt to assist in cooling the double rollers, wherein the water amount is 20-30L/min, the water pressure is 0.1-0.5 MPa, and extruding to form Al2O3/ZrO2Amorphous and solid solution ribbons.
The specific implementation mode is eight: method for preparing Al by aluminum oxide combustion synthesis quenching method2O3The method for preparing the amorphous and solid solution ceramic micron powder mixture specifically comprises the following steps:
firstly, mixing Al and Al2O3And ZrO2Drying in a vacuum drying oven at 60-120 ℃ for 8-16 h and 0.05-0.09 MPa, ball-milling by a planetary ball mill at a ball-material mass ratio of 3:1 for 2-8 h, sieving with a 40-200 mesh sieve, and mixing uniformly to obtain mixed powder; wherein the dosage of Al is 10-40 parts by mass, and the diluent Al2O3And ZrO2The total amount of the (B) is 60-90 parts;
secondly, the mixed powder obtained in the step one is put into a pressure-resistant reactor with a nozzle at the lower end, and a nozzle ruler of the nozzleThe diameter is 1-20mm, and oxidizing gas with pressure of 5-50 MPa and O with oxidizing gas of 5-30 MPa is introduced2And 0 to 20MPa of N2Then installing the pressure-resistant reactor into a circulating water cooling device, setting the theoretical temperature to be 2100-4000 ℃, igniting the mixed powder to initiate a synthesis reaction, then preserving the heat for 1-60 s, then opening a nozzle of the pressure-resistant reactor, wherein Al in the pressure-resistant reactor2O3/ZrO2Spraying the composite melt onto a pair of rollers of a rotating metal disc or roller device for cooling, then cleaning, drying, crushing by a crusher, ball-milling and sieving to obtain Al2O3/ZrO2The mixture of amorphous and solid solution ceramic micron powder is used for preparing Al by an aluminum oxide combustion synthesis quenching method2O3A method for preparing a mixture of amorphous and solid solution ceramic micropowder; wherein the rotating metal disc is an iron disc, a copper disc or a steel disc;
if the composite melt is sprayed into a rotating metal disc, the radius of the rotating metal disc is 50-200 cm, and the rotating speed is 60-150 r/min; spraying Al on one side of rotating metal disc2O3/ZrO2Spraying high-pressure and high-speed water flow to the other side of the composite melt for auxiliary cooling, wherein the water amount is 20-30L/min, the water pressure is 0.1-0.5 MPa, and Al is formed by solidification on the surface of the rotating metal disc2O3/ZrO2Amorphous and solid solution films;
if the composite melt is sprayed into a pair roller of a roller device, the double roller device is adopted, the roller pressure is 30-70 MPa, and the roller rotating speed is 100-4000 rpm; spraying Al between the pair of rollers2O3/ZrO2Spraying high-pressure and high-speed water flow on two sides of the composite melt to assist in cooling the double rollers, wherein the water amount is 20-30L/min, the water pressure is 0.1-0.5 MPa, and extruding to form Al2O3/ZrO2Amorphous and solid solution ribbons.
The specific implementation method nine: method for preparing Al by aluminum oxide combustion synthesis quenching method2O3The method for preparing the amorphous and solid solution ceramic micron powder mixture specifically comprises the following steps:
firstly, mixing Al and Al2O3And ZrO2Drying in a vacuum drying oven at 60-120 deg.C,drying for 8-16 h, keeping the vacuum degree at 0.05-0.09 MPa, then carrying out ball milling by adopting a planetary ball mill, controlling the ball-material mass ratio at 3:1, carrying out ball milling for 2-8 h, then sieving by using a 40-200-mesh sieve, and uniformly mixing to obtain mixed powder; wherein the dosage of Al is 10-40 parts by mass, and the diluent Al2O3And ZrO2The total amount of the (B) is 60-90 parts;
secondly, the mixed powder obtained in the first step is put into a pressure-resistant reactor with a nozzle at the lower end, the nozzle size of the nozzle is phi 1-20mm, oxidizing gas with the pressure of 5-50 MPa is introduced, and the oxidizing gas is O with the pressure of 5-30 MPa2And 0 to 20MPa of N2Then the pressure-resistant reactor is arranged in a circulating water cooling device, mixed powder is heated to 25-300 ℃, the theoretical temperature is set to 2100-4000 ℃, the reaction pressure is 5-50 MPa, resistance wires ignite the mixed powder to initiate synthesis reaction, then the temperature is kept for 1-60 s, then a nozzle of the pressure-resistant reactor is opened, and Al in the pressure-resistant reactor2O3/ZrO2Spraying the composite melt onto a pair of rollers of a rotating metal disc or roller device for cooling, then cleaning, drying, crushing by a crusher, ball-milling and sieving to obtain Al2O3/ZrO2The mixture of amorphous and solid solution ceramic micron powder is used for preparing Al by an aluminum oxide combustion synthesis quenching method2O3A method for preparing a mixture of amorphous and solid solution ceramic micropowder; wherein the rotating metal disc is an iron disc, a copper disc or a steel disc;
if the composite melt is sprayed into a rotating metal disc, the radius of the rotating metal disc is 50-200 cm, and the rotating speed is 60-150 r/min; spraying Al on one side of rotating metal disc2O3/ZrO2Spraying high-pressure and high-speed water flow to the other side of the composite melt for auxiliary cooling, wherein the water amount is 20-30L/min, the water pressure is 0.1-0.5 MPa, and Al is formed by solidification on the surface of the rotating metal disc2O3/ZrO2Amorphous and solid solution films;
if the composite melt is sprayed into a pair roller of a roller device, the double roller device is adopted, the roller pressure is 30-70 MPa, and the roller rotating speed is 100-4000 rpm; spraying Al between the pair of rollers2O3/ZrO2Composite melt, spraying high on both sidesPressing and high-speed water flow auxiliary cooling paired rollers, the water amount is 20-30L/min, the water pressure is 0.1-0.5 MPa, and Al is formed by extrusion2O3/ZrO2Amorphous and solid solution ribbons.
