CN102821892B - 粉末冶金用润滑剂以及金属粉末组合物 - Google Patents
粉末冶金用润滑剂以及金属粉末组合物 Download PDFInfo
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- CN102821892B CN102821892B CN201180016623.2A CN201180016623A CN102821892B CN 102821892 B CN102821892 B CN 102821892B CN 201180016623 A CN201180016623 A CN 201180016623A CN 102821892 B CN102821892 B CN 102821892B
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- powder metallurgy
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- metal
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- 229910052751 metal Inorganic materials 0.000 title claims description 15
- 239000002184 metal Substances 0.000 title claims description 15
- 125000003118 aryl group Chemical group 0.000 claims abstract description 9
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 6
- 125000000304 alkynyl group Chemical group 0.000 claims abstract description 4
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 14
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 7
- 239000000428 dust Substances 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
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- FHUODBDRWMIBQP-UHFFFAOYSA-N Ethyl p-anisate Chemical compound CCOC(=O)C1=CC=C(OC)C=C1 FHUODBDRWMIBQP-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 229940126214 compound 3 Drugs 0.000 description 2
- 229940125898 compound 5 Drugs 0.000 description 2
- IPIVAXLHTVNRBS-UHFFFAOYSA-N decanoyl chloride Chemical compound CCCCCCCCCC(Cl)=O IPIVAXLHTVNRBS-UHFFFAOYSA-N 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
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- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 2
- VKOBVWXKNCXXDE-UHFFFAOYSA-N icosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCC(O)=O VKOBVWXKNCXXDE-UHFFFAOYSA-N 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
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- RKISUIUJZGSLEV-UHFFFAOYSA-N n-[2-(octadecanoylamino)ethyl]octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NCCNC(=O)CCCCCCCCCCCCCCCCC RKISUIUJZGSLEV-UHFFFAOYSA-N 0.000 description 2
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 description 2
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- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 2
- ALSTYHKOOCGGFT-KTKRTIGZSA-N (9Z)-octadecen-1-ol Chemical compound CCCCCCCC\C=C/CCCCCCCCO ALSTYHKOOCGGFT-KTKRTIGZSA-N 0.000 description 1
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- WSULSMOGMLRGKU-UHFFFAOYSA-N 1-bromooctadecane Chemical compound CCCCCCCCCCCCCCCCCCBr WSULSMOGMLRGKU-UHFFFAOYSA-N 0.000 description 1
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- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- QTMHHQFADWIZCP-UHFFFAOYSA-N 4-decanoyloxybenzoic acid Chemical compound CCCCCCCCCC(=O)OC1=CC=C(C(O)=O)C=C1 QTMHHQFADWIZCP-UHFFFAOYSA-N 0.000 description 1
- HBQUXMZZODHFMJ-UHFFFAOYSA-N 4-hexoxybenzoic acid Chemical compound CCCCCCOC1=CC=C(C(O)=O)C=C1 HBQUXMZZODHFMJ-UHFFFAOYSA-N 0.000 description 1
- FJKROLUGYXJWQN-UHFFFAOYSA-N 4-hydroxybenzoic acid Chemical compound OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
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- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
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- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- HGPXWXLYXNVULB-UHFFFAOYSA-M lithium stearate Chemical compound [Li+].CCCCCCCCCCCCCCCCCC([O-])=O HGPXWXLYXNVULB-UHFFFAOYSA-M 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
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- BVWTXUYLKBHMOX-UHFFFAOYSA-N methyl vanillate Chemical group COC(=O)C1=CC=C(O)C(OC)=C1 BVWTXUYLKBHMOX-UHFFFAOYSA-N 0.000 description 1
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- GTDHYNXLIKNVTJ-UHFFFAOYSA-N n-(1-hydroxy-2-methylpropan-2-yl)octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NC(C)(C)CO GTDHYNXLIKNVTJ-UHFFFAOYSA-N 0.000 description 1
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- FATBGEAMYMYZAF-KTKRTIGZSA-N oleamide Chemical compound CCCCCCCC\C=C/CCCCCCCC(N)=O FATBGEAMYMYZAF-KTKRTIGZSA-N 0.000 description 1
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- 229910052698 phosphorus Inorganic materials 0.000 description 1
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- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 1
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- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 1
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- 238000001556 precipitation Methods 0.000 description 1
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- 102200082816 rs34868397 Human genes 0.000 description 1
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- 238000003756 stirring Methods 0.000 description 1
- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 description 1
- 238000002076 thermal analysis method Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M129/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen
- C10M129/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen having a carbon chain of less than 30 atoms
- C10M129/26—Carboxylic acids; Salts thereof
- C10M129/48—Carboxylic acids; Salts thereof having carboxyl groups bound to a carbon atom of a six-membered aromatic ring
- C10M129/50—Carboxylic acids; Salts thereof having carboxyl groups bound to a carbon atom of a six-membered aromatic ring monocarboxylic
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
- C10M105/08—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen
- C10M105/22—Carboxylic acids or their salts
- C10M105/24—Carboxylic acids or their salts having only one carboxyl group bound to an acyclic carbon atom, cycloaliphatic carbon atom or hydrogen
-
- 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
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/103—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing an organic binding agent comprising a mixture of, or obtained by reaction of, two or more components other than a solvent or a lubricating agent
-
- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
- C10M105/08—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen
- C10M105/22—Carboxylic acids or their salts
- C10M105/28—Carboxylic acids or their salts having only one carboxyl group bound to a carbon atom of a six-membered aromatic ring
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
- C10M105/08—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen
- C10M105/22—Carboxylic acids or their salts
- C10M105/30—Carboxylic acids or their salts having more than one carboxyl group bound to a carbon atom of a six-membered aromatic ring
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
- C10M105/08—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen
- C10M105/32—Esters
- C10M105/40—Esters containing free hydroxy or carboxyl groups
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
- C10M125/02—Carbon; Graphite
-
- C—CHEMISTRY; METALLURGY
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Abstract
本发明的粉末冶金用润滑剂,配合由下述式(1)表示的芳香族羧酸而形成:(Z)n-Ar-COOH (1) (式中,Ar为芳基,Z为直接键合于所述芳基的取代基,且为R、OR、OCOR及COOR中的任一种。R为烷基、烯基及炔基中的任一种。n为1~4的整数。在n为2以上的情况下,Z彼此可以相同也可以不同)。
Description
技术领域
本发明涉及粉末冶金用润滑剂以及配合其而形成的金属粉末组合物。
背景技术
作为制造金属部件的技术,粉末冶金是已知的。在粉末冶金中,可以不进行切削,而以高精度高速且大量的生产复杂形状的金属部件。此外还可以仅通过改变金属粉的组成来制造各种组成的合金,因而期待应用于各种领域。
在这种粉末冶金中,在主原料粉末中添加混合合金成分或石墨等的粉末作为用于改善烧结体的物性(强度特性或加工特性)的成分,并进行压缩成型形成压粉体,接着将压粉体进行烧结而制成产品烧结体。这时,为了降低粉末相互之间以及粉末与模具之间的摩擦,从而使粉末的压缩性及脱模性良好,一般在上述的金属粉末中混合硬脂酸锌粉、硬脂酸锂粉及亚乙基双硬脂酰胺粉等成型用润滑剂(例如,参照专利文献1)。
现有技术文献
专利文献
专利文献1:日本特开平11-193404号公报。
发明内容
发明要解决的课题
但是,就使用专利文献1等现有技术中公开的润滑剂的金属粉末而言,从模具的脱模性不充分。另外,由于在重复进行粉末冶金中烧结炉发生污染,因此定期的烧结炉清扫也是必要的。所以,难以提高生产速度,且无法充分发挥粉末冶金的优点。
本发明的目的在于提供一种从模具的脱模性优异且污染烧结炉的可能性小的粉末冶金用润滑剂,以及配合其而成的金属粉末组合物。
解决课题的手段
为了解决上述课题,本发明提供如下的粉末冶金用润滑剂以及配合其而形成的金属粉末组合物。
[1]粉末冶金用润滑剂,其特征在于配合由下述式(1)表示的仅由碳、氢及氧构成的芳香族羧酸而形成:
(式中,Ar为芳基,Z为直接键合于所述芳基的取代基,且为R、OR、OCOR及COOR中的任一种。R为烷基、烯基及炔基中的任一种。n为1~4的整数。在n为2以上的情况下,Z彼此可以相同也可以不同。)。
[2]粉末冶金用润滑剂,其特征在于,在上述的粉末冶金用润滑剂中,所述式(1)中的R的碳原子数为6以上24以下。
[3]粉末冶金用润滑剂,其特征在于,在上述的粉末冶金用润滑剂中,所述式(1)中的Ar为苯基、萘基及联苯基中的任一种。
[4]粉末冶金用润滑剂,其特征在于,在上述的粉末冶金用润滑剂中,所述式(1)中的Ar为苯基。
[5]粉末冶金用润滑剂,其特征在于,在上述的粉末冶金用润滑剂中,所述式(1)中的n为1,所述Z的取代位置为羧基的对位。
[6]粉末冶金用润滑剂,其特征在于,在上述的粉末冶金用润滑剂中,该粉末冶金用润滑剂的平均粒径为30μm以下。
[7]金属粉末组合物,其特征在于,配合上述的粉末冶金用润滑剂而形成。
[8]金属粉末组合物,其特征在于,在上述的金属粉末组合物中,配合以组合物总量为基准计为3质量%以下的所述润滑剂而形成。
[9]金属粉末组合物,其特征在于,在上述的金属粉末组合物中,进一步配合粘合剂和石墨而形成。
发明效果
本发明的粉末冶金用润滑剂,由于将仅由碳、氢及氧构成的规定的芳香族羧酸作为主成分,因此从模具的脱模性优异,且污染烧结炉的可能性也小。
具体实施方式
本发明的粉末冶金用润滑剂(以下,也称为“本润滑剂”。)为配合由下述式(1)表示的仅由碳、氢及氧构成的芳香族羧酸而形成的润滑剂
上述的式(1)中,Ar为芳基。作为芳基,可以列举:苯基、萘基及联苯基等。它们之中,从烧结时容易蒸发分解的观点考虑,优选苯基。
Z为直接键合于上述芳基的取代基,且为R、OR、OCOR及COOR中的任一种。其中,R为烷基、烯基及炔基中的任一种,可以是直链结构也可以是支链结构。但是,从润滑性的观点考虑,优选直链结构。另外,在这些取代基中,优选OR或OCOR。
作为R,从本润滑剂的稳定性的观点考虑,优选烷基。作为R的碳原子数,从保持润滑性及适度的熔点的观点考虑,优选6~24。
n为1~4的整数。n为2以上的情况下,Z彼此可以相同也可以不同。
另外,Ar为苯基且n为1的情况下,Z的取代位置优选为羧基的对位。这种结构的本润滑剂,结晶性良好,熔点高,而且流动性也良好,因此用于粉末冶金极其优异。
式(1)的芳香族羧酸在本润滑剂中所占的配合量,从脱模性的观点考虑,以润滑剂总量为基准计,优选为50质量%以上,更优选为70质量%以上,进一步优选为90质量%以上。当然,本润滑剂中式(1)的芳香族羧酸也可以实质上占100质量%。
在混合于金属粉末中使用时,本润滑剂为粉末状在金属粉末中的分散方面是优选的,特别是更优选本润滑剂的平均粒径为30μm以下。进一步优选的平均粒径为15μm以下,最优选的平均粒径为5μm以下。但是,若平均粒径过小,则有流动性恶化的可能,因此优选大于1μm。
需说明的是,该平均粒径可以通过例如光散射法进行测定。
作为本发明的金属粉末组合物中使用的原料(金属等),可适合地使用粉末冶金用常用的原料。例如,可以列举:铁(作为雾化铁粉或还原铁粉等的纯铁粉)、铜、钼、铬、锰、镍、钛、镁、锌、钨、磷及石墨形式的碳等。它们例如可以作为部分合金化钢粉、完全合金化钢粉或混合物而使用。作为合金化钢粉,已知有SUS304、SUS316等的不锈钢。
另外,本发明的金属粉末组合物也可以是含有铝、硼、镁、钛等的陶瓷,可以适合用于加压成型。也可以使用这种陶瓷与金属粉的混合粉。
本发明的金属粉末组合物是在上述的原料粉末中配合本发明的润滑剂而形成的组合物。从润滑性(从模具的脱模性)的观点考虑,以组合物总量为基准计,配合量优选为0.5质量%以上,若配合量增多,则成型体的密度降低,从而强度降低,因此优选为3质量%以下,更优选为2质量%以下,进一步优选为1质量%以下。
这里,制备本组合物时,优选也配合粘合剂。粘合剂是指能增强石墨与金属粉(铁粉等)之间的粘着性的物质,例如可优选列举:聚乙烯、聚丙烯、聚乙烯醚、聚丙烯酸酯、聚甲基丙烯酸酯、聚酰胺、聚亚烷基二醇、聚乙烯醇缩丁醛及聚乙烯醇缩甲醛等聚合物,或硬脂酸、油酸、肉豆蔻酸、棕榈酸及花生酸等高级脂肪酸,硬脂酰胺、油酰胺及亚乙基双硬脂酰胺等高级脂肪酰胺,硬脂醇及油醇等高级醇。
作为使用本发明的粉末冶金用润滑油进行粉末冶金的方法(成型法),例如可以列举压缩成型法和喷射成型法。作为压缩成型法,可以使用改变模具温度的冷轧成型法和温轧成型法中的任一种。作为润滑剂的供给方法,可以列举与金属粉混合作为本组合物然后成型的方法,或在模具中涂布本润滑剂的模具润滑法。本润滑剂也可以应用于任意的方法。
另外,本润滑剂或本组合物也可以应用于金属粉末喷射成型法(MIM法)等。
上述的本发明的粉末冶金用润滑剂,由于将仅由碳、氢及氧构成的规定的芳香族羧酸作为主成分,因此仅通过涂布于模具使用即可提高成型后从模具的脱模性,另外,污染烧结炉的可能性也小。而且,配合该润滑剂而形成的本发明的金属粉末组合物,成型后从模具的脱模性也优异,同样污染模具的可能性小。因此,通过使用本润滑剂或本组合物可以显著提高粉末冶金的生产能力。
实施例
以下通过实施例进一步详细地说明本发明,但本发明并不受这些例子的任何限定。
[实施例1]
作为粉末冶金用润滑剂,使用下述的4-己氧基苯甲酸(化合物1,东京化成制造),进行以下所示的评价。将结果表示在表1中。
需说明的是,润滑剂在使用前用球磨机粉碎,然后用106μm目的筛子进行分级(以下的各实施例也同样如此)。
[化1]
(1)从模具的脱模性(润滑性)
(1.1)摩擦系数
使用Bowden-Leben (バウデン)试验机,在试验钢球:SUJ2(3/16英寸)、试验用板材:SUS304、荷重:5kg、速度:20m/s、滑动距离:50mm、滑动次数:5次、试验温度:室温(25℃)的条件下实施。具体而言,在试验用板材上涂布润滑剂,求出滑动次数5次的平均摩擦系数。
(1.2)拉拔力
进行平板拉拔试验。在WC珠(ビードWC )、试验片:S45C、荷重:10.8kN、滑动速度:500m/s、滑动距离:500mm、温度:室温(25℃)的条件下实施。具体而言,在试验片上涂布润滑剂,求出拉拔试验片时的力(最大值)作为拉拔力。
(2)污染性
通过热特性(TG-DTA),简易地评价使用润滑剂时对成型品周边的污染的程度。具体而言,作为热分析装置使用SII公司制造的TG-DTA 6200,放置润滑剂后,在氮气200mL/分钟的气流下,以10℃/分钟的速度从50℃升温至500℃,由DTA曲线求出软化点、熔点,由TG曲线求出95%分解温度。若分解温度低且加热后不残留不挥发性残渣,则作为粉末冶金用润滑剂是优选的。
[实施例2]
作为粉末冶金用润滑剂,合成下述所示的4-十八烷氧基苯甲酸(化合物2),然后进行与实施例1同样的评价。将结果表示在表1中。
[化2]
化合物2的合成方法如下所述。
将4-羟基苯甲酸乙酯49.8g(0.3mol)、硬脂基溴99.9g(0.3mol)、碳酸钾82.8g、二甲基甲酰胺150mL在120℃加热1小时。
冷却至室温后,用水稀释,过滤生成的结晶,水洗,在减压下于60℃干燥,得到4-十八烷氧基苯甲酸乙酯123g(收率98%)。
将该4-十八烷氧基苯甲酸乙酯110g加入220mL的甲苯中,进行加热回流使之溶解。向其中加入220mL的乙醇,加入将29.5g氢氧化钾溶解于30mL水中得到的溶液,加热回流1小时。
冷却至室温后,加入60mL的浓盐酸,进一步加入200mL水,过滤生成的结晶。水洗结晶后,在减压下于60℃干燥,得到4-十八烷氧基苯甲酸 (化合物2) 98g (收率95%)。
[实施例3]
作为粉末冶金用润滑剂,合成下述所示的6-十八烷氧基-2-萘甲酸(化合物3),然后进行与实施例1同样的评价。将结果表示在表1中。
[化3]
除了使用6-羟基-2-萘甲酸甲酯代替4-羟基苯甲酸乙酯以外,化合物3与化合物2同样操作进行合成。
[实施例4]
作为粉末冶金用润滑剂,合成下述所示的4-癸酰氧基苯甲酸(化合物4),然后进行与实施例1同样的评价。将结果表示在表1中。
[化4]
化合物4的合成方法如下所述。
在4-羟基苯甲酸13.8g(0.1mol)、THF140mL、三乙胺22.2g(0.22mol)中,慢慢加入癸酰氯30.3g(0.1mol)。在室温下搅拌30分钟后,加热回流2小时。
冷却至室温后,加入5%盐酸水溶液至pH变为1。过滤生成的沉淀,水洗,在减压下于60℃干燥。得到36.9g的无色结晶(化合物4)(收率91%)。
[实施例5]
作为粉末冶金用润滑剂,合成下述所示的3-甲氧基-4-十八烷酰氧基苯甲酸(化合物5),然后进行与实施例1同样的评价。将结果表示在表1中。
[化5]
除了使用3-甲氧基-4-羟基苯甲酸甲酯代替4-羟基苯甲酸甲酯以外,化合物5与化合物2同样操作进行合成。
[实施例6]
作为粉末冶金用润滑剂,合成下述所示的3-十八烷酰氧基苯甲酸(化合物6),然后进行与实施例1同样的评价。将结果表示在表1中。
[化6]
除了使用3-羟基苯甲酸甲酯代替4-羟基苯甲酸甲酯、用硬脂酰氯代替癸酰氯以外,化合物6与化合物4同样操作进行合成。
[比较例1]
作为粉末冶金用润滑剂,使用ヘガネス公司制造的ケノルーブ(Kenolube P11)进行与实施例1同样的评价。将结果表示在表1中。需说明的是,Kenolube的主成分为亚乙基双酰胺。
[比较例2]
作为粉末冶金用润滑剂,使用アデカ・ファインケミカル公司制造的ZNS-730,进行与实施例1同样的评价。将结果表示在表1中。需说明的是,ZNS-730的主成分为硬脂酸锌。
[表1]
。
[评价结果]
由表1的结果可知,实施例1~6的润滑剂显示出良好的脱模性(润滑性)。另外,也可以理解,这些润滑剂为仅由碳、氧及氢构成的化合物,因此,即使进行烧结,润滑剂也不会残留在产品中,且不会污染烧结炉。
另一方面,比较例1的Kenolube,摩擦系数和拉拔力高,脱模性(润滑性)差。另外,比较例2的ZNS-730,由于主成分为硬脂酸锌,烧结时有污染烧结炉的可能。
[真机试验]
对上述的实施例2的化合物2,与比较例1及比较例2的润滑剂一起进行真机试验。对化合物2,使用喷射磨机进行粉碎,使其平均粒径成为3μm后使用。
在粉末冶金用不锈钢粉(相当于大同特殊钢制造 DAP304的产品)96.4质量%、电解铜粉(相当于福田金属箔工业 CE-25的产品)2.9质量%中加入0.7质量%的润滑剂,使用V型混合器进行混合。
使用机械式粉末压缩,将上述的混合粉体成型为门锁部件,使成型体密度为6.5g/cm3(成型体的质量均为41.45g) 。测定这时的填充高度、压缩荷重、压缩荷重的偏差及工作温度。
另外,将各成型体置于烧结炉中于1100℃进行煅烧,观察成型品的外观。成型品的外观按照以下的基准进行评价:
A:没有伤痕、污染、破裂中的任一种
B:可见伤痕、污染、破裂中的任一种。
进而,观察烧结炉的污染,按照以下的基准进行评价:
A:烧结炉内部的表面上没有析出物(污染)
B:烧结炉内部的表面上有析出物(污染)。
将它们的结果表示在表2中
。
[真机试验的结果]
化合物2与Kenolube(比较例2的润滑剂)相比,填充高度低,显示出良好的流动性,并且工作温度也低,润滑性也良好。另外,即使将成型体于1100℃进行煅烧,成型后的外观也良好,且未见烧结炉的污染。另一方面,ZNS-730在烧结时析出氧化锌,且污染烧结炉。
由上述的结果可以理解,具备本发明的构成的化合物2优于比较例1和2的润滑剂。
Claims (17)
1.一种粉末冶金用润滑剂,其特征在于,配合由下述式(1)表示的仅由碳、氢及氧构成的芳香族羧酸,该粉末冶金用润滑剂是粉末状的,该粉末冶金用润滑剂的平均粒径大于1μm且为30μm以下,
式中,Ar为芳基,Z为直接键合于所述芳基的取代基,且为R、OR、OCOR及COOR中的任一种;R为烷基、烯基及炔基中的任一种;n为1~4的整数;在n为2以上的情况下,Z彼此可以相同也可以不同。
2.权利要求1所述的粉末冶金用润滑剂,其特征在于,所述式(1)中R为烷基。
3.权利要求1所述的粉末冶金用润滑剂,其特征在于,所述式(1)中R是直链结构。
4.权利要求1所述的粉末冶金用润滑剂,其特征在于,所述式(1)中R的碳原子数为6以上24以下。
5.权利要求1所述的粉末冶金用润滑剂,其特征在于,所述式(1)中的Ar为苯基、萘基及联苯基中的任一种。
6.权利要求5所述的粉末冶金用润滑剂,其特征在于,所述式(1)中的Ar为苯基。
7.权利要求1所述的粉末冶金用润滑剂,其特征在于,所述式(1)中的n为1,所述Z的取代位置为羧基的对位。
8.权利要求1所述的粉末冶金用润滑剂,其特征在于,该粉末冶金用润滑剂的平均粒径为5μm以下。
9.一种粉末冶金用润滑剂,其特征在于,权利要求1所述的平均粒径通过用光散射法测定而求得。
10.权利要求1所述的粉末冶金用润滑剂,其特征在于,所述式(1)的芳香族羧酸在该粉末冶金用润滑剂中所占的配合量,以该润滑剂总量为基准计为50质量%以上。
11.一种金属粉末组合物,其特征在于,配合权利要求1~10中任一项所述的粉末冶金用润滑剂而形成。
12.权利要求11所述的金属粉末组合物,其特征在于,配合以组合物总量为基准计为3质量%以下的所述润滑剂而形成。
13.权利要求12所述的金属粉末组合物,其特征在于,配合以组合物总量为基准计为0.5质量%以上的所述润滑剂而形成。
14.权利要求11所述的金属粉末组合物,其特征在于,进一步配合粘合剂和石墨而形成。
15.权利要求11所述的金属粉末组合物,其特征在于,进一步配合陶瓷而形成。
16.一种进行粉末冶金的方法,其特征在于,使用权利要求1~10中任一项所述的粉末冶金用润滑剂。
17.权利要求16所述的进行粉末冶金的方法,其特征在于,其为金属粉末喷射成型法。
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PCT/JP2011/054895 WO2011122230A1 (ja) | 2010-03-31 | 2011-03-03 | 粉末冶金用潤滑剤および金属粉末組成物 |
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