CN106128758B - A kind of modified form semiconductor ceramic capacitor material and preparation method thereof - Google Patents
A kind of modified form semiconductor ceramic capacitor material and preparation method thereof Download PDFInfo
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- CN106128758B CN106128758B CN201610410609.5A CN201610410609A CN106128758B CN 106128758 B CN106128758 B CN 106128758B CN 201610410609 A CN201610410609 A CN 201610410609A CN 106128758 B CN106128758 B CN 106128758B
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- 239000003985 ceramic capacitor Substances 0.000 title claims abstract description 35
- 239000000463 material Substances 0.000 title claims abstract description 35
- 239000004065 semiconductor Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 36
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims abstract description 36
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 34
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000000919 ceramic Substances 0.000 claims abstract description 21
- 229910000480 nickel oxide Inorganic materials 0.000 claims abstract description 19
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 19
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 19
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910002115 bismuth titanate Inorganic materials 0.000 claims abstract description 18
- 239000003365 glass fiber Substances 0.000 claims abstract description 18
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 18
- 229910002113 barium titanate Inorganic materials 0.000 claims abstract description 17
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 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 abstract description 17
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 17
- XEPNJJFNSJKTSO-UHFFFAOYSA-N azanium;zinc;chloride Chemical compound [NH4+].[Cl-].[Zn] XEPNJJFNSJKTSO-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000011787 zinc oxide Substances 0.000 claims abstract description 15
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 8
- 239000003398 denaturant Substances 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims description 24
- 238000004925 denaturation Methods 0.000 claims description 19
- 230000036425 denaturation Effects 0.000 claims description 19
- 239000012190 activator Substances 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 11
- 239000012298 atmosphere Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 238000000967 suction filtration Methods 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- ONIKNECPXCLUHT-UHFFFAOYSA-N 2-chlorobenzoyl chloride Chemical compound ClC(=O)C1=CC=CC=C1Cl ONIKNECPXCLUHT-UHFFFAOYSA-N 0.000 claims description 8
- 230000000694 effects Effects 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 230000035484 reaction time Effects 0.000 claims description 8
- KXDAEFPNCMNJSK-UHFFFAOYSA-N Benzamide Chemical compound NC(=O)C1=CC=CC=C1 KXDAEFPNCMNJSK-UHFFFAOYSA-N 0.000 claims description 6
- 239000004793 Polystyrene Substances 0.000 claims description 6
- 229920000058 polyacrylate Polymers 0.000 claims description 6
- 229920002223 polystyrene Polymers 0.000 claims description 6
- 229920002689 polyvinyl acetate Polymers 0.000 claims description 4
- 239000011118 polyvinyl acetate Substances 0.000 claims description 4
- 239000011347 resin Substances 0.000 claims description 4
- 229920005989 resin Polymers 0.000 claims description 4
- FDDDEECHVMSUSB-UHFFFAOYSA-N sulfanilamide Chemical compound NC1=CC=C(S(N)(=O)=O)C=C1 FDDDEECHVMSUSB-UHFFFAOYSA-N 0.000 claims description 3
- LMYRWZFENFIFIT-UHFFFAOYSA-N toluene-4-sulfonamide Chemical compound CC1=CC=C(S(N)(=O)=O)C=C1 LMYRWZFENFIFIT-UHFFFAOYSA-N 0.000 claims description 3
- -1 Lauxite Polymers 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims 1
- 229910052797 bismuth Inorganic materials 0.000 claims 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims 1
- 239000010936 titanium Substances 0.000 claims 1
- 229910052719 titanium Inorganic materials 0.000 claims 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical group O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 12
- 239000003990 capacitor Substances 0.000 description 8
- 238000011056 performance test Methods 0.000 description 7
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 6
- 239000001569 carbon dioxide Substances 0.000 description 6
- 229910002092 carbon dioxide Inorganic materials 0.000 description 6
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 5
- 239000002253 acid Substances 0.000 description 5