The detailed implementation mode is ten: method for preparing Al by aluminum oxide combustion synthesis quenching method2O3The method for preparing the amorphous and solid solution ceramic micron powder mixture specifically comprises the following steps:
firstly, putting Al and a diluent into a vacuum drying oven for drying, controlling the drying temperature to be 60-120 ℃, the drying time to be 8-16 h and the vacuum degree to be 0.05-0.09 MPa, then carrying out ball milling by adopting a planetary ball mill for 2-8 h, then sieving by using a sieve of 40-200 meshes, and uniformly mixing to obtain mixed powder; wherein the dosage of Al is 10-40 parts by mass, and the dosage of the diluent is 60-90 parts by mass; the diluent is one or a mixture of more of barium oxide, iron oxide, vanadium oxide, molybdenum oxide, aluminum oxide, zirconium oxide, magnesium oxide, calcium oxide, strontium oxide, scandium oxide, titanium oxide, chromium oxide, cobalt oxide, nickel oxide, yttrium oxide, niobium oxide, hafnium oxide, tantalum oxide, lanthanum oxide, cerium oxide, praseodymium oxide, neodymium oxide, samarium oxide, europium oxide, gadolinium oxide, terbium oxide, dysprosium oxide, holmium oxide, erbium oxide, thulium oxide, ytterbium oxide, lutetium oxide and silicon oxide; when Al is present2O3When the base amorphous and solid solution ceramic micron powder mixture contains zirconium oxide, Y2O3And ZrO2The molar ratio of (0-15) to 100; CeO (CeO)2And ZrO2The molar ratio of (0-30) to 100; MgO and ZrO2The molar ratio of (0-28) to 100; CaO and ZrO2The molar ratio of (0-33.45) to 100; TiO 22And ZrO2The molar ratio of (0-44.41) to 100; sc (Sc)2O3And ZrO2The molar ratio of (0-20) to 100;
secondly, the mixed powder obtained in the first step is put into a pressure-resistant reactor with a nozzle at the lower end, the nozzle size of the nozzle is phi 1-20mm, oxidizing gas with the pressure of 5-50 MPa is introduced, and the oxidizing gas is O with the pressure of 5-30 MPa2And 0 to 20MPa of N2Then the pressure-resistant reactor is arranged to be cooled by circulating waterIn the device, the theoretical temperature is set to be 2100-4000 ℃, the reaction pressure is set to be 5-50 MPa, the resistance wire ignites the mixed powder to initiate the synthetic reaction, then the temperature is kept for 1-60 s, then the nozzle of the pressure-resistant reactor is opened, and Al in the pressure-resistant reactor2O3/ZrO2Spraying the composite melt onto a pair of rollers of a rotating metal disc or roller device for cooling, then cleaning, drying, crushing by a crusher, ball-milling and sieving to obtain Al2O3/ZrO2The mixture of amorphous and solid solution ceramic micron powder is used for preparing Al by an aluminum oxide combustion synthesis quenching method2O3A method for preparing a mixture of amorphous and solid solution ceramic micropowder; wherein the rotating metal disc is an iron disc, a copper disc or a steel disc;
if the composite melt is sprayed into a rotating metal disc, the radius of the rotating metal disc is 50-200 cm, and the rotating speed is 60-150 r/min; spraying Al on one side of rotating metal disc2O3/ZrO2Spraying high-pressure and high-speed water flow to the other side of the composite melt for auxiliary cooling, wherein the water amount is 20-30L/min, the water pressure is 0.1-0.5 MPa, and Al is formed by solidification on the surface of the rotating metal disc2O3/ZrO2Amorphous and solid solution films;
if the composite melt is sprayed into a pair roller of a roller device, the double roller device is adopted, the roller pressure is 30-70 MPa, and the roller rotating speed is 100-4000 rpm; spraying Al between the pair of rollers2O3/ZrO2Spraying high-pressure and high-speed water flow on two sides of the composite melt to assist in cooling the double rollers, wherein the water amount is 20-30L/min, the water pressure is 0.1-0.5 MPa, and extruding to form Al2O3/ZrO2Amorphous and solid solution ribbons.
