WO2005023461A1 - ニッケル粉およびその製造方法 - Google Patents
ニッケル粉およびその製造方法 Download PDFInfo
- Publication number
- WO2005023461A1 WO2005023461A1 PCT/JP2003/014754 JP0314754W WO2005023461A1 WO 2005023461 A1 WO2005023461 A1 WO 2005023461A1 JP 0314754 W JP0314754 W JP 0314754W WO 2005023461 A1 WO2005023461 A1 WO 2005023461A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- cobalt
- nickel
- nickel powder
- aqueous solution
- particle diameter
- Prior art date
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Classifications
-
- 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
- C22C1/0433—Nickel- or cobalt-based alloys
-
- 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
- B22F1/14—Treatment of metallic powder
- B22F1/148—Agglomerating
-
- 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
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
Definitions
- the present invention relates to nickel particles suitable as conductive particles for a conductive paste and a conductive resin, and a method for producing the same.
- the conductive paste and conductive resin used in these applications are a paste obtained by kneading conductive particles and various resins, and a molded product obtained by curing the paste.
- the characteristics required of the conductive particles include high conductivity of the particles themselves, and low electrical resistance, high migration resistance, and excellent weather resistance even in a molded product obtained by kneading with a resin.
- noble metal powders have high conductivity and low electric resistance, but have a problem that they are expensive.
- Base metal powders such as Ni and Cu, are inexpensive and have high conductivity, but have poor weather resistance. When used for a long time, there is a problem that the electric resistance increases.
- carbon powder is inexpensive and has high weather resistance, but has a problem of low electrical conductivity and high electric resistance when kneaded with resin.
- the present invention is inexpensive, has excellent weather resistance, has a low electric resistance in a state of being kneaded with a resin, can be used stably for a long period of time, and is used for conductive paste and conductive resin A nickel powder suitable as the conductive particles of the above, and a method for producing the same.
- the present inventors have conducted research on the electrical resistance of a molded body obtained by kneading nickel powder with a resin. As a result, the effects of the particle size and the evening density of the nickel powder on the electrical resistance of the molded body are described. Was found to be the largest, and by controlling these to a specific range, the electrical resistance of the molded article was significantly reduced.
- cobalt to nickel powder is effective in improving the weather resistance of nickel powder, particularly when cobalt is added only to the primary particles in the surface layer of nickel powder, that is, the surface layer of secondary particles.
- they have found that weather resistance can be improved.
- the nickel powder provided by the present invention has an average primary particle diameter of 0.2 to 2.0 xm by observation with a scanning electron microscope, an average secondary particle diameter of 8 to 50 mm by a laser particle size distribution measurement, and a tap density. Is 0.5 to 2.0 g / m 1, and contains 1 to 20% by weight of cobalt.
- the ratio between the average secondary particle diameter measured by the laser particle size distribution measurement and the average primary particle diameter measured by the scanning electron microscope observation is desirably in the range of 5 to 100.
- the meaning of the average is that the average secondary particle diameter (D 50) is the particle diameter at which the cumulative volume is 50% by laser particle size distribution measurement.
- the average primary particle size is obtained by measuring the average particle size of 100 particles in the field of view of a scanning electron microscope (SEM) 5000 magnification photograph and calculating the average.
- the primary particles in the surface layer that is, the primary particles in the surface layer of the secondary particles, contain cobalt
- the cobalt content in the surface layer is preferably 1 to 40% by weight.
- the upper limit of the cobalt content when containing cobalt as a whole is 20% by weight, whereas the upper limit of the cobalt content when only cobalt is contained in the surface layer is 40% by weight. This is because the amount of cobalt can be reduced when it is included only in the surface layer compared with the case where cobalt is included, which is advantageous in terms of cost.