- 239000001099 ammonium carbonate Substances 0.000 description 5
- 235000012501 ammonium carbonate Nutrition 0.000 description 5
- ITHZDDVSAWDQPZ-UHFFFAOYSA-L barium acetate Chemical compound [Ba+2].CC([O-])=O.CC([O-])=O ITHZDDVSAWDQPZ-UHFFFAOYSA-L 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 238000002604 ultrasonography Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- NSEQHAPSDIEVCD-UHFFFAOYSA-N N.[Zn+2] Chemical compound N.[Zn+2] NSEQHAPSDIEVCD-UHFFFAOYSA-N 0.000 description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 3
- PTXMVOUNAHFTFC-UHFFFAOYSA-N alumane;vanadium Chemical compound [AlH3].[V] PTXMVOUNAHFTFC-UHFFFAOYSA-N 0.000 description 3
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 239000011591 potassium Substances 0.000 description 3
- 229910052700 potassium Inorganic materials 0.000 description 3
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical compound CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- QQEXMHVHLWKOQT-UHFFFAOYSA-N benzene;formamide Chemical compound NC=O.C1=CC=CC=C1 QQEXMHVHLWKOQT-UHFFFAOYSA-N 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- YAZSBRQTAHVVGE-UHFFFAOYSA-N 2-aminobenzenesulfonamide Chemical compound NC1=CC=CC=C1S(N)(=O)=O YAZSBRQTAHVVGE-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- UBXWAYGQRZFPGU-UHFFFAOYSA-N manganese(2+) oxygen(2-) titanium(4+) Chemical compound [O--].[O--].[Ti+4].[Mn++] UBXWAYGQRZFPGU-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- UFWIBTONFRDIAS-UHFFFAOYSA-N naphthalene-acid Natural products C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 1
- 210000003739 neck Anatomy 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/06—Solid dielectrics
- H01G4/08—Inorganic dielectrics
- H01G4/12—Ceramic dielectrics
- H01G4/1209—Ceramic dielectrics characterised by the ceramic dielectric material
- H01G4/1218—Ceramic dielectrics characterised by the ceramic dielectric material based on titanium oxides or titanates
- H01G4/1227—Ceramic dielectrics characterised by the ceramic dielectric material based on titanium oxides or titanates based on alkaline earth titanates
Landscapes
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Power Engineering (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses a kind of modified form semiconductor ceramic capacitor material, it is made from the following raw materials in parts by weight：12 26 parts of barium titanate, 5 17 parts of neodymia, 3 12 parts of titanium dioxide, 15 35 parts of nano-ceramic powder, 25 parts of glass fibre, 29 parts of silica, 3 12 parts of zinc oxide, 37 parts of strontium titanates, 26 parts of bismuth titanates, 25 parts of nickel oxide, 37 parts of manganese dioxide, 47 parts of zinc ammonium chloride, 7 13 parts of organic bond, 26 parts of denaturant, 38 parts of reducing agent.The modified form semiconductor ceramic capacitor material being prepared, its capacitance is big, and capacitive property is stable, has higher dielectric constant, small volume, can apply to high-performance, multifunction electronic product industry.Meanwhile also disclose the preparation method of this modified form semiconductor ceramic capacitor material.
Description
Technical field
The present invention relates to field of capacitor material technology, more particularly to a kind of modified form semiconductor ceramic capacitor material and
Its preparation method.
Background technology
With socialization and industrialized development, in order to solve the problems, such as that capacitor fails because moist, using ceramics as material
Material, ceramic disc capacitor simple in construction arise at the historic moment, the extensive use in low capacity circuit.Hereafter, differing dielectric constant, difference
Structure, the ceramic capacitor of difference in functionality occur in succession.Contemporary electronic technology develops towards high frequency direction, only ceramic capacitor
It could be played a role in the range of ability gigahertz frequencies above.Thermo-compensation capacitor can ensure the situation in variation of ambient temperature
Under, also can normal work.In recent years, for electronic component towards frivolous and miniaturization, the requirement to capacitor is then increase electricity
Capacitance of the container per unit volume, multilayer ceramic capacitor have adapted to the development of this trend with Large Copacity, small size.When
Modern ceramic capacitor either in terms of the quantity still potentiality in future development, has all occupied leading position.