The concrete implementation mode eleven: the present embodiment differs from one of the first to tenth embodiments in that: the pressure-resistant reaction vessel comprises a reactor 1, a pressing sheet 4, a nozzle 5, a nozzle support 6, a sealing preload piece 8, an upper sliding plate 10, a lower sliding plate 11 and a dragging device 9, wherein two-stage stepped circular holes are formed along the thickness direction of the bottom of the reactor 1, a first stepped circular hole 2 is positioned at the upper part of a second stepped circular hole 3, and the diameter of the first stepped circular hole 2 is larger than that of the second stepped circular hole 3;
the nozzle support 6 is of a coaxial integrated structure formed by a circular plate-shaped support body part 6-1 and a cylindrical part 6-2, an insertion hole 6-3 is formed along the central axis of the nozzle support 6, a circular ring groove 6-4 is formed in the end face of the cylindrical part 6-2, the nozzle support 6 is inserted and embedded into a two-stage stepped circular hole, the cylindrical part 6-2 is matched with a second stepped circular hole 3, the circular plate-shaped support body part 6-1 is matched with a first stepped circular hole 2, the lower surface of the circular plate-shaped support body part 6-1 is lapped on the stepped surface of the two-stage stepped circular hole, and a sealing preload piece 8 is embedded in the circular ring groove 6-4;
the pressing sheet 4 is arranged on the upper surface of the circular plate-shaped frame body 6-1, the pressing sheet 4 is in threaded connection with the first stepped round hole 2, and a pressing sheet through hole is formed in the center of the pressing sheet 4;
the nozzle 5 is arranged in a pressing sheet through hole of the pressing sheet 4 and an insertion hole 6-3 of the nozzle support 6, a graphite core is arranged in the nozzle 5, the bottom surface of the nozzle 5 abuts against the upper surface of the sealing preload piece 8, the upper plate surface of the upper sliding plate 10 is in contact with the outer surface of the bottom of the reactor 1, the lower sliding plate 11 is in contact with the lower part of the upper sliding plate 10, sliding plate through holes are respectively formed in the upper sliding plate 10 and the lower sliding plate 11, the sealing preload piece 8 is guaranteed to pass through the sliding plate through holes, the sliding plate through holes in the lower sliding plate 11 are opposite to the sealing preload piece 8, and the upper sliding plate 10 is driven to move horizontally by the dragging device 9.
The invention is not limited to the above embodiments, and one or a combination of several embodiments may also achieve the object of the invention.
The following examples were employed to demonstrate the effects of the present invention
The following examples are all carried out by adopting a pressure-resistant reaction vessel, the pressure-resistant reaction vessel comprises a reactor 1, a resistance wire, a nozzle 5, a sealing preload piece 8, an upper sliding plate 10, a lower sliding plate 11 and a dragging device 9, the resistance wire is arranged on the inner side of an upper cover of the reactor 1, a vertical through hole is arranged along the thickness direction of the bottom of the reactor 1, the nozzle 5 is screwed into the vertical through hole and connected through threads, a pretension piece groove is arranged on the circumference of the lower nozzle of the vertical through hole, the sealing pretension piece 8 is inserted into the pretension piece groove, the longitudinal section of the sealing preload part 8 is U-shaped, the upper plate surface of the upper sliding plate 10 is in contact with the outer surface of the bottom of the reactor 1, the lower sliding plate 11 is in contact with the lower part of the upper sliding plate 10, sliding plate through holes are respectively formed in the upper sliding plate 10 and the lower sliding plate 11, the sealing preload part 8 is ensured to pass through the hole diameter of each sliding plate through hole, the sliding plate through holes in the lower sliding plate 11 are opposite to the sealing preload part 8, and the upper sliding plate 10 is driven by the dragging device 9 to move horizontally.
The first embodiment is as follows: method for preparing Al by aluminum oxide combustion synthesis quenching method2O3The method for preparing the amorphous and solid solution ceramic micron powder mixture specifically comprises the following steps:
firstly, mixing Al and Al2O3And ZrO2Drying in a vacuum drying oven at 80 deg.C for 10h and under 0.06MPa, ball-milling with a planetary ball mill at ball-to-material mass ratio of 3:1 for 3h, sieving with 100 mesh sieve, and mixing to obtain mixed powder; the Al content in the mixed powder was 131.79g, Al2O3399.22g ZrO2In the form of 468.98g of a powder,
secondly, the mixed powder obtained in the step one is put into a pressure-resistant reactor with a nozzle at the lower end, the nozzle size of the nozzle is phi 8mm, and O with the pressure of 13MPa is introduced2Then the pressure-resistant reactor is arranged in a circulating water cooling device, resistance wires ignite the mixed powder to initiate synthesis reaction, then the temperature is kept for 10s, then a nozzle of the pressure-resistant reactor is opened, and Al in the pressure-resistant reactor2O3/ZrO2Spraying the composite melt to a rotating metal disc for cooling, then cleaning, drying, crushing by a crusher, then ball-milling by a planetary ball mill, controlling the ball-material mass ratio to be 3:1 and the ball-milling time to be 4h, and sieving to obtain Al2O3/ZrO2The mixture of amorphous and solid solution ceramic micron powder is used for preparing Al by an aluminum oxide combustion synthesis quenching method2O3A method for preparing a mixture of amorphous and solid solution ceramic micropowder; wherein the rotating metal disc is an iron disc, a copper disc or a steel disc;
spraying the composite melt into a rotating metal disc, wherein the radius of the rotating metal disc is 80cm, and the rotating speed is 100 r/min; spraying Al on one side of rotating metal disc2O3/ZrO2Spraying high-pressure and high-speed water flow to the other side of the composite melt for auxiliary cooling, wherein the water amount is 30L/min, the water pressure is 0.5MPa, and Al is formed on the surface of the rotating metal disc by solidification2O3/ZrO2Thin amorphous and solid solutionAnd (3) a membrane.
