CN1072540C - 金属复合材料的制备方法 - Google Patents
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- 239000000843 powder Substances 0.000 claims abstract description 29
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 20
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical class [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052751 metal Inorganic materials 0.000 claims abstract description 8
- 239000002184 metal Substances 0.000 claims abstract description 8
- 125000000962 organic group Chemical group 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 239000012298 atmosphere Substances 0.000 claims abstract description 6
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 19
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 229910052719 titanium Inorganic materials 0.000 claims description 6
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 229910052721 tungsten Inorganic materials 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 229910052758 niobium Inorganic materials 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 229910052715 tantalum Inorganic materials 0.000 claims description 4
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- 238000007669 thermal treatment Methods 0.000 claims 2
- 210000005252 bulbus oculi Anatomy 0.000 claims 1
- -1 carboxylate salt Chemical class 0.000 claims 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 239000003960 organic solvent Substances 0.000 claims 1
- 229910002651 NO3 Inorganic materials 0.000 abstract description 4
- 150000003839 salts Chemical class 0.000 abstract description 4
- 230000008020 evaporation Effects 0.000 abstract description 3
- 125000000524 functional group Chemical group 0.000 abstract description 3
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 238000010561 standard procedure Methods 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 description 8
- 239000007789 gas Substances 0.000 description 5
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- ZBYYWKJVSFHYJL-UHFFFAOYSA-L cobalt(2+);diacetate;tetrahydrate Chemical compound O.O.O.O.[Co+2].CC([O-])=O.CC([O-])=O ZBYYWKJVSFHYJL-UHFFFAOYSA-L 0.000 description 2
- 238000010902 jet-milling Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 description 1
- PMVSDNDAUGGCCE-TYYBGVCCSA-L Ferrous fumarate Chemical group [Fe+2].[O-]C(=O)\C=C\C([O-])=O PMVSDNDAUGGCCE-TYYBGVCCSA-L 0.000 description 1
- 239000002262 Schiff base Substances 0.000 description 1