In order to adapt to the demand for development of ceramic capacitor, tackle the requirement of industry, the development of ceramic capacitor be also required to
When all enter, keep up with the growth requirement of industry.Just seem particularly so developing the capacitor material closely bound up with capacitor
It is important.It is contemplated that studying a kind of modified form semiconductor ceramic capacitor material, the material for enabling to develop meets capacitor
The new demand of industry development, new standard, performance enhancement, stability are higher.
The content of the invention
In order to solve the above technical problems, the present invention provides a kind of modified form semiconductor ceramic capacitor material and its preparation side
Method, it is combined by using specified raw material, coordinates corresponding production technology, has obtained a kind of modified form semiconductive ceramic electric capacity
Equipment material, its capacitance is big, and capacitive property is stable, has a higher dielectric constant, small volume, can apply to high-performance, more
Function electronic product industry, there is preferable application prospect.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of modified form semiconductor ceramic capacitor material, is made from the following raw materials in parts by weight：Barium titanate 12-26 parts,
Neodymia 5-17 parts, titanium dioxide 3-12 parts, nano-ceramic powder 15-35 parts, glass fibre 2-5 parts, silica 2-9 parts, oxygen
Change zinc 3-12 parts, strontium titanates 3-7 parts, bismuth titanates 2-6 parts, nickel oxide 2-5 parts, manganese dioxide 3-7 parts, zinc ammonium chloride 4-7 parts, have
Machine adhesive 7-13 parts, denaturant 2-6 parts, reducing agent 3-8 parts.
Preferably, the organic bond is selected from polystyrene, polyvinyl acetate resin, Lauxite, polyacrylate
In one or more.
Preferably, the denaturant is selected from benzamide, P-aminobenzene-sulfonamide, N- ethyls para toluene sulfonamide, 1- naphthalenes
One or more in acetamide.
Preferably, one or more of the reducing agent in ammonium carbonate, potassium aluminium vanadium, ammonium persulfate, barium acetate.
The preparation method of described modified form semiconductor ceramic capacitor material, comprises the following steps：
（1）Each raw material is weighed according to parts by weight；
（2）By barium titanate, neodymia, titanium dioxide, nano-ceramic powder, glass fibre, silica, zinc oxide, metatitanic acid
In strontium, the chlorobenzoyl chloride solution of quality such as bismuth titanates mixing, addition, ultrasonic disperse effect is carried out, ultrasonic time 2-5 hours, is surpassed
Acoustical power 200-500W, obtains pre-blended mixture；
（3）Pre-blended mixture is injected in autoclave, and sequentially adds nickel oxide, manganese dioxide, zinc ammonium chloride, change
Property agent, the pressure of autoclave is 10-16MPa, and the reaction time is 30-60 minutes, and the mixture of acquisition is denaturation activator；
（4）Obtained denaturation activator is put into banbury, organic bond, reducing agent are added, in reducibility gas
90-120 minutes, rotating speed 1000-1200r/min are kneaded in atmosphere, reaction temperature is 800-1000 DEG C, is subsequently cooled to 200-
300 DEG C, obtained mixed liquor is finished product stoste；
（5）Above-mentioned finished product stoste is injected in suction filtration machine and filtered；
（6）The liquid filtered out, which is directly injected into screw extruder, to be melted, extrudes, plastotype, is got product.
Preferably, the step（4）In, reducibility gas atmosphere is carbon dioxide atmosphere.
Preferably, the step（5）In, the aperture for filtering machine is 10-20 μm.