Example one is shown in fig. 5, which shows the surface microscopic SEM picture of the milled and ball-milled micropowder, and it can be seen from the SEM picture of the micropowder in fig. 5 that the powder size is from submicron to several microns and the particle size is relatively uniform. These results further illustrate that: al is heated by a high-temperature heating device2O3/ZrO2The composite powder is melted and cooled by rotating an iron disc, a copper disc and a steel disc, so that high-purity micron-sized powder can be prepared; and the method has low cost, is green and environment-friendly, and is suitable for large-scale industrial production.
Carrying out hot-pressing sintering densification treatment on amorphous and solid solution micron powder, and carrying out three-point bending test on the prepared material, wherein the performance is as follows: fracture toughness 8.35MPa m1/2The flexural strength was 710 MPa.
Example two: method for preparing Al by aluminum oxide combustion synthesis quenching method2O3The method for preparing the amorphous and solid solution ceramic micron powder mixture specifically comprises the following steps:
firstly, mixing Al and Al2O3And ZrO2Drying in a vacuum drying oven at 80 deg.C for 10h and under 0.06MPa, ball-milling with a planetary ball mill at ball-to-material mass ratio of 3:1 for 3h, sieving with a 40-mesh sieve, and mixing to obtain mixed powder; the Al content in the mixed powder was 207.69g, Al2O3554.08g ZrO2In the form of 238.24g of a powder,
secondly, the mixed powder obtained in the step one is put into a pressure-resistant reactor with a nozzle at the lower end, the nozzle size of the nozzle is phi 3mm, and O with the pressure of 22MPa is introduced2Then the pressure-resistant reactor is arranged in a circulating water cooling device, resistance wires ignite the mixed powder to initiate synthesis reaction, then the temperature is kept for 20s, then a nozzle of the pressure-resistant reactor is opened, and Al in the pressure-resistant reactor2O3/ZrO2Spraying the composite melt to a rotating metal disc for cooling, then cleaning, drying, crushing by a crusher, then ball-milling by a planetary ball mill, controlling the ball-material mass ratio to be 3:1 and the ball-milling time to be 3h, and sieving to obtain Al2O3/ZrO2The mixture of amorphous and solid solution ceramic micron powder is used for preparing Al by an aluminum oxide combustion synthesis quenching method2O3A method for preparing a mixture of amorphous and solid solution ceramic micropowder; wherein the rotating metal disc is an iron disc, a copper disc or a steel disc;
spraying the composite melt into a rotating metal disc, wherein the radius of the rotating metal disc is 80cm, and the rotating speed is 90 r/min; spraying Al on one side of rotating metal disc2O3/ZrO2Spraying high-pressure and high-speed water flow to the other side of the composite melt for auxiliary cooling, wherein the water amount is 20L/min, the water pressure is 0.5MPa, and Al is formed on the surface of the rotating metal disc by solidification2O3/ZrO2Amorphous and solid solution films.
Example three: method for preparing Al by aluminum oxide combustion synthesis quenching method2O3The method for preparing the amorphous and solid solution ceramic micron powder mixture specifically comprises the following steps:
firstly, mixing Al and Al2O3And ZrO2And a stabilizer Y2O3Drying in a vacuum drying oven at 100 deg.C for 8h and under 0.05MPa, ball-milling with a planetary ball mill at ball-to-material mass ratio of 3:1 for 3h, sieving with a 60-mesh sieve, and mixing to obtain mixed powder; the Al content in the mixed powder was 154.76g, Al2O3367.14g ZrO2478.10g and Y2O3175.79 g;
secondly, the mixed powder obtained in the step one is put into a pressure-resistant reactor with a nozzle at the lower end, the nozzle size of the nozzle is phi 4mm, and O with the pressure of 15MPa is introduced2Then the pressure-resistant reactor is arranged in a circulating water cooling device, resistance wires ignite the mixed powder to initiate synthesis reaction, then the temperature is kept for 10s, then a nozzle of the pressure-resistant reactor is opened, and Al in the pressure-resistant reactor2O3/ZrO2(Y2O3) Spraying the composite melt into a pair of rollers of a roller device for cooling, then cleaning, drying, crushing by a crusher, ball-milling and sieving to obtain Al2O3/ZrO2(Y2O3) Mixing amorphous and solid solution ceramic micron powderMethod for preparing Al by aluminum oxide combustion synthesis quenching method2O3A method for preparing a mixture of amorphous and solid solution ceramic micropowder;
spraying the composite melt into a pair roller of a roller device, wherein the roller pressure is 50MPa, and the roller rotating speed is 2000 rpm; spraying Al between the pair of rollers2O3/ZrO2(Y2O3) Spraying high-pressure and high-speed water flow on two sides of the composite melt to assist in cooling the double rollers, wherein the water amount is 25L/min, the water pressure is 0.3MPa, and extruding to form Al2O3/ZrO2(Y2O3) Amorphous and solid solution ribbons.
