Classifications

• • 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
• • 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
• • B22F1/0003—
• • 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
  • H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
• • 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
  • B22F2301/00—Metallic composition of the powder or its coating
  • B22F2301/15—Nickel or cobalt

Definitions

• the present invention relates to a nickel paste that can be suitably used for an internal electrode of a multilayer ceramic capacitor, for example, and a method for producing the nickel paste.
• nickel paste used for an internal electrode of a multilayer ceramic capacitor (hereinafter also referred to as “MLCC”) is manufactured by kneading nickel powder in a vehicle, and contains a large number of aggregates of nickel powder.
• the final stage of the nickel powder manufacturing process usually has a drying process regardless of the metal powder manufacturing method (dry method, wet method), and the drying process in this drying process promotes the aggregation of nickel particles. Therefore, the obtained nickel powder generally contains aggregates produced during drying.
• Recent multilayer ceramic capacitors are required to increase the number of laminated ceramic green sheets with internal electrode layers from several hundred to about 1000 layers in order to achieve a small size and large capacity. For this reason, studies have been made to reduce the thickness of the internal electrode layer from the conventional several micron level to the submicron level, and accordingly, the particle size of the nickel powder of the electrode material for the internal electrode has been reduced. Yes.
• the metal ultrafine powder such as nickel ultrafine powder has poor dispersibility, and when aggregates are present, the nickel powder sinters in the firing step during the production of the ceramic capacitor, and penetrates the ceramic sheet layer. The electrode is short-circuited. Further, even if the ceramic sheet layer cannot be penetrated, the current between the electrodes is reduced due to the short distance between the electrodes, which causes the life of the multilayer ceramic capacitor to deteriorate.
• Patent Document 1 discloses the following technique. That is, first, a process homogenizer or the like is obtained by adding 0.3 part by mass of a specific anionic surfactant to 100 parts by mass of metal ultrafine powder in a metal ultrafine powder water slurry (metal ultrafine powder concentration: 50% by mass). Is carried out for a predetermined time to disperse aggregates of ultrafine metal powder in water to primary particles. Thereafter, 10 parts by mass of, for example, terpineol as an organic solvent is added to 100 parts by mass of the metal ultrafine powder. Thereby, the terpineol layer containing the metal powder becomes a continuous layer and becomes a precipitate, and water is separated as a supernatant to obtain a metal ultrafine powder organic solvent slurry.
• a process homogenizer or the like is obtained by adding 0.3 part by mass of a specific anionic surfactant to 100 parts by mass of metal ultrafine powder in a metal ultrafine powder water slurry (metal ultrafine powder concentration: 50% by mass). Is
• Patent Document 2 uses the molecular cross-sectional area (adsorption cross-sectional area) per molecule of the dispersion transfer accelerator with respect to the addition amount of the dispersion transfer accelerator to be added.
• This theoretical calculation amount can be regarded as the amount equivalent to the minimum amount of dispersion transfer accelerator required to uniformly adsorb and coat the entire surface area of the nickel powder, so the dispersion transfer accelerator can be used efficiently. It can be said that this is a technology for producing a nickel paste.
• Patent Document 1 in order to produce a nickel powder organic slurry, first, a specific anionic surfactant is added to the nickel powder water slurry, and then mixed with an organic solvent to replace the nickel powder. By doing so, a nickel powder organic slurry is obtained, and the process becomes complicated and an efficient treatment cannot be performed. Also, in the method of Patent Document 2, as in the method of Patent Document 1, first, a specific dispersion transfer accelerator and an organic solvent are added to a nickel water slurry to obtain a nickel powder organic slurry. Thereafter, the nickel powder organic slurry needs to be further kneaded with an organic vehicle, and in order to obtain a nickel paste, the nickel powder organic slurry is once obtained as an intermediate product and then made into a nickel paste. Is required.
• the present invention has been proposed in view of such circumstances, and a nickel paste in which ultrafine nickel powder is dispersed in a state with little aggregation, and a nickel paste capable of producing the nickel paste in a simple process.
• An object is to provide a manufacturing method.
• the present inventors have made extensive studies to solve the above-described problems.
• a dispersion transfer accelerator is added to and mixed with a vehicle prepared by dissolving a specific binder resin in an organic solvent in advance, and a nickel powder water slurry is added to the vehicle containing the dispersion transfer accelerator.
• the inventors have obtained the knowledge that a nickel paste in which nickel powder is dispersed with less aggregation can be obtained, and the present invention has been completed. That is, the present invention provides the following.