- the method for producing nickel powder comprises: a first stage reductive precipitation step of adding a reducing agent to an aqueous solution containing a divalent nickel salt to precipitate nickel; A second step of reducing and precipitating nickel by adding a divalent nickel salt solution, and in at least the second step of the first and second steps of reducing and precipitating, 2 Nickel is precipitated in a state where a valent cobalt salt is added.
- a bivalent cobalt salt is added to the aqueous solution in the second-stage reduction precipitation step so that the cobalt content is 1 to 40% by weight based on the total amount of nickel and cobalt. It is preferable to obtain nickel powder containing cobalt only in the surface layer by addition.
- the aqueous solution in the first and second reduction precipitation steps may contain 1 to 20% by weight of cobalt with respect to the total of nickel and cobalt.
- a nickel powder containing cobalt as a whole can be obtained by adding a divalent cobalt salt.
- the nickel powder obtained by the present invention is inexpensive, the electric resistance of a molded article obtained by kneading the nickel powder and the resin is extremely low, and the molded article has excellent weather resistance and is stable for a long time. Can be used.
- This nickel powder is extremely suitable as conductive particles for conductive paste and conductive resin.
- FIG. 1 is an SEM photograph (XI 500) of the nickel powder of the present invention.
- FIG. 2 is an SEM photograph (X5000) of the nickel powder of the present invention. BEST MODE FOR CARRYING OUT THE INVENTION
- the nickel powder of the present invention is composed of secondary particles in which primary particles are strongly aggregated.
- the nickel powder of the present invention has an average primary particle diameter of 0.2 to 2.0 m as observed by a scanning electron microscope (SEM) and an average secondary particle diameter (D50) of 8 to 50 m as measured by a laser particle size distribution measurement.
- And density should be in the range of 0.5 to 2.0 gZml.
- the average secondary particle diameter (D50) is the particle diameter at which the cumulative volume becomes 50% by laser particle size distribution measurement.
- the average primary particle size was obtained by measuring the average particle size of 100 particles in the field of view of a scanning electron microscope (SEM) 5000x photograph and calculating the average.
- the primary particle diameter determined by SEM observation indicates the particle diameter of each aggregated primary particle.
- the primary particles are appropriately aggregated to form secondary particles having a complex shape such as a chain.
- the secondary particles are entangled with each other to form a network, and thus the molded product exhibits extremely low electric resistance.
- the average primary particle diameter is less than 0.2 m, the primary particles are too agglomerated, and the secondary particles after agglomeration are extremely large lumps or spheres.
- the average primary particle diameter exceeds 2.0 m, the primary particles are less likely to aggregate and remain close to a state in which the primary particles are dispersed.
- the secondary particle diameter determined by laser particle size distribution measurement indicates the particle diameter of the secondary particles in which the primary particles are aggregated.
- the average secondary particle diameter (D50) in this laser single particle size distribution measurement in the range of 8 to 50 im, the number of places where nickel powders come into contact with each other after kneading with the resin increases, and the electric resistance is significantly reduced. I do.
- the average secondary particle diameter (D50) is less than 8, the number of entangled portions is reduced because the primary particles are less agglomerated, and the resistance of a molded article kneaded with nickel powder and resin is increased. If the average secondary particle diameter (D50) exceeds 50 mm, the dispersion of nickel powder in the resin will be uneven. Not preferred.
- the tap density of the nickel powder affects the degree of dispersion in the resin.
- the tap density is in the range of 0.5 to 2.0 g / m 1
- the nickel powder is uniformly dispersed in the resin, and the electric resistance of the obtained molded article is extremely low.
- the sunset density exceeds 2.0 g / m1
- nickel powder is unevenly distributed in the resin and the mutual contact decreases.On the other hand, if it is less than 0.5 g Zml, kneading with the resin is difficult. And a compact cannot be obtained.
- the nickel powder of the present invention is significantly improved and improved in weather resistance by adding a small amount of cobalt. Although the reason is not clear, it is considered that cobalt (Co) is slightly lower than nickel (Ni), so that cobalt is preferentially corroded to improve the weather resistance of nickel. . However, if the cobalt content is less than 1% by weight of the entire nickel powder, there is no effect of improving the weather resistance, and if it exceeds 20% by weight, the cost is high, which is not preferable.
- cobalt is contained only in the surface layer of the nickel powder.
- the surface layer portion of the nickel powder is a portion formed in the second reduction precipitation step in the manufacturing method described later, and is composed of primary particles present on the surface side of the secondary particles in which the primary particles are aggregated.
- the cobalt content of the primary particles in the surface layer is preferably in the range of 1 to 40% by weight.
- the cobalt content of 1% by weight or more of the primary particles in the surface layer is required. Although the content is necessary, even if it is added in excess of 40% by weight, it is difficult to further improve the weather resistance, and the nickel powder becomes ferromagnetic and is used in electronic parts and the like. Not preferred.
- the ratio of the average secondary particle diameter (D50) measured by laser particle size distribution measurement and the average primary particle diameter measured by SEM is preferably in the range of 5 to: L00.
- the particle diameter (SEM diameter) is preferably in the range of 5 to 100.
- the nickel powder of the present invention is produced from an aqueous solution containing a divalent nickel salt by a two-stage reduction precipitation process. That is, in the first-stage reduction precipitation step, a reducing agent is added (usually in excess) to an aqueous solution containing a divalent nickel salt to deposit almost all of the nickel, and the second step is continued with bow I
- nickel is added by adding a divalent nickel salt solution to the aqueous solution containing the precipitated nigel powder after the completion of the first reduction precipitation step, and further adding a reducing agent as necessary. Further precipitate.
- a polyvalent carboxylic acid such as tartaric acid, a commonly used complexing agent such as ethylenediamine, and sodium hydroxide for adjusting pH can be added to the aqueous solution containing a divalent nickel salt.
- the reducing agent is not particularly limited as long as it can reduce and precipitate nickel, and a hydrazine-based reducing agent can be suitably used.
- nickel particles precipitated by the first stage reduction precipitation process become secondary particles in which primary particles are appropriately aggregated, but their cohesion is weak, and separation from the reacted solution is performed. During operation or kneading with resin, they are easily separated and become single particles.
- the precipitated nickel further strengthened the coagulation and maintained a proper coagulation state without separation in the subsequent operation.
- the electrical resistance of the molded body due to kneading with the resin is also extremely low.
- the nickel primary particles deposited in the second reduction precipitation step aggregate outside the nickel secondary particles precipitated and aggregated in the first reduction precipitation step, and are connected in a network structure to reduce strength. It is thought to form high nickel powder.
- the nickel powder produced through the two-stage reduction precipitation process can adjust the concentration of the nickel salt and the reducing agent, the temperature of the aqueous solution and other conditions to obtain the above-mentioned powder characteristics, that is, by scanning electron microscope observation.
- the average primary particle size should be 0.2 to 2.0 im
- the average secondary particle size by laser particle size distribution measurement should be 8 to 50 m
- the tap density should be 0.5 to 2.0 g / m1. Can be.
- the aqueous solution must contain divalent cobalt in only the second stage, or in both the first and second stages, of the two-stage reduction precipitation process described above. What is necessary is just to deposit nickel in a state where the salt is added. In particular, in the case where cobalt is not contained in the inner portion of the nickel powder and cobalt is contained only in the surface layer portion, no cobalt is added in the first reduction precipitation step, and water is added in the second reduction precipitation step. Add divalent cobalt salt to the solution. The amount of the cobalt salt added at this time is 1 to 40% by weight based on the total amount of nickel and cobalt in the aqueous solution, whereby the cobalt content in the nickel powder surface layer can be 1 to 40% by weight. it can.
- a divalent cobalt salt is added to each aqueous solution in the first and second reduction precipitation steps.
- the amount of the cobalt salt to be added is 1 to 20% by weight based on the total amount of nickel and cobalt in the aqueous solution in each of the first and second reduction precipitation steps, or It may be adjusted so that the cobalt content of the entire nickel powder is 1 to 20% by weight.
- Sodium hydroxide and tartaric acid were added to 7500 ml of pure water, and the mixture was heated to 85 ° C with stirring.
- To this aqueous solution were added 60 ml of hydrazine and 13 g of an aqueous solution of Ni-nickel equivalent in Ni equivalent weight, and nickel was precipitated by a first-stage reduction reaction.
- an aqueous solution obtained by mixing an aqueous solution of cobalt chloride and an aqueous solution of nickel chloride so that the Co content becomes 10% by weight with respect to the Ni + Co amount was added to the aqueous solution after the completion of the first-stage reduction precipitation.
- the obtained nickel powder of sample 1 contained cobalt only in the surface layer, and the powder characteristics are shown in Table 1 below.
- the total C0 content is the analytical value, but the C0 content in the surface layer is the value calculated from the C0 content with respect to the Ni + C0 content in the aqueous solution in the second stage reduction precipitation process. It is.
- the SEM diameter in Table 1 means a uniform uniform particle diameter as observed by SEM observation, and D50 means an average secondary particle diameter as measured by laser particle size distribution measurement.
- the nickel powder of Sample 1 was kneaded with 3 g of a thermosetting resin (phenol resin), molded into a sheet, and cured to obtain a formed body. Cut this to 12 mm width After extraction, the electrical resistance was measured at an electrode spacing of 5 mm, and the initial resistance was 4.5 ⁇ . Furthermore, to evaluate the weather resistance, the nickel powder of the same sample 1 was kept in a thermo-hygrostat set at 85 ° C-85% RH for 40 hours, and then a thermosetting resin (phenol resin) was used. The electrical resistance of the molded body obtained by kneading with the mixture was measured, and the resistance after the moisture resistance test was 36.5 ⁇ . The results are shown in Table 2 below, together with the rate of increase in resistance before and after the moisture resistance test.
- a thermosetting resin phenol resin
- Example 2 In the same manner as in Example 1, two-step reductive precipitation of nickel was performed.
- an aqueous solution obtained by mixing an aqueous solution of cobalt chloride and an aqueous solution of nickel chloride so that the Co content becomes 100% by weight with respect to the amount of Ni + Co is used.
- This aqueous solution was added in an amount of 13 N i + Co equivalents to obtain a nickel powder of Sample 2.
- the obtained nickel powder of Sample 2 contained cobalt in its entirety (inside and on the surface), and the powder properties are shown in Table 1 below.
- the electrical resistance of the molded body obtained in the same manner as in Example 1 for the nickel powder of Sample 2 was 5.1 ⁇ , and the resistance after the moisture resistance test was 40 ⁇ . 3 ⁇ , and these results are summarized in Table 2 below.
- nickel was reduced and precipitated in two stages.
- 6 g of an aqueous solution of nickel chloride was added in an amount of Ni equivalent at the first stage of 0 reduction precipitation, and the Co content of the aqueous solution of cobalt chloride and nickel chloride was reduced to Ni only at the time of reduction and precipitation at the second stage.
- a nickel powder of Sample 3 was obtained by adding 20 g of an aqueous solution mixed so as to be 3.5% by weight with respect to the + Co amount, in an Ni + Co equivalent.
- Nigel powder of Sample 3 contained cobalt only in the surface layer.
- the powder characteristics of the nigel powder are shown in Table 1 below.
- the electrical resistance of the nickel powder of Sample 3 measured with respect to the compact obtained in the same manner as in Example 1 was 7.6 ⁇ as the initial resistance, and 75.7 ⁇ after the moisture resistance test. The results are summarized in Table 2 below.
- nickel was reduced and precipitated in two stages.
- 13 g of an aqueous solution of nickel chloride was added in an amount of Ni equivalent of 13 g during the first-stage reduction precipitation, and the Co content of the aqueous solution of cobalt chloride and nickel chloride was reduced to N i + only during the second-stage reduction and precipitation.
- 13 g of an aqueous solution mixed so as to be 30% by weight with respect to the Co amount was added in an amount of Ni + Co equivalent to obtain a nickel powder of Sample 4.
- the obtained nickel powder of sample 4 contained cobalt only in the surface layer.
- the powder characteristics of the nickel powder are shown in Table 1 below.
- the electrical resistance of the molded body obtained in the same manner as in Example 1 for the nickel powder of Sample 4 was 4.8 ⁇ in initial resistance, and 23.5 ⁇ after moisture resistance test. The results are summarized in Table 2 below.
- the nickel powder of Sample 5 obtained contained cobalt as a whole (inside and on the surface).
- the powder characteristics of the nickel powder are shown in Table 1 below.
- the electrical resistance of the molded body obtained in the same manner as in Example 1 was 5.3 ⁇ in initial resistance and 70.0 ⁇ after moisture resistance test. The results are summarized in Table 2 below.
- Nickel was reduced and precipitated in two stages in the same manner as in Example 1.However, at the time of the first stage of reduction deposition, 13 g of an aqueous solution of nickel chloride was added in an Ni equivalent weight of 13 g. An aqueous solution obtained by mixing an aqueous cobalt solution and an aqueous nickel chloride solution such that the Co content becomes 40% by weight with respect to the Ni + Co amount is Ni +. By adding 13 g at 0 equivalent, nickel powder of Sample 6 was obtained.
- the obtained nickel powder of Sample 6 contained cobalt only in the surface layer.
- the powder characteristics of the nickel powder are shown in Table 1 below.
- the electrical resistance measured for the molded body obtained in the same manner as in Example 1 was 6.2 ⁇ in the initial resistance and 28.5 ⁇ after the moisture resistance test.
- the results are shown in Table 2 below. Are shown together.
- Example 2 nickel was reduced and precipitated in two stages.
- an eckel powder of Sample 7 was obtained without adding an aqueous solution of cobalt chloride at the time of the first and second reduction precipitations.
- the nickel chloride aqueous solution was added in an amount of 13 g in terms of Ni equivalent during the first-stage reduction precipitation, and 5 g in terms of Ni equivalent was added during the second-stage reduction precipitation.
- the obtained nickel powder of Sample 7 does not contain cobalt.
- the powder characteristics of the nickel powder are shown in Table 1 below. With respect to the nickel powder of Sample 7, the electrical resistance value of the molded body obtained in the same manner as in Example 1 was 5.2 ⁇ , and the resistance value after the moisture resistance test was 123 ⁇ . 1 ⁇ , and these results are summarized in Table 2 below.
- Table 1 below shows the powder properties of typical filler-like nickel powder commercially available as conductive particles for conductive paste and conductive resin as Sample 7a.
- the initial resistance was 5.2 ⁇
- the resistance after the moisture resistance test was 10 ⁇ . It was 2.5 ⁇ .
- the results are also shown in Table 2 below for reference.
- Sodium hydroxide and tartaric acid were added to 7500 ml of pure water, and the mixture was heated to 85 ° C with stirring.
- aqueous solution were added 60 ml of hydrazine and 26 g of an aqueous nickel chloride solution with an Ni equivalent weight, and nickel powder was precipitated by a single-stage reduction precipitation process. Then, after filtration and washing with water, the powder was dried at 80 ° C. in the air to obtain nickel powder of Sample 8.
- a nickel powder of Sample 9 was obtained in the same manner as described above except that ethylenediamine was used instead of tartaric acid as a complexing agent.
- the obtained Nigel powders of Samples 8 and 9 do not contain coparte.
- the powder characteristics of the nickel powder are shown in Table 1 below.
- the sample 8 and have nickel powder Nitsu sample 9 the measured electrical resistance value for the molded body obtained in the same manner as in Example 1, the initial resistance value was extremely high exceed 1 0 6 Omega, Do not measure the resistance after the moisture resistance test. won.