Example four: method for preparing Al by aluminum oxide combustion synthesis quenching method2O3The method for preparing the amorphous and solid solution ceramic micron powder mixture specifically comprises the following steps:
firstly, mixing Al and Al2O3And ZrO2And a stabilizer CeO2Drying in a vacuum drying oven at 100 deg.C for 8h and under 0.05MPa, ball-milling with a planetary ball mill at ball-to-material mass ratio of 3:1 for 3h, sieving with a 60-mesh sieve, and mixing to obtain mixed powder; the Al content in the mixed powder was 178.62g, Al2O3334.37g ZrO2487.01g of CeO2204.42 g;
secondly, the mixed powder obtained in the step one is put into a pressure-resistant reactor with a nozzle at the lower end, the nozzle size of the nozzle is phi 8mm, and O with the pressure of 20MPa is introduced2Then the pressure-resistant reactor is arranged in a circulating water cooling device, resistance wires ignite the mixed powder to initiate synthesis reaction, then the temperature is kept for 10s, then a nozzle of the pressure-resistant reactor is opened, and Al in the pressure-resistant reactor2O3/ZrO2(CeO2) Spraying the composite melt to a rotating metal disc for cooling, then cleaning, drying, crushing by a crusher, then ball-milling by a planetary ball mill, controlling the ball-material mass ratio to be 3:1 and the ball-milling time to be 3h, and sieving to obtain Al2O3/ZrO2(CeO2) The mixture of amorphous and solid solution ceramic micron powder completes the alumina burningPreparation of Al by synthetic quenching method2O3A method for preparing a mixture of amorphous and solid solution ceramic micropowder; wherein the rotating metal disc is an iron disc, a copper disc or a steel disc;
spraying the composite melt into a rotating metal disc, wherein the radius of the rotating metal disc is 80cm, and the rotating speed is 90 r/min; spraying Al on one side of rotating metal disc2O3/ZrO2(CeO2) Spraying high-pressure and high-speed water flow to the other side of the composite melt for auxiliary cooling, wherein the water amount is 20L/min, the water pressure is 0.5MPa, and Al is formed on the surface of the rotating metal disc by solidification2O3/ZrO2(CeO2) Amorphous and solid solution films.
Example five: method for preparing Al by aluminum oxide combustion synthesis quenching method2O3The method for preparing the amorphous and solid solution ceramic micron powder mixture specifically comprises the following steps:
firstly, mixing Al and Al2O3And ZrO2Drying in a vacuum drying oven at 100 deg.C for 8h and under 0.05MPa, ball-milling with a planetary ball mill at ball-to-material mass ratio of 3:1 for 3h, sieving with a 60-mesh sieve, and mixing to obtain mixed powder; wherein the mixed powder contains Al 168.97g and ZrO2483.41g of Al2O3347.62 g;
secondly, the mixed powder obtained in the step one is put into a pressure-resistant reactor with a nozzle at the lower end, the nozzle size of the nozzle is phi 4mm, and O with the pressure of 15MPa is introduced2And N of 3MPa2Then the pressure-resistant reactor is arranged in a circulating water cooling device, resistance wires ignite the mixed powder to initiate synthesis reaction, then the temperature is kept for 10s, then a nozzle of the pressure-resistant reactor is opened, and Al in the pressure-resistant reactor2O3/ZrO2Spraying the composite melt to a rotating metal disc for cooling, then cleaning, drying, crushing by a crusher, ball-milling by a planetary ball mill, controlling the ball-material mass ratio to be 3:1 and the ball-milling time to be 3h, ball-milling, and sieving to obtain Al2O3/ZrO2The mixture of amorphous and solid solution ceramic micron powder is used for preparing Al by an aluminum oxide combustion synthesis quenching method2O3A method for preparing a mixture of amorphous and solid solution ceramic micropowder; wherein the rotating metal disc is an iron disc, a copper disc or a steel disc;
spraying the composite melt into a rotating metal disc, wherein the radius of the rotating metal disc is 80cm, and the rotating speed is 90 r/min; spraying Al on one side of rotating metal disc2O3/ZrO2Spraying high-pressure and high-speed water flow to the other side of the composite melt for auxiliary cooling, wherein the water amount is 20L/min, the water pressure is 0.5MPa, and Al is formed on the surface of the rotating metal disc by solidification2O3/ZrO2Amorphous and solid solution films.
Example six: method for preparing Al by aluminum oxide combustion synthesis quenching method2O3The method for preparing the amorphous and solid solution ceramic micron powder mixture specifically comprises the following steps:
firstly, mixing Al and Al2O3And ZrO2Drying in a vacuum drying oven at 100 deg.C for 8h and under 0.05MPa, ball-milling with a planetary ball mill at ball-to-material mass ratio of 3:1 for 3h, sieving with a 60-mesh sieve, and mixing to obtain mixed powder; wherein the mixed powder contains 1317.3g of Al and ZrO24697.8g of Al2O33984.9 g;
secondly, the mixed powder obtained in the step one is put into a pressure-resistant reactor with a nozzle at the lower end, the nozzle size of the nozzle is phi 6mm, and O with the pressure of 13MPa is introduced2Then the pressure-resistant reactor is arranged in a circulating water cooling device, the mixed powder is heated to 300 ℃, resistance wires are used for igniting the mixed powder to initiate a synthesis reaction, then the temperature is kept for 10s, then a nozzle of the pressure-resistant reactor is opened, and Al in the pressure-resistant reactor2O3/ZrO2Spraying the composite melt to a rotating metal disc for cooling, then cleaning, drying, crushing by a crusher, ball-milling by a planetary ball mill, controlling the ball-material mass ratio to be 3:1 and the ball-milling time to be 3h, ball-milling, and sieving to obtain Al2O3/ZrO2The mixture of amorphous and solid solution ceramic micron powder is used for preparing Al by an aluminum oxide combustion synthesis quenching method2O3Amorphous and solid solution based ceramic micron powderA method of mixing; wherein the rotating metal disc is an iron disc, a copper disc or a steel disc;
spraying the composite melt into a rotating metal disc, wherein the radius of the rotating metal disc is 80cm, and the rotating speed is 90 r/min; spraying Al on one side of rotating metal disc2O3/ZrO2Spraying high-pressure and high-speed water flow to the other side of the composite melt for auxiliary cooling, wherein the water amount is 20L/min, the water pressure is 0.5MPa, and Al is formed on the surface of the rotating metal disc by solidification2O3/ZrO2Amorphous and solid solution films.
Example seven: method for preparing Al by aluminum oxide combustion synthesis quenching method2O3The method for preparing the amorphous and solid solution ceramic micron powder mixture specifically comprises the following steps:
firstly, mixing Al, MgO and HfO2Drying in a vacuum drying oven at 80 deg.C for 12h and under 0.07MPa, ball-milling with a planetary ball mill at ball-to-material mass ratio of 3:1 for 3h, sieving with a 60-mesh sieve, and mixing to obtain mixed powder; wherein the mixed powder contains 145.20g of Al, 429.56g of MgO and HfO2425.23 g;
secondly, the mixed powder obtained in the step one is put into a pressure-resistant reactor with a nozzle at the lower end, the nozzle size of the nozzle is phi 4mm, and O with the pressure of 15MPa is introduced2Then the pressure-resistant reactor is arranged in a circulating water cooling device, resistance wires ignite the mixed powder to initiate synthesis reaction, then the temperature is kept for 10s, then a nozzle of the pressure-resistant reactor is opened, and Al in the pressure-resistant reactor2O3/MgO/HfO2Spraying the composite melt to a rotating metal disc for cooling, then cleaning, drying, crushing by a crusher, ball-milling by a planetary ball mill, controlling the ball-material mass ratio to be 3:1 and the ball-milling time to be 3h, ball-milling, and sieving to obtain Al2O3/MgO/HfO2The mixture of amorphous and solid solution ceramic micron powder is used for preparing Al by an aluminum oxide combustion synthesis quenching method2O3A method for preparing a mixture of amorphous and solid solution ceramic micropowder; wherein the rotating metal disc is an iron disc, a copper disc or a steel disc;
spraying the composite melt onto the rotating goldIn the disc, the radius of the rotating metal disc is 80cm, and the rotating speed is 90 r/min; spraying Al on one side of rotating metal disc2O3/MgO/HfO2Spraying high-pressure and high-speed water flow to the other side of the composite melt for auxiliary cooling, wherein the water amount is 20L/min, the water pressure is 0.5MPa, and Al is formed on the surface of the rotating metal disc by solidification2O3/MgO/HfO2Amorphous and solid solution films.
Example eight: method for preparing Al by aluminum oxide combustion synthesis quenching method2O3The method for preparing the amorphous and solid solution ceramic micron powder mixture specifically comprises the following steps:
firstly, mixing Al and TiO2Drying in a vacuum drying oven at 80 deg.C for 12h and under 0.07MPa, ball-milling with a planetary ball mill at ball-to-material mass ratio of 3:1 for 3h, sieving with a 60-mesh sieve, and mixing to obtain mixed powder; wherein the mixed powder contains 114.2g of Al and TiO2885.8 g;
secondly, the mixed powder obtained in the step one is put into a pressure-resistant reactor with a nozzle at the lower end, the nozzle size of the nozzle is phi 8mm, and O with the pressure of 10MPa is introduced2Then the pressure-resistant reactor is arranged in a circulating water cooling device, the mixed powder is ignited to initiate the synthesis reaction, then the temperature is kept for 10s, then the nozzle of the pressure-resistant reactor is opened, and Al in the pressure-resistant reactor2O3/TiO2Spraying the composite melt to a rotating metal disc for cooling, then cleaning, drying, crushing by a crusher, ball-milling by a planetary ball mill, controlling the ball-material mass ratio to be 3:1 and the ball-milling time to be 3h, ball-milling, and sieving to obtain Al2O3/TiO2The mixture of amorphous and solid solution ceramic micron powder is used for preparing Al by an aluminum oxide combustion synthesis quenching method2O3A method for preparing a mixture of amorphous and solid solution ceramic micropowder; wherein the rotating metal disc is an iron disc, a copper disc or a steel disc;
spraying the composite melt into a rotating metal disc, wherein the radius of the rotating metal disc is 80cm, and the rotating speed is 90 r/min; spraying Al on one side of rotating metal disc2O3/TiO2Spraying high pressure on the other side of the composite meltHigh-speed water flow auxiliary cooling is carried out, the water amount is 20L/min, the water pressure is 0.5MPa, and Al is formed by solidification on the surface of the rotating metal disc2O3/TiO2Amorphous and solid solution films.