• the first invention of the present invention contains at least nickel powder, a dispersion transfer accelerator, and a vehicle, wherein the vehicle has an acid amount of a raw material binder resin of 20 to 300 ⁇ mol / g,
• the content of the dispersion transfer accelerator is 0.16 to 3.0 parts by mass with respect to 100 parts by mass of the nickel powder, the nickel concentration is 50 to 70% by mass, and the viscosity of the paste is 8 to 150 Pa ⁇ It is nickel paste which is s.
• the dispersion migration accelerator is a dispersion migration accelerator having an anionic surfactant structure or a dispersion migration accelerator having a polymer structure. Nickel paste.
• the dispersion transfer accelerator is a dispersion transfer accelerator having an anionic surfactant structure, and the following general formula (1) It is a nickel paste that is one or more selected from the compounds shown in (3).
• n is an integer of 10 to 20.
• a fourth invention of the present invention is a method for producing a nickel paste comprising at least nickel powder, a dispersion transfer accelerator, and a vehicle, wherein the nickel concentration is 50 to 70% by mass, and the vehicle
• a second step of separating and removing water is a method for producing a nickel paste comprising at least nickel powder, a dispersion transfer accelerator, and a vehicle, wherein the nickel concentration is 50 to 70% by mass, and the vehicle
• a second step of separating and removing water is a method for producing a nickel paste comprising at least nickel powder, a dispersion transfer
• a vehicle in which the acid amount of the raw material binder resin is 20 to 300 ⁇ mol / g is used, and the dispersion transfer to the vehicle It is a manufacturing method of nickel paste which adds an accelerator.
• the content of the dispersion transition accelerator in the nickel paste is added in the second step.
• the dispersion transfer accelerator is added to the vehicle so as to be 0.16 to 3.0 parts by mass with respect to 100 parts by mass of nickel powder contained in the nickel powder slurry.
• a nickel whose content of the raw material binder resin is 5% by mass or more is used in the first step. It is a manufacturing method of a paste.
• a nickel paste that can be used suitably for, for example, an internal electrode of a multilayer ceramic capacitor by dispersing nickel ultrafine powder with little aggregation. Moreover, according to the manufacturing method which concerns on this invention, such a nickel paste can be manufactured in a simple process.
• the present embodiment a specific embodiment of the present invention (hereinafter referred to as “the present embodiment”) will be described in detail.
• this invention is not limited to the following embodiment, A various change is possible in the range which does not change the summary of this invention.
• the expression “X to Y” (X and Y are arbitrary numerical values) means “X or more and Y or less” unless otherwise specified.
• the nickel paste according to the present embodiment is a nickel paste containing at least nickel powder, a dispersion transfer accelerator, and a vehicle. This nickel paste has a nickel concentration of 50 to 70% by mass and a viscosity of 8 to 150 Pa ⁇ s.
• the vehicle has an acid amount of 20-300 ⁇ mol / g of the binder resin as a raw material, and the content of the dispersion transfer accelerator is 0.16-3.
• the range is 0 part by mass.
• the nickel powder as a constituent component is dispersed with less aggregation, and can be suitably used, for example, for an internal electrode of a highly multilayer ceramic capacitor.
• Nickel powder is a constituent component of the nickel paste, and various nickel powders can be used regardless of a production method such as a wet method or a dry method.
• a production method such as a wet method or a dry method.
• it may be nickel powder by a so-called dry method such as a CVD method, an evaporative quenching method, a hydrogen reduction method using nickel salt or nickel hydroxide, and a reducing agent such as hydrazine is added to the nickel salt solution.
• Nickel powder by a so-called wet method such as the used wet reduction method may be used.
• the nickel powder is preferably ultrafine particles having an average particle size of 0.05 to 0.5 ⁇ m.
• the ultrafine nickel powder can be suitably used as, for example, an internal electrode of a multilayer ceramic capacitor. From the viewpoint of corresponding to the thinning recently required as an internal electrode of MLCC, it is necessary to use nickel powder having an average particle diameter of about 0.05 to 0.3 ⁇ m, and particularly, an internal electrode of 1000 layer level. In order to obtain an electrode, nickel powder having an average particle size of submicron is required, and it is more preferable to use nickel powder of 0.05 to 0.1 ⁇ m.
• the dispersion transfer accelerator is adsorbed and coated on the surface of the nickel powder, and acts to improve the dispersibility in the nickel paste.