Preferably, the step（6）In, the screw speed of screw extruder is 1000-1200 r/min, barrel temperature
200-300℃。
Compared with prior art, its advantage is the present invention：
（1）The modified form semiconductor ceramic capacitor material of the present invention is made pottery with barium titanate, neodymia, titanium dioxide, nanometer
Porcelain powder, glass fibre, silica, zinc oxide, strontium titanates, bismuth titanates are main component, by adding nickel oxide, titanium dioxide
Manganese, zinc ammonium chloride, denaturant, organic bond, reducing agent, it is aided with Ultrasonic Pulverization, high pressure denaturation, high temperature banburying, suction filtration, molten
Melt, extrude, the technique such as plastotype so that the modified form semiconductor ceramic capacitor material being prepared, its capacitance is big, capacitive character
Can be stable, there is higher dielectric constant, small volume, can apply to high-performance, multifunction electronic product industry, have preferable
Application prospect.
（2）Modified form semiconductor ceramic capacitor material feedstock of the invention is cheap, technique is simple, suitable for large-scale industry
Change and use, it is practical.
Embodiment
The technical scheme of invention is described in detail with reference to specific embodiment.
Embodiment 1
（1）12 parts of barium titanate, neodymia 5,3 parts of titanium dioxide, 15 parts of nano-ceramic powder, glass fibers are weighed according to parts by weight
2 parts of dimension, 2 parts of silica, 3 parts of zinc oxide, 3 parts of strontium titanates, 2 parts of bismuth titanates, 2 parts of nickel oxide, 3 parts of manganese dioxide, zinc chloride
4 parts of ammonium, 7 parts of polystyrene, 2 parts of benzamide, 3 parts of ammonium carbonate；
（2）By barium titanate, neodymia, titanium dioxide, nano-ceramic powder, glass fibre, silica, zinc oxide, metatitanic acid
In strontium, the chlorobenzoyl chloride solution of quality such as bismuth titanates mixing, addition, ultrasonic disperse effect, ultrasonic time 2 hours, ultrasound are carried out
Power 200W, obtains pre-blended mixture；
（3）Pre-blended mixture is injected in autoclave, and sequentially adds nickel oxide, manganese dioxide, zinc ammonium chloride, benzene
Formamide, the pressure of autoclave is 10MPa, and the reaction time is 30 minutes, and the mixture of acquisition is denaturation activator；
（4）Obtained denaturation activator is put into banbury, polystyrene, ammonium carbonate are added, in carbon dioxide
It is kneaded 90 minutes, rotating speed 1000r/min in atmosphere, reaction temperature is 800 DEG C, is subsequently cooled to 200 DEG C, obtained mixed liquor is
Finished product stoste；
（5）Above-mentioned finished product stoste is injected in suction filtration machine and filtered, the aperture for filtering machine is 10 μm；
（6）The liquid filtered out, which is directly injected into screw extruder, to be melted, extrudes, plastotype, is got product, screw extruder
Screw speed be 1000r/min, 200 DEG C of barrel temperature.
The performance test results of obtained modified form semiconductor ceramic capacitor material are as shown in table 1.
Embodiment 2
（1）17 parts of barium titanate, 9 parts of neodymia, 7 parts of titanium dioxide, 22 parts of nano-ceramic powder, glass are weighed according to parts by weight
3 parts of fiber, 4 parts of silica, 5 parts of zinc oxide, 4 parts of strontium titanates, 3 parts of bismuth titanates, 3 parts of nickel oxide, 4 parts of manganese dioxide, chlorination
5 parts of zinc ammonium, 9 parts of polyvinyl acetate resin, 3 parts of P-aminobenzene-sulfonamide, 5 parts of potassium aluminium vanadium；
（2）By barium titanate, neodymia, titanium dioxide, nano-ceramic powder, glass fibre, silica, zinc oxide, metatitanic acid
In strontium, the chlorobenzoyl chloride solution of quality such as bismuth titanates mixing, addition, ultrasonic disperse effect, ultrasonic time 3 hours, ultrasound are carried out
Power 300W, obtains pre-blended mixture；
（3）Pre-blended mixture is injected in autoclave, and sequentially adds nickel oxide, manganese dioxide, zinc ammonium chloride, right
Aminobenzene sulfonamide, the pressure of autoclave is 12MPa, and the reaction time is 40 minutes, and the mixture of acquisition activates for denaturation
Thing；
（4）Obtained denaturation activator is put into banbury, polyvinyl acetate resin, potassium aluminium vanadium are added, in titanium dioxide
It is kneaded 100 minutes, rotating speed 1050r/min in carbon atmosphere, reaction temperature is 900 DEG C, is subsequently cooled to 220 DEG C, obtains
Mixed liquor is finished product stoste；
（5）Above-mentioned finished product stoste is injected in suction filtration machine and filtered, the aperture for filtering machine is 12 μm；
（6）The liquid filtered out, which is directly injected into screw extruder, to be melted, extrudes, plastotype, is got product, screw extruder
Screw speed be 1050r/min, 220 DEG C of barrel temperature.
The performance test results of obtained modified form semiconductor ceramic capacitor material are as shown in table 1.
Embodiment 3
（1）21 parts of barium titanate, 13 parts of neodymia, 10 parts of titanium dioxide, 30 parts of nano-ceramic powder, glass are weighed according to parts by weight
4 parts of glass fiber, 7 parts of silica, 11 parts of zinc oxide, 6 parts of strontium titanates, 5 parts of bismuth titanates, 4 parts of nickel oxide, 6 parts of manganese dioxide, chlorine
Change 6 parts of zinc ammonium, 10 parts of Lauxite, 5 parts of N- ethyls para toluene sulfonamide, 7 parts of ammonium persulfate；
（2）By barium titanate, neodymia, titanium dioxide, nano-ceramic powder, glass fibre, silica, zinc oxide, metatitanic acid
In strontium, the chlorobenzoyl chloride solution of quality such as bismuth titanates mixing, addition, ultrasonic disperse effect, ultrasonic time 4 hours, ultrasound are carried out
Power 400W, obtains pre-blended mixture；
（3）Pre-blended mixture is injected in autoclave, and sequentially adds nickel oxide, manganese dioxide, zinc ammonium chloride, N-
Ethyl para toluene sulfonamide, the pressure of autoclave is 14MPa, and the reaction time is 50 minutes, and the mixture of acquisition is denaturation
Activator；
（4）Obtained denaturation activator is put into banbury, Lauxite, ammonium persulfate are added, in carbon dioxide gas
It is kneaded 110 minutes, rotating speed 1100r/min in body atmosphere, reaction temperature is 950 DEG C, is subsequently cooled to 260 DEG C, obtained mixing
Liquid is finished product stoste；
（5）Above-mentioned finished product stoste is injected in suction filtration machine and filtered, the aperture for filtering machine is 18 μm；
（6）The liquid filtered out, which is directly injected into screw extruder, to be melted, extrudes, plastotype, is got product, screw extruder
Screw speed be 1100 r/min, 260 DEG C of barrel temperature.
The performance test results of obtained modified form semiconductor ceramic capacitor material are as shown in table 1.
Embodiment 4
（1）26 parts of barium titanate, 17 parts of neodymia, 12 parts of titanium dioxide, 35 parts of nano-ceramic powder, glass are weighed according to parts by weight
5 parts of glass fiber, 9 parts of silica, 12 parts of zinc oxide, 7 parts of strontium titanates, 6 parts of bismuth titanates, 5 parts of nickel oxide, 7 parts of manganese dioxide, chlorine
Change 7 parts of zinc ammonium, 13 parts of polyacrylate, 6 parts of 1- NADs, 8 parts of barium acetate；
（2）By barium titanate, neodymia, titanium dioxide, nano-ceramic powder, glass fibre, silica, zinc oxide, metatitanic acid
In strontium, the chlorobenzoyl chloride solution of quality such as bismuth titanates mixing, addition, ultrasonic disperse effect, ultrasonic time 5 hours, ultrasound are carried out
Power 500W, obtains pre-blended mixture；
（3）Pre-blended mixture is injected in autoclave, and sequentially adds nickel oxide, manganese dioxide, zinc ammonium chloride, 1-
NAD, the pressure of autoclave is 16MPa, and the reaction time is 60 minutes, and the mixture of acquisition is denaturation activator；
（4）Obtained denaturation activator is put into banbury, polyacrylate, barium acetate are added, in carbon dioxide gas
It is kneaded 120 minutes, rotating speed 1200r/min in body atmosphere, reaction temperature is 1000 DEG C, is subsequently cooled to 300 DEG C, obtained mixing
Liquid is finished product stoste；
（5）Above-mentioned finished product stoste is injected in suction filtration machine and filtered, the aperture for filtering machine is 20 μm；
（6）The liquid filtered out, which is directly injected into screw extruder, to be melted, extrudes, plastotype, is got product, screw extruder
Screw speed be 1200 r/min, 300 DEG C of barrel temperature.
The performance test results of obtained modified form semiconductor ceramic capacitor material are as shown in table 1.
Comparative example 1
（1）12 parts of barium titanate, 15 parts of nano-ceramic powder, 2 parts of glass fibre, 2 parts of silica, oxygen are weighed according to parts by weight
Change 3 parts of zinc, 3 parts of strontium titanates, 2 parts of bismuth titanates, 2 parts of nickel oxide, 3 parts of manganese dioxide, 4 parts of zinc ammonium chloride, 7 parts of polystyrene, benzene
2 parts of formamide, 3 parts of ammonium carbonate；
（2）Barium titanate, nano-ceramic powder, glass fibre, silica, zinc oxide, strontium titanates, bismuth titanates are mixed, added
Enter etc. in the chlorobenzoyl chloride solution of quality, carry out ultrasonic disperse effect, ultrasonic time 2 hours, ultrasonic power 200W, premixed
Mixture；
（3）Pre-blended mixture is injected in autoclave, and sequentially adds nickel oxide, manganese dioxide, zinc ammonium chloride, benzene
Formamide, the pressure of autoclave is 10MPa, and the reaction time is 30 minutes, and the mixture of acquisition is denaturation activator；
（4）Obtained denaturation activator is put into banbury, polystyrene, ammonium carbonate are added, in carbon dioxide
It is kneaded 90 minutes, rotating speed 1000r/min in atmosphere, reaction temperature is 800 DEG C, is subsequently cooled to 200 DEG C, obtained mixed liquor is
Finished product stoste；
（5）Above-mentioned finished product stoste is injected in suction filtration machine and filtered, the aperture for filtering machine is 10 μm；
（6）The liquid filtered out, which is directly injected into screw extruder, to be melted, extrudes, plastotype, is got product, screw extruder
Screw speed be 1000r/min, 200 DEG C of barrel temperature.
The performance test results of obtained modified form semiconductor ceramic capacitor material are as shown in table 1.
Comparative example 2
（1）According to parts by weight weigh 17 parts of neodymia, 12 parts of titanium dioxide, 35 parts of nano-ceramic powder, 5 parts of glass fibre,
7 parts of strontium titanates, 6 parts of bismuth titanates, 5 parts of nickel oxide, 7 parts of manganese dioxide, 7 parts of zinc ammonium chloride, 13 parts of polyacrylate, 1- naphthalene acetyl
6 parts of amine, 8 parts of barium acetate；
（2）Neodymia, titanium dioxide, nano-ceramic powder, glass fibre, strontium titanates, bismuth titanates are mixed, the quality such as addition
Chlorobenzoyl chloride solution in, carry out ultrasonic disperse effect, ultrasonic time 5 hours, ultrasonic power 500W, obtain pre-blended mixture；
（3）Pre-blended mixture is injected in autoclave, and sequentially adds nickel oxide, manganese dioxide, zinc ammonium chloride, 1-
NAD, the pressure of autoclave is 16MPa, and the reaction time is 60 minutes, and the mixture of acquisition is denaturation activator；
（4）Obtained denaturation activator is put into banbury, polyacrylate, barium acetate are added, in carbon dioxide gas
It is kneaded 120 minutes, rotating speed 1200r/min in body atmosphere, reaction temperature is 1000 DEG C, is subsequently cooled to 300 DEG C, obtained mixing
Liquid is finished product stoste；
（5）Above-mentioned finished product stoste is injected in suction filtration machine and filtered, the aperture for filtering machine is 20 μm；
（6）The liquid filtered out, which is directly injected into screw extruder, to be melted, extrudes, plastotype, is got product, screw extruder
Screw speed be 1200 r/min, 300 DEG C of barrel temperature.
The performance test results of obtained modified form semiconductor ceramic capacitor material are as shown in table 1.
By embodiment 1-4 and comparative example 1-2 modified form semiconductor ceramic capacitor material carry out respectively compressive resistance value,
Dielectric constant, dielectrical loss（Under 1MHz working alternating currents）, ratio resistance and than this several performance tests of tolerance.
Table 1
| Compressive resistance value（Kv/mm） | Dielectric constant（εr） | Dielectric loss（Under tan δ, 1MHz working alternating currents） | Ratio resistance（Ω.cm） | Compare tolerance（ΔC/C,%,-30℃-+85℃） | |
| Embodiment 1 | 49 | 2.1*106 | 4.3*10-3 | 7.8*1011 | -5.8++5.6 |
| Embodiment 2 | 51 | 2.5*106 | 5.0*10-3 | 7.9*1011 | -6.9-+6.1 |
| Embodiment 3 | 50 | 2.2*106 | 4.5*10-3 | 8.1*1011 | -5.3-+5.9 |
| Embodiment 4 | 52 | 2.3*106 | 4.8*10-3 | 8.3*1011 | -5.8-6.3 |
| Comparative example 1 | 16 | 5.7*103 | 7.5*10-2 | 7.1*108 | -11.9-+16.1 |
| Comparative example 2 | 17 | 4.3*103 | 6.9*10-2 | 6.3*108 | -11.8-16.3 |
The modified form semiconductor ceramic capacitor material of the present invention is with barium titanate, neodymia, titanium dioxide, nano ceramics
Powder, glass fibre, silica, zinc oxide, strontium titanates, bismuth titanates are main component, by add nickel oxide, manganese dioxide,
Zinc ammonium chloride, denaturant, organic bond, reducing agent, be aided with Ultrasonic Pulverization, high pressure denaturation, high temperature banburying, suction filtration, melting, squeeze
Go out, the technique such as plastotype so that the modified form semiconductor ceramic capacitor material being prepared, its capacitance is big, and capacitive property is steady
It is fixed, there is higher dielectric constant, small volume, can apply to high-performance, multifunction electronic product industry, preferably should have
Use prospect.Modified form semiconductor ceramic capacitor material feedstock of the invention is cheap, technique is simple, is transported suitable for heavy industrialization
With practical.
Embodiments of the invention are the foregoing is only, are not intended to limit the scope of the invention, it is every to utilize this hair
The equivalent structure or equivalent flow conversion that bright description is made, or directly or indirectly it is used in other related technology necks
Domain, it is included within the scope of the present invention.
Claims (6)
- A kind of 1. modified form semiconductor ceramic capacitor material, it is characterised in that：It is made from the following raw materials in parts by weight：Barium titanate 12-26 parts, neodymia 5-17 parts, titanium dioxide 3-12 parts, nano-ceramic powder 15-35 parts, glass fibre 2-5 parts, silica 2-9 parts, zinc oxide 3-12 parts, strontium titanates 3-7 parts, bismuth titanates 2-6 parts, nickel oxide 2-5 parts, manganese dioxide 3-7 parts, zinc ammonium chloride 4-7 parts, organic bond 7-13 parts, denaturant 2-6 parts, reducing agent 3-8 parts.
- 2. modified form semiconductor ceramic capacitor material according to claim 1, it is characterised in that：The organic bond One or more in polystyrene, polyvinyl acetate resin, Lauxite, polyacrylate.
- 3. modified form semiconductor ceramic capacitor material according to claim 1, it is characterised in that：The denaturant is selected from One or more in benzamide, P-aminobenzene-sulfonamide, N- ethyls para toluene sulfonamide, 1- NADs.
- 4. according to the preparation method of any described modified form semiconductor ceramic capacitor materials of claim 1-3, its feature exists In comprising the following steps：（1）Each raw material is weighed according to parts by weight；（2）By barium titanate, neodymia, titanium dioxide, nano-ceramic powder, glass fibre, silica, zinc oxide, strontium titanates, titanium In the chlorobenzoyl chloride solution of quality such as sour bismuth mixing, addition, ultrasonic disperse effect, ultrasonic time 2-5 hours, ultrasonic power are carried out 200-500W, obtain pre-blended mixture；（3）Pre-blended mixture is injected in autoclave, and sequentially adds nickel oxide, manganese dioxide, zinc ammonium chloride, denaturation Agent, the pressure of autoclave is 10-16MPa, and the reaction time is 30-60 minutes, and the mixture of acquisition is denaturation activator；（4）Obtained denaturation activator is put into banbury, organic bond, reducing agent are added, in reducibility gas atmosphere Middle mixing 90-120 minutes, rotating speed 1000-1200r/min, reaction temperature are 800-1000 DEG C, are subsequently cooled to 200-300 DEG C, Obtained mixed liquor is finished product stoste；（5）Above-mentioned finished product stoste is injected in suction filtration machine and filtered；（6）The liquid filtered out, which is directly injected into screw extruder, to be melted, extrudes, plastotype, is got product.
- 5. the preparation method of modified form semiconductor ceramic capacitor material according to claim 4, it is characterised in that described Step（5）In, the aperture for filtering machine is 10-20 μm.
- 6. the preparation method of modified form semiconductor ceramic capacitor material according to claim 4, it is characterised in that described Step（6）In, the screw speed of screw extruder is 1000-1200 r/min, 200-300 DEG C of barrel temperature.
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|---|---|---|---|---|
| GB2219287A (en) * | 1988-06-03 | 1989-12-06 | Nippon Oils & Fats Co Ltd | Ceramic composition for reduction-reoxidation type semiconductive capacitor |
| CN1249286A (en) * | 1998-09-28 | 2000-04-05 | 株式会社村田制作所 | Dielectric ceramic composition and stacked ceramic capacitor |
| CN101182201A (en) * | 2007-11-27 | 2008-05-21 | 清华大学 | Preparation of Dielectric Materials for Base Metal Internal Electrode Multilayer Ceramic Chip Capacitors by Nano-doping |
| CN101814371A (en) * | 2009-02-25 | 2010-08-25 | 株式会社村田制作所 | Laminated ceramic capacitor |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2219287A (en) * | 1988-06-03 | 1989-12-06 | Nippon Oils & Fats Co Ltd | Ceramic composition for reduction-reoxidation type semiconductive capacitor |
| CN1249286A (en) * | 1998-09-28 | 2000-04-05 | 株式会社村田制作所 | Dielectric ceramic composition and stacked ceramic capacitor |
| CN101182201A (en) * | 2007-11-27 | 2008-05-21 | 清华大学 | Preparation of Dielectric Materials for Base Metal Internal Electrode Multilayer Ceramic Chip Capacitors by Nano-doping |
| CN101814371A (en) * | 2009-02-25 | 2010-08-25 | 株式会社村田制作所 | Laminated ceramic capacitor |
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