Example nine: method for preparing Al by aluminum oxide combustion synthesis quenching method2O3The method for preparing the amorphous and solid solution ceramic micron powder mixture specifically comprises the following steps:
firstly, mixing Al and Al2O3Drying in a vacuum drying oven at 100 deg.C for 8h and under 0.05MPa, ball-milling with a planetary ball mill at ball-to-material mass ratio of 3:1 for 3h, sieving with a 60-mesh sieve, and mixing to obtain mixed powder; wherein the mixed powder contains Al 136g and Al2O3864 g;
secondly, the mixed powder obtained in the step one is put into a pressure-resistant reactor with a nozzle at the lower end, the nozzle size of the nozzle is phi 6mm, and O with the pressure of 13MPa is introduced2Mixing with 3MPa air, loading the pressure-resistant reactor into a circulating water cooling device, igniting the mixed powder by using a resistance wire to initiate a synthesis reaction, keeping the temperature for 15s, starting a nozzle of the pressure-resistant reactor, and keeping Al in the pressure-resistant reactor2O3Spraying the melt to a rotating metal disc for cooling, then cleaning, drying, crushing by a crusher, ball-milling by a planetary ball mill with the ball-material mass ratio of 3:1 and the ball-milling time of 3h, ball-milling and sieving to obtain Al2O3The mixture of amorphous and solid solution ceramic micron powder is used for preparing Al by an aluminum oxide combustion synthesis quenching method2O3A method for preparing a mixture of amorphous and solid solution ceramic micropowder; wherein the rotating metal disc is an iron disc, a copper disc or a steel disc;
spraying the composite melt into a rotating metal disc, wherein the radius of the rotating metal disc is 80cm, and the rotating speed is 90 r/min; spraying Al on one side of rotating metal disc2O3Spraying high-pressure and high-speed water flow to the other side of the composite melt for auxiliary cooling, wherein the water amount is 20L/min, the water pressure is 0.5MPa, and Al is formed on the surface of the rotating metal disc by solidification2O3Amorphous and solid solution films.
Example ten: method for preparing Al by aluminum oxide combustion synthesis quenching method2O3The method for preparing the amorphous and solid solution ceramic micron powder mixture specifically comprises the following steps:
firstly, mixing Al and Al2O3And ZrO2And a stabilizer Y2O3Drying in a vacuum drying oven at 100 deg.C for 8h and under 0.05MPa, ball-milling with a planetary ball mill at ball-to-material mass ratio of 3:1 for 3h, sieving with a 60-mesh sieve, and mixing to obtain mixed powder; the Al content in the mixed powder was 179.39g, Al2O3587.43g ZrO2233.18g and Y2O334.25 g;
secondly, the mixed powder obtained in the step one is put into a pressure-resistant reactor with a nozzle at the lower end, the nozzle size of the nozzle is phi 10mm, and O with the pressure of 20MPa is introduced2And 2MPa of N2Then the pressure-resistant reactor is arranged in a circulating water cooling device, resistance wires ignite the mixed powder to initiate synthesis reaction, then the temperature is kept for 10s, then a nozzle of the pressure-resistant reactor is opened, and Al in the pressure-resistant reactor2O3/ZrO2(Y2O3) Spraying the composite melt into a pair of rollers of a roller device for cooling, then cleaning, drying, crushing by a crusher, ball-milling and sieving to obtain Al2O3/ZrO2(Y2O3) The mixture of amorphous and solid solution ceramic micron powder is used for preparing Al by an aluminum oxide combustion synthesis quenching method2O3A method for preparing a mixture of amorphous and solid solution ceramic micropowder;
spraying the composite melt into a pair roller of a roller device, wherein the roller pressure is 50MPa, and the roller rotating speed is 2000 rpm; spraying Al between the pair of rollers2O3/ZrO2(Y2O3) Spraying high-pressure and high-speed water flow on two sides of the composite melt to assist in cooling the double rollers, wherein the water amount is 25L/min, the water pressure is 0.3MPa, and extruding to form Al2O3/ZrO2(Y2O3) Amorphous and solid solution ribbons.
ExamplesEleven: method for preparing Al by aluminum oxide combustion synthesis quenching method2O3The method for preparing the amorphous and solid solution ceramic micron powder mixture specifically comprises the following steps:
firstly, mixing Al and Al2O3And ZrO2And a stabilizer Y2O3Drying in a vacuum drying oven at 100 deg.C for 8h and under 0.05MPa, ball-milling with a planetary ball mill at ball-to-material mass ratio of 3:1 for 3h, sieving with a 60-mesh sieve, and mixing to obtain mixed powder; the Al content in the mixed powder was 142.89g, Al2O3518.54g ZrO2338.56g and Y2O318.66 g;
secondly, the mixed powder obtained in the step one is put into a pressure-resistant reactor with a nozzle at the lower end, the nozzle size of the nozzle is phi 3mm, and O with the pressure of 14MPa is introduced2And 2MPa of air, then placing the pressure-resistant reactor into a circulating water cooling device, heating the mixed powder to 200 ℃, igniting the mixed powder by using a resistance wire to initiate a synthesis reaction, then preserving heat for 15s, then opening a nozzle of the pressure-resistant reactor, and placing Al in the pressure-resistant reactor2O3/ZrO2(Y2O3) Spraying the composite melt into a pair of rollers of a roller device for cooling, then cleaning, drying, crushing by a crusher, ball-milling and sieving to obtain Al2O3/ZrO2(Y2O3) The mixture of amorphous and solid solution ceramic micron powder is used for preparing Al by an aluminum oxide combustion synthesis quenching method2O3A method for preparing a mixture of amorphous and solid solution ceramic micropowder;
spraying the composite melt into a pair roller of a roller device, wherein the roller pressure is 50MPa, and the roller rotating speed is 2000 rpm; spraying Al between the pair of rollers2O3/ZrO2(Y2O3) Spraying high-pressure and high-speed water flow on two sides of the composite melt to assist in cooling the double rollers, wherein the water amount is 30L/min, the water pressure is 0.3MPa, and extruding to form Al2O3/ZrO2(Y2O3) Amorphous and solid solution ribbons.
For amorphous and solidThe solution micron powder is subjected to hot-pressing sintering densification treatment, and the prepared material is subjected to a three-point bending test, and the performance of the material is as follows: fracture toughness 9.25MPa m1/2The flexural strength was 920 MPa.
Example twelve: method for preparing Al by aluminum oxide combustion synthesis quenching method2O3The method for preparing the amorphous and solid solution ceramic micron powder mixture specifically comprises the following steps:
firstly, mixing Al and Al2O3And ZrO2And a stabilizer CeO2Drying in a vacuum drying oven at 100 deg.C for 8h and under 0.05MPa, ball-milling with a planetary ball mill at ball-to-material mass ratio of 3:1 for 3h, sieving with a 60-mesh sieve, and mixing to obtain mixed powder; the Al content in the mixed powder was 114.11g, Al2O3Is 3.56g, ZrO2882.32g of CeO2It was 129.54 g.
Secondly, the mixed powder obtained in the step one is put into a pressure-resistant reactor with a nozzle at the lower end, the nozzle size of the nozzle is phi 6mm, and O with the pressure of 12MPa is introduced2Then the pressure-resistant reactor is arranged in a circulating water cooling device, resistance wires ignite the mixed powder to initiate synthesis reaction, then the temperature is kept for 10s, then a nozzle of the pressure-resistant reactor is opened, and Al in the pressure-resistant reactor2O3/ZrO2(CeO2) Spraying the composite melt to a rotating metal disc for cooling, then cleaning, drying, crushing by a crusher, then ball-milling by a planetary ball mill, controlling the ball-material mass ratio to be 3:1 and the ball-milling time to be 3h, and sieving to obtain Al2O3/ZrO2(CeO2) The mixture of amorphous and solid solution ceramic micron powder is used for preparing Al by an aluminum oxide combustion synthesis quenching method2O3A method for preparing a mixture of amorphous and solid solution ceramic micropowder; wherein the rotating metal disc is an iron disc, a copper disc or a steel disc;
spraying the composite melt into a rotating metal disc, wherein the radius of the rotating metal disc is 80cm, and the rotating speed is 90 r/min; spraying Al on one side of rotating metal disc2O3/ZrO2(CeO2) Composite melt corresponding to anotherSide-spraying high-pressure and high-speed water flow for auxiliary cooling, wherein the water amount is 20L/min, the water pressure is 0.5MPa, and Al is formed on the surface of the rotating metal disc by solidification2O3/ZrO2(CeO2) Amorphous and solid solution films.
Carrying out hot-pressing sintering densification treatment on amorphous and solid solution micron powder, and carrying out three-point bending test on the prepared material, wherein the performance is as follows: fracture toughness 13.15MPa m1/2The flexural strength was 1020 MPa.
Example thirteen: method for preparing Al by aluminum oxide combustion synthesis quenching method2O3The method for preparing the amorphous and solid solution ceramic micron powder mixture specifically comprises the following steps:
firstly, mixing Al and Al2O3And ZrO2Drying in a vacuum drying oven at 100 deg.C for 8h and under 0.05MPa, ball-milling with a planetary ball mill at ball-to-material mass ratio of 3:1 for 3h, sieving with a 60-mesh sieve, and mixing to obtain mixed powder; wherein the mixed powder contains Al 147.26g and ZrO2680.39g of Al2O3172.35 g;
secondly, the mixed powder obtained in the step one is put into a pressure-resistant reactor with a nozzle at the lower end, the nozzle size of the nozzle is phi 3mm, and O with the pressure of 15MPa is introduced2Then the pressure-resistant reactor is arranged in a circulating water cooling device, resistance wires ignite the mixed powder to initiate synthesis reaction, then the temperature is kept for 20s, then a nozzle of the pressure-resistant reactor is opened, and Al in the pressure-resistant reactor2O3/ZrO2Spraying the composite melt to a rotating metal disc for cooling, then cleaning, drying, crushing by a crusher, ball-milling by a planetary ball mill, controlling the ball-material mass ratio to be 3:1 and the ball-milling time to be 3h, ball-milling, and sieving to obtain Al2O3/ZrO2The mixture of amorphous and solid solution ceramic micron powder is used for preparing Al by an aluminum oxide combustion synthesis quenching method2O3A method for preparing a mixture of amorphous and solid solution ceramic micropowder; wherein the rotating metal disc is an iron disc, a copper disc or a steel disc;
spraying the composite melt onto the rotating goldIn the disc, the radius of the rotating metal disc is 80cm, and the rotating speed is 90 r/min; spraying Al on one side of rotating metal disc2O3/ZrO2Spraying high-pressure and high-speed water flow to the other side of the composite melt for auxiliary cooling, wherein the water amount is 20L/min, the water pressure is 0.5MPa, and Al is formed on the surface of the rotating metal disc by solidification2O3/ZrO2Amorphous and solid solution films.
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