- 150000004753 Schiff bases Chemical class 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 150000007942 carboxylates Chemical class 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- QGUAJWGNOXCYJF-UHFFFAOYSA-N cobalt dinitrate hexahydrate Chemical compound O.O.O.O.O.O.[Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QGUAJWGNOXCYJF-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- ZYBWTEQKHIADDQ-UHFFFAOYSA-N ethanol;methanol Chemical compound OC.CCO ZYBWTEQKHIADDQ-UHFFFAOYSA-N 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000000935 solvent evaporation Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/18—Non-metallic particles coated with metal
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
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- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Powder Metallurgy (AREA)
Abstract
根据本发明的方法，将低碳含量或不含碳的Men(NO3)和Men(SO4)m以及其他类似的含有X-基团的Men-Xm化合物中的至少一种，优选为Me-硝酸盐，与一种或多种含有有机基团的至少一种铁族的金属盐溶解于至少一种极性溶剂中，并使其与至少一种含有OH或NR3(R＝H或烷基)官能基的配合物前体配位键合，将硬组分粉末加入所述溶液中，蒸发除去溶剂，将留下的粉末在惰性和/或弱还原气氛中热处理。结果得到一种涂覆的硬组分粉末，在加入成型剂后，可以按标准方法对其进行压实和烧结。
Description
本发明涉及一种制备金属复合材料，例如硬质合金的方法。
美国专利5,505,902披露了一种方法，该方法中，将含有有机基团的至少一种铁族金属的一种或多种金属盐溶于至少一种极性溶剂中并配位键合到至少一种含有OH或NR，(R＝H或烷基)官能基的配合物前体中。将硬组分粉末，以及选择性的可溶性碳源加入到该溶液中。蒸发除去溶剂并将剩下的粉末在情性和/或还原性气氛中进行热处理。结果得到涂覆的硬组分粉末，在加入成型剂后，可按标准方法进行压实和烧结，得到在粘结相中含有硬组分的烧结体。所述方法存在的一个问题是，将大量的(＞1千克)涂覆粉末进行热处理必须在纯氢气中和/或需要不必要的高的气体流速以得到所希望的碳含量，对于硬质合金，碳含量必须保持在一非常窄的范围内。
因此，本发明的目的是提供一种替代上述的美国专利的方法。该方法基本上不用进行氢气还原。
按照本发明方法，上述专利中所述的至少一种有机盐被一种不含或基本上不含碳的盐部分或全部替换。
本发明方法包括下述步骤，其中，Me＝Co、Ni和铁Fe，优选为Co：
1、将碳含量低于5％(重量)、优选为低于2％(重量)、特别优选是不含碳的Men(NO3)m和Men(SO4)m的至少一种，优选为Me-硝酸盐，与至少一种含有有机基团的Me-盐，例如羧酸盐、乙酰丙酮化物、含氮有机基团，例如席夫碱，优选是Me-乙酸盐，溶于至少一种极性溶剂，例如乙醇、乙腈、N，N-二甲基甲酰胺或二甲亚砜以及溶剂的混合物，例如甲醇一乙醇和水-1，2-乙二醇中，优选是甲醇中。以Me-盐的总量计，低碳含量或不含碳Me-盐的用量应大于10％，优选为大于50％。在搅拌下加入三乙醇胺或其他的配合物前体，特别是含有多于2个官能基，即OH或NR3的分子，其中R＝H或烷基(每摩尔金属0.1-2.0摩尔配合物前体，优选为每摩尔金属的0.5摩尔配合物前体)。
2、将硬组分粉末，例如WC、(Ti，W)C、(Ta，Nb)C、(Ti，Ta，Nb)C、(Ti，W)(C，N)，TiC、TaC、NbC、VC和Cr3C2，优选是良好解聚集的，例如喷射研磨过的硬组分粉末在中等搅拌下加入，并升温以加速溶剂的挥发。当混合物变得非常粘稠时，将面团状混合物捏合，并在几乎干燥时平稳粉碎以促进溶剂蒸发(避免存留下溶剂)。
3、将由上述步骤得到的松散的粉末块在情性和/或弱还原气氛中在约400-1100℃、优选是500-900℃进行热处理。为了得到完全还原的粉末，可能需要保温。热处理时间受工艺参数例如粉末床的厚度、批处理量、气体组成以及热处理温度的影响，其是通过实验来确定的。通常使用氮和/或氢，但是也可以使用氩、氦和氨(或其混合物)，由此可使组合物和涂覆层的微结构得到改善。
4、热处理后，将涂覆的粉末单独或与其他的涂覆的硬组分粉末和/或未涂覆的硬组分粉末和/或粘结相金属以及，如果可能的话，碳或钨与成型助剂在乙醇中混合以形成浆液，得到所希望的组合物。随后将浆液干燥，以常用的方式压实并烧结，得到硬组分在粘结相中的烧结体。
大部分的溶剂可以回收，这对于工业规模的生产来说是非常重要的。
另一种选择是，可在步骤2中将成型助剂与硬组分粉末一起加入，直接干燥、并按步骤3所述的条件压实和烧结。
实施例1
按照下述方式制备WC-6％ Co硬质合金粉末混合物：将72.36克硝酸钴六水合物(Co(NO3)2·6H2O)和62.26克乙酸钴四水合物(Co(C2H3O2)·4H2O)，硝酸盐/乙酸盐的比例为7/6，的混合物溶于800ml甲醇中。搅拌下加入36.1ml三乙醇胺((C2H5O)3N)(0.5摩尔TEA/摩尔Co))。随后加入500克喷射研磨的WC粉末，并将温度升至70℃，在甲醇的蒸发过程中连续细心地搅拌，直至混合物变得非常粘稠。当其几乎变干时，将面团状的混合物在轻微的压力下处理和粉碎。
将得到的粉末在约1厘米厚的多孔床烧结炉中以不同的批处理量和在不同的流动气氛下进行烧结(气体流速：2000l/h)，以10℃/分钟的升温速度加热到700℃，保温时间：3小时，冷却速率为10℃/分钟。
分析各批量粉末的钴和碳含量，热处理的结果总结如下：批处理 批处理量 气体混合物 粉末分析 wt％序号 (kg) (N2/H2) Co 总碳量*1 0.2 N2(100％) 5.4 6.642 0.2 N2(75％)/H2(25％) 5.4 5.793 3.0 N2(75％)/H2(25％) 5.4 5.79
*化学计量碳含量为5.79％(重量)。
进行了对比批处理，热处理是以与以上所述相同的方式进行，只是将上述的硝酸盐/乙酸盐混合物用134.89克乙酸钴四水合物(Co(C2H3O2)2·4H2O)替代。分析对比粉末中的钴和碳含量，热处理结果总结如下：批处理 批处理量 气体混合物 粉末分析 wt％序号 (kg) (N2/H2) Co 总碳量*4 0.2 N2(100％) 5.4 6.645 0.2 N2(75％)/H2(25％) 5.4 5.796 3.0 N2(75％)/H2(25％) 5.4 5.79*化学计量碳含量为5.79％(重量)。
Claims (11)
1、一种制备涂覆有至少一种铁族金属Me的硬组分粉末的方法，其特征在于，该方法包括下述步骤：
——将低碳含量或不含碳的Men(NO3)m和Men(SO4)m中的至少一种，与至少一种含有有机基团的Me-盐溶解于至少一种极性溶剂中，并使其与至少一种含有OH或NR3官能基的配合物前体配位键合而形成一种溶液，其中，R＝H或烷基，Me＝Co、Ni和铁Fe，且以Me-盐的总量计，所述的低碳含量或不含碳的Me-盐的用量大于10％
——将硬组分粉末加入上述溶液中，
——通过蒸发溶剂回收上述粉末，
——在惰性和/或弱还原气氛中对上述粉末进行热处理以得到所述的涂覆有至少一种铁族金属的硬组分粉末。
2、权利要求1的方法，其特征在于，所述的低碳含量或不含碳的Me-盐的用量大于50％。
3、权利要求1的方法，其特征在于，所述的低碳含量或不含碳的Me-盐含有低于5％(重量)的碳。
4、权利要求3的方法，其特征在于，所述的低碳含量或不含碳的Me-盐含有低于2％(重量)的碳。
5、权利要求1的方法，其特征在于，所述的有机溶剂包括：甲醇、乙醇、乙睛、N，N-二甲基甲酰胺或二甲亚砜或这些溶剂的混合物。
6、权利要求1的方法，其特征在于，所述的硬组分粉末包括WC、(Ti，W)C、(Ta，Nb)C、(Ti，Ta，Nb)C、(Ti，W)(C，N)，TiC、TaC、NbC、VC和Cr3C2或它们的组合。
7、权利要求1的方法，其特征在于，所述的热处理是在400-1100℃下进行的。
8、权利要求7的方法，其特征在于，所述的热处理是在500-900℃下进行的。
9、权利要求1的方法，其特征在于，所述的热处理气氛包括：氮、氢、氛、氦，氨或它们的混合物。
10、权利要求1的方法，其特征在于，所述含有有机基团的Me-盐是羧酸盐。
11、权利要求10的方法，其特征在于，所述含有有机基团的Me-盐是Me-乙酸盐
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SE9503419-5 | 1995-09-29 | ||
| SE9503419A SE507211C2 (sv) | 1995-09-29 | 1995-09-29 | Sätt att tillverka ett belagt hårdämnespulver |
| US08/721,766 US5887242A (en) | 1995-09-29 | 1996-09-25 | Method of making metal composite materials |
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| Publication Number | Publication Date |
|---|---|
| CN1198115A CN1198115A (zh) | 1998-11-04 |
| CN1072540C true CN1072540C (zh) | 2001-10-10 |
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| CN96197309A Expired - Fee Related CN1072540C (zh) | 1995-09-29 | 1996-09-27 | 金属复合材料的制备方法 |
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| Country | Link |
|---|---|
| US (1) | US5887242A (zh) |
| EP (1) | EP0852526B1 (zh) |
| CN (1) | CN1072540C (zh) |
| SE (1) | SE507211C2 (zh) |
| WO (1) | WO1997011804A1 (zh) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SE510659C2 (sv) * | 1997-10-14 | 1999-06-14 | Sandvik Ab | Sätt att framställa en hårdmetall innefattande beläggning av partiklar av hårdämnet med bindemetall |
| SE510749C2 (sv) * | 1997-12-22 | 1999-06-21 | Sandvik Ab | Sätt att framställa ett metallkompositmaterial innehållande hårda partiklar och bindemetall |