• a dispersion transfer accelerator having an anionic surfactant structure or a dispersion transfer accelerator having a polymer structure can be used as this dispersion transfer accelerator.
• the surface of the nickel powder has basic properties. Therefore, by using a dispersion transfer accelerator having an anionic surfactant structure or a dispersion transfer accelerator having a polymer structure as a dispersion transfer accelerator, it can be efficiently adsorbed on the surface of nickel powder, Can be improved.
• Dispersion migration accelerator having an anionic surfactant structure for example, any one of the compounds (1) to (3) having a specific structure represented by the following general formula can be used. .
• n in the formula is an integer of 10 to 20.
• the number of n is smaller than 10, hydrophilicity becomes strong, and there is a possibility that water is difficult to escape during kneading in the production of the nickel paste.
• the number of n is larger than 20, it becomes lipophilic and easily removes water, but it is difficult to dissolve in an organic solvent and the surface of nickel powder may not be efficiently coated.
• cocoyl sarcosinate generally formula (1), molecular formula: C 16 H 31 NO 3
• myristoyl sarcosinate generally formula (1), molecular formula: C 17 H 33 NO 3
• palmitoyl sarcosine generally formula ( 1), molecular formula: C 19 H 37 NO 3
• stearoyl sarcosine generally formula (1), molecular formula: C 21 H 41 NO 3
• Dispersion transfer accelerator having a polymer structure for example, a dispersion transfer accelerator having a polymer structure having a functional group (acid group) such as carboxylic acid at the terminal or in the molecule is used. be able to.
• examples of the dispersion transfer accelerator having a polymer structure having a functional group (acid group) such as carboxylic acid at the terminal include a urethane polymer dispersant.
• a urethane type polymer dispersing agent a brand name: Solsperse 55000 (average molecular weight 55000), a brand name: Solsperse 36000 (average molecular weight 36000), a brand name: Solsperse 21000 (average molecular weight 21000), etc. are marketed (all are Japan). Lubrizol Co., Ltd.) can be used preferably.
• a single carboxylic acid type trade name: Solsperse 3000 can also be used effectively.
• the structure of the dispersion transfer accelerator is not particularly limited, but a comb-shaped polymer is particularly preferable.
• the dispersion transfer accelerator having a comb-like structure has a carboxylic acid group in the anchor portion and a polyoxyalkylene group in the graft portion, and has a structure in which the balance between hydrophobicity and hydrophilicity differs depending on the composition.
• a polymer dispersing agent which is a comb polymer for example, Marialim AWC series and SC series manufactured by NOF Corporation are commercially available.
• the content of the dispersion migration accelerator is in the range of 0.16 to 3.0 parts by mass with respect to 100 parts by mass of nickel powder.
• the content of the dispersion transfer accelerator is less than 0.16 parts by mass with respect to 100 parts by mass of the nickel powder, the water is not efficiently separated during the kneading to prepare the nickel paste, Residual moisture increases.
• the content of the dispersion transfer accelerator exceeds 3.0% by mass, the separation effect of water is not further improved. Impact may occur.
• the vehicle is obtained by dissolving a raw material binder resin in an organic solvent.
• a resin having an acid amount of 20 to 300 ⁇ mol / g in the binder resin as the raw material.
• the present inventors have found that not only the above-described dispersion transfer accelerator but also a binder resin having an acid amount in the above-mentioned range can be efficiently adsorbed on the surface of the nickel powder.
• the surface of the nickel powder is contained by containing the above-described dispersion transfer accelerator and the vehicle containing the binder resin having the acid amount in the above range.
• the adsorbed dispersion transfer accelerator and the binder resin contained in the vehicle the dispersibility of the nickel powder can be effectively improved, and the nickel ultrafine powder can be dispersed in a state with very little aggregation.
• the content of the dispersion transfer accelerator can be reduced by including a vehicle containing such a binder resin.
• the surface of the nickel powder can be more efficiently adsorbed as described above. Water based on the nickel powder water slurry to be kneaded can be separated and removed more efficiently, and the manufacturing process can be simplified.
• the nickel paste according to the present embodiment is added to and mixed with a vehicle containing the specific binder resin, and the resulting vehicle containing the dispersion transfer accelerator is mixed. It can be obtained by adding a nickel powder water slurry and kneading. In such a manufacturing method, since the nickel powder organic slurry as an intermediate product is not generated as in the prior art, it can be manufactured by a simple process.
• the acid amount of the binder resin if the acid amount is lower than 20 ⁇ mol / g, the amount of adsorption to the nickel powder becomes insufficient, and water is not sufficiently separated during kneading to prepare the nickel paste, The amount of residual moisture increases.
• the acid amount of the binder resin exceeds 300 ⁇ mol / g, although the adsorption with the nickel powder is efficiently performed, the viscosity of the nickel paste produced due to the excessive amount of acid becomes too high. When used as an electrode, an appropriate viscosity cannot be obtained. For this reason, it is necessary to use a binder resin having an acid amount in an appropriate range. Specifically, as described above, a binder resin having an acid amount in the range of 20 to 300 ⁇ mol / g is used.
• the binder resin has, for example, a structure selected from a cellulose structure, a cellulose ester structure, and a cellulose ether structure, and has at least one functional group (acid group) such as a carboxyl group introduced therein. Can be used.
• a binder resin having a functional group (acid group) such as carboxylic acid introduced therein and having an acid amount of 20 to 300 ⁇ mol / g is selected, and the binder resin is dissolved in an organic solvent.
• the vehicle can be made by
• the concentration of the binder resin in the vehicle is not particularly limited, but is preferably 5% by mass or more. If the concentration of the binder resin in the vehicle is less than 5% by mass, the viscosity becomes low, no torque is applied during kneading, and the water separation and removal effect may be reduced.
• the organic solvent is not particularly limited as long as it dissolves the above-described binder resin, and those usually used for conductive paste applications can be used.
• a solvent such as a terpene alcohol or aliphatic hydrocarbon can be used.
• terpene alcohol-based organic solvent include terpineol (terpineol), dihydroterpineol, terpineol acetate, borneol, geraniol, linalool and the like.
• the aliphatic hydrocarbon organic solvent include n-decane, n-dodecane, mineral spirit, and the like. About these organic solvents, you may use individually by 1 type and may use 2 or more types together.
• the nickel paste which concerns on this Embodiment can be made to contain various additives as needed in the range which does not impair the effect
• a dispersing agent for further improving the dispersibility of nickel powder a viscosity adjusting agent for adjusting the viscosity, a rheology control agent for improving thixotropy, and the like can be added.
• the nickel paste according to the present embodiment can be manufactured by the following two procedures.
• [Procedure A] A dispersion transfer accelerator is added to the vehicle and mixed to obtain a vehicle containing the dispersion transfer accelerator.
• [Procedure B] A nickel water slurry is added to a vehicle containing a dispersion transfer accelerator and kneaded, and water is separated and removed to obtain a nickel paste having a nickel concentration of 50 to 70% by mass.
• the vehicle to be used can be prepared by dissolving a binder resin in an organic solvent.
• a resin having an acid amount of 20 to 300 ⁇ mol / g is selected as the binder resin constituting the vehicle.
• an organic solvent a terpene alcohol type
• a vehicle prepared by dissolving the binder resin in an organic solvent so that the concentration of the binder resin is 5% by mass or more.
• concentration of the binder resin is less than 5% by mass, the viscosity is low and it is difficult to apply torque during kneading, and water separation is insufficient, which may increase the residual moisture content of the nickel paste.
• dispersion transfer accelerator As the dispersion transfer accelerator, as described above, a dispersion transfer accelerator having an anionic surfactant structure or a dispersion transfer accelerator having a polymer structure can be used. Since the surface of the nickel powder is basic, it can be efficiently adsorbed on the surface of the nickel powder by using these dispersion transfer accelerators. In the present embodiment, these dispersion transfer accelerators are added to the vehicle and mixed to obtain a vehicle containing the dispersion transfer accelerator.
• the nickel powder 100 contained in the nickel powder water slurry in which the content of the dispersion transfer accelerator in the resulting nickel paste is kneaded in the next procedure (procedure B). It is preferable to calculate and add so as to be in the range of 0.16 parts by mass to 3.0 parts by mass with respect to parts by mass.
• the dispersion transfer accelerator when the dispersion transfer accelerator is added so that the content in the nickel paste is less than 0.16 parts by mass with respect to 100 parts by mass of the nickel powder, the water separation is efficient at the time of kneading to prepare the nickel paste. The amount of residual moisture in the resulting nickel paste increases. On the other hand, even if a dispersion transfer accelerator is added so that the content exceeds 3.0% by mass with respect to 100 parts by mass of nickel powder, the separation effect of water is not further improved. The viscosity of the paste may be affected.