- the obtained nickel powder of sample 10 does not contain cobalt.
- the powder characteristics of the nickel powder are shown in Table 1 below.
- the electrical resistance of the molded product obtained in the same manner as in Example 1 was measured for the nickel powder of Sample 10, the initial resistance was as high as 150 ⁇ . Not measured.
- the nickel hydroxide powder was reduced at 450 ° C. in a hydrogen / nitrogen mixed atmosphere to obtain a sample 11 Ni powder.
- the Ni powder of Sample 11 obtained by this dry method did not contain Co, and the powder properties are shown in Table 1 below.
- the electrical resistance of the Ni powder of Sample 11 was measured in the same manner as in Example 1. The initial resistance was high at 173 ⁇ , so the resistance was measured after the moisture resistance test. Did not. These results are summarized in Table 2 below.
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Abstract
Description
Claims
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AU2003304458A AU2003304458A1 (en) | 2003-08-29 | 2003-11-19 | Nickel powder and process for producing the same |
JP2005508798A JP4135014B2 (ja) | 2003-08-29 | 2003-11-19 | ニッケル粉およびその製造方法 |
CA002489893A CA2489893C (en) | 2003-08-29 | 2003-11-19 | Nickel powder and production method therefor |
US10/970,849 US7186289B2 (en) | 2003-08-29 | 2004-10-19 | Nickel powder and production method therefor |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2003305704 | 2003-08-29 | ||
JP2003-305704 | 2003-08-29 |
Related Child Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US10/970,849 Continuation US7186289B2 (en) | 2003-08-29 | 2004-10-19 | Nickel powder and production method therefor |
Publications (1)
Publication Number | Publication Date |
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WO2005023461A1 true WO2005023461A1 (ja) | 2005-03-17 |
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ID=34269359
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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PCT/JP2003/014754 WO2005023461A1 (ja) | 2003-08-29 | 2003-11-19 | ニッケル粉およびその製造方法 |
Country Status (5)
Country | Link |
---|---|
US (1) | US7186289B2 (ja) |
JP (1) | JP4135014B2 (ja) |
AU (1) | AU2003304458A1 (ja) |
CA (1) | CA2489893C (ja) |
WO (1) | WO2005023461A1 (ja) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2007063851A1 (ja) | 2005-11-29 | 2007-06-07 | Tyco Electronics Raychem K.K. | ニッケル粉およびその製造方法、ならびに該ニッケル粉を用いたポリマーptc素子 |
US8164414B2 (en) | 2004-06-08 | 2012-04-24 | Tyco Electronics Japan G.K. | Polymer PTC element |
Families Citing this family (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR100709822B1 (ko) * | 2004-12-15 | 2007-04-23 | 삼성전기주식회사 | 산 용액을 이용한 니켈 입자의 표면 처리 방법 |
JP2007191786A (ja) * | 2005-12-20 | 2007-08-02 | Shinano Kenshi Co Ltd | ニッケル粉およびニッケル粉の製造方法 |
JP2007173131A (ja) * | 2005-12-26 | 2007-07-05 | Hitachi Ltd | 微粒子分散液、およびそれを用いた導電パターン形成装置 |
KR20130136639A (ko) * | 2012-06-05 | 2013-12-13 | 삼성전기주식회사 | 니켈 나노 입자, 그 제조방법 및 이를 이용한 적층 세라믹 커패시터 |
CN103769599A (zh) * | 2014-01-06 | 2014-05-07 | 沈阳化工大学 | 一种分散纳米铁颗粒的制备方法 |
CN111537344B (zh) * | 2020-05-11 | 2022-03-08 | 西南石油大学 | 刚性堵漏材料抗压强度测试方法 |
CN115283687B (zh) * | 2022-05-25 | 2024-05-17 | 苏州艾美特企业管理有限公司 | 一种金属颗粒及其制备方法 |
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US7097686B2 (en) * | 1997-02-24 | 2006-08-29 | Cabot Corporation | Nickel powders, methods for producing powders and devices fabricated from same |
JP2945644B2 (ja) * | 1997-12-12 | 1999-09-06 | 三井金属鉱業株式会社 | ニッケル微粉末及びその製造方法 |
JP3280372B2 (ja) | 1999-11-12 | 2002-05-13 | 三井金属鉱業株式会社 | ニッケル粉及び導電ペースト |
JP2001316701A (ja) | 2000-02-28 | 2001-11-16 | Mitsui Mining & Smelting Co Ltd | ニッケル粉及び導電ペースト |
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2003
- 2003-11-19 CA CA002489893A patent/CA2489893C/en not_active Expired - Fee Related
- 2003-11-19 WO PCT/JP2003/014754 patent/WO2005023461A1/ja active Application Filing
- 2003-11-19 JP JP2005508798A patent/JP4135014B2/ja not_active Expired - Fee Related
- 2003-11-19 AU AU2003304458A patent/AU2003304458A1/en not_active Abandoned
-
2004
- 2004-10-19 US US10/970,849 patent/US7186289B2/en not_active Expired - Fee Related
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JPH08246001A (ja) * | 1995-03-10 | 1996-09-24 | Kawasaki Steel Corp | 積層セラミックコンデンサー用ニッケル超微粉 |
WO1996037325A1 (de) * | 1995-05-26 | 1996-11-28 | H.C. Starck Gmbh & Co. Kg | Kobaltmetallagglomerate, verfahren zu ihrer herstellung sowie deren verwendung |
EP1151814A1 (en) * | 1999-11-12 | 2001-11-07 | Mitsui Mining and Smelting Co., Ltd | Nickel powder and conductive paste |
EP1127638A2 (en) * | 2000-02-28 | 2001-08-29 | Mitsui Mining and Smelting Co., Ltd | Nickel powder and conductive paste |
JP2003155506A (ja) * | 2001-11-21 | 2003-05-30 | Murata Mfg Co Ltd | ニッケル粉末の製造方法、ニッケル粉末、導電性ペースト、及び積層セラミック電子部品 |
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US8164414B2 (en) | 2004-06-08 | 2012-04-24 | Tyco Electronics Japan G.K. | Polymer PTC element |
WO2007063851A1 (ja) | 2005-11-29 | 2007-06-07 | Tyco Electronics Raychem K.K. | ニッケル粉およびその製造方法、ならびに該ニッケル粉を用いたポリマーptc素子 |
JP2007146251A (ja) * | 2005-11-29 | 2007-06-14 | Sumitomo Metal Mining Co Ltd | ニッケル粉およびその製造方法、ならびに該ニッケル粉を用いたポリマーptc素子 |
CN101316673B (zh) * | 2005-11-29 | 2011-11-09 | 泰科电子雷伊化学株式会社 | 镍粉及其制造方法、以及使用该镍粉的聚合物ptc元件 |
TWI402116B (zh) * | 2005-11-29 | 2013-07-21 | Tyco Electronics Raychem Kk | 鎳粉及其製造方法以及使用該鎳粉之聚合物正溫度係數(ptc)裝置 |
KR101356377B1 (ko) | 2005-11-29 | 2014-01-27 | 타이코 일렉트로닉스 레이켐 케이. 케이. | 니켈분 및 그 제조 방법 및 상기 니켈분을 이용한 폴리머ptc 소자 |
Also Published As
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JP4135014B2 (ja) | 2008-08-20 |
CA2489893C (en) | 2008-10-07 |
AU2003304458A1 (en) | 2005-03-29 |
US7186289B2 (en) | 2007-03-06 |
US20050072270A1 (en) | 2005-04-07 |
JPWO2005023461A1 (ja) | 2006-11-02 |
CA2489893A1 (en) | 2005-02-28 |
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