| US6179894B1 (en) * | 1999-11-29 | 2001-01-30 | Delphi Technologies, Inc. | Method of improving compressibility of a powder and articles formed thereby |
| US20030097907A1 (en) * | 2001-11-28 | 2003-05-29 | Carroll Daniel F. | Methods of producing composite powders |
| GB2399824A (en) * | 2002-09-21 | 2004-09-29 | Univ Birmingham | Metal coated metallurgical particles |
| EP3309269A1 (en) * | 2005-10-11 | 2018-04-18 | Baker Hughes Incorporated | Hard metal composite material for enhancing the durability of earth-boring and method for making it |
| CN102296197A (zh) * | 2011-08-12 | 2011-12-28 | 成都西顿硬质合金有限公司 | 硬质合金石蜡工艺的控碳方法 |
| CN110616344B (zh) * | 2018-06-19 | 2020-07-17 | 中国科学院苏州纳米技术与纳米仿生研究所 | 采用纳米尺度晶粒抑制剂碳化钒制备超细硬质合金的方法 |
| CN116043088B (zh) * | 2023-01-17 | 2024-10-01 | 株洲硬质合金集团有限公司 | 一种碳化物复合粉前驱体及其制备方法与应用 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4233063A (en) * | 1979-05-14 | 1980-11-11 | Gte Products Corporation | Process for producing cobalt powder |
| JPS62192501A (ja) * | 1986-02-18 | 1987-08-24 | Mitsubishi Metal Corp | Ｃｏ―Ｗ被覆ＷＣ粉末およびその製造方法 |
| JPS6369901A (ja) * | 1986-09-09 | 1988-03-30 | Daido Steel Co Ltd | 焼結用複合粉末及びその製造法 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SE504244C2 (sv) * | 1994-03-29 | 1996-12-16 | Sandvik Ab | Sätt att tillverka kompositmaterial av hårdämnen i en metallbindefas |
-
1995
- 1995-09-29 SE SE9503419A patent/SE507211C2/sv not_active IP Right Cessation
-
1996
- 1996-09-25 US US08/721,766 patent/US5887242A/en not_active Expired - Fee Related
- 1996-09-27 WO PCT/SE1996/001213 patent/WO1997011804A1/en active IP Right Grant
- 1996-09-27 CN CN96197309A patent/CN1072540C/zh not_active Expired - Fee Related
- 1996-09-27 EP EP96932913A patent/EP0852526B1/en not_active Expired - Lifetime
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4233063A (en) * | 1979-05-14 | 1980-11-11 | Gte Products Corporation | Process for producing cobalt powder |
| JPS62192501A (ja) * | 1986-02-18 | 1987-08-24 | Mitsubishi Metal Corp | Ｃｏ―Ｗ被覆ＷＣ粉末およびその製造方法 |
| JPS6369901A (ja) * | 1986-09-09 | 1988-03-30 | Daido Steel Co Ltd | 焼結用複合粉末及びその製造法 |
Also Published As
| Publication number | Publication date |
|---|---|
| EP0852526B1 (en) | 2000-03-08 |
| WO1997011804A1 (en) | 1997-04-03 |
| US5887242A (en) | 1999-03-23 |
| EP0852526A1 (en) | 1998-07-15 |
| CN1198115A (zh) | 1998-11-04 |
| SE9503419D0 (sv) | 1995-09-29 |
| SE9503419L (sv) | 1997-03-30 |
| SE507211C2 (sv) | 1998-04-27 |
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