• a mixing method after adding the dispersion transfer accelerator to the vehicle for example, a known kneading apparatus such as a stirrer, a self-revolving mixer, or a planetary mixer can be used.
• a known kneading apparatus such as a stirrer, a self-revolving mixer, or a planetary mixer can be used.
• a dispersion transfer accelerator is added at a predetermined ratio to a vehicle using a specific binder resin as a raw material, followed by stirring and mixing. It is characterized by obtaining a vehicle containing a dispersion transfer accelerator.
• the water in the nickel powder slurry can be efficiently separated and removed by adding and kneading the nickel powder water slurry to the vehicle containing the dispersion transfer accelerator.
• the dispersion transfer accelerator is efficiently adsorbed on the surface of the nickel powder, and the binder resin has a specific acid amount contained in the vehicle. Since it also adsorbs to the surface of the nickel powder, the nickel powder can be effectively dispersed, and the water based on the added nickel powder water slurry can be efficiently separated. This makes it possible to produce a nickel paste with very little residual moisture by a simple process. Specifically, a nickel paste having a moisture content of less than 1% by the Karl Fischer method can be obtained.
• Nickel powder water slurry Various nickel powders contained in the nickel powder water slurry can be used regardless of the production method such as the wet method and the dry method as described above. Further, the average particle diameter may be ultrafine particles of about 0.05 ⁇ m to 0.5 ⁇ m, preferably 0.05 ⁇ m to 0.3 ⁇ m, more preferably 0.05 ⁇ m to 0.1 ⁇ m. Such an ultrafine nickel powder is suitably used as an internal electrode application of a multilayer ceramic capacitor.
• the nickel powder water slurry can be obtained by dispersing ultrafine nickel powder as described above in water by a conventionally known method.
• the nickel content in the nickel powder water slurry is not particularly limited.
• the thing which added the dispersion transfer promoter may be used.
• the dispersion transfer promoter the same ones as those added to the vehicle in the procedure A can be used as described above.
• Nickel paste (Kneading of vehicle and nickel powder water slurry) As described above, by adding the nickel powder water slurry to the vehicle containing the dispersion transfer accelerator and performing the kneading process, the water contained in the nickel powder water slurry is efficiently separated, and the residual water content is small. Nickel paste can be obtained.
• the kneading method of the vehicle and the nickel powder water slurry is not particularly limited, and can be performed by a known method. Specifically, it can be performed by a method using a kneading apparatus such as a roll mill, a ball mill, a homogenizer, a lycra machine, a kneader, or a planetary mixer. Further, if necessary, the pressure may be reduced using a vacuum pump or an aspirator, defoaming or dehydration treatment may be performed, or heat treatment may be performed. Thereby, the moisture content of the nickel paste obtained can be reduced more effectively, and the moisture content by the Karl Fischer method can be made less than 1% by mass more efficiently.
• a kneading apparatus such as a roll mill, a ball mill, a homogenizer, a lycra machine, a kneader, or a planetary mixer.
• the pressure may be reduced using a vacuum pump or an aspirator, defoam
• the nickel concentration of the obtained nickel paste is treated so as to be 50% by mass or more and less than 70% by mass.
• the nickel concentration in the paste is less than 50% by mass, it is difficult to apply torque during kneading, and water separation is insufficient, resulting in an increased amount of residual moisture in the nickel paste.
• the nickel concentration in the paste exceeds 70% by mass, the nickel concentration is too high and the fluidity is lost, so that the water is not sufficiently separated during the kneading and the residual moisture amount increases. If the nickel concentration is too high, it is difficult to dilute with an organic solvent to make a paste.
• a dielectric component barium titanate which is a constituent component of the multilayer ceramic capacitor
• a dispersant can be added in order to further improve the dispersibility of nickel in the paste
• an organic solvent can be added to adjust the viscosity.
• a rheology control agent or the like can be added and kneaded.
• the dispersion transfer accelerator is added to the vehicle and mixed, and then the obtained vehicle including the dispersion transfer accelerator is mixed.
• a nickel paste having a nickel concentration of 50 to 70% by mass is obtained by adding and kneading the nickel powder water slurry and removing the separated water.
• the manufacturing method it is possible to effectively separate and remove moisture, and it is possible to obtain a nickel paste in which the amount of residual moisture is small and nickel powder is dispersed with very little aggregation. Further, unlike the conventional case, it is not necessary to produce an organic powder of nickel powder as an intermediate product, and a nickel paste can be produced by an extremely simple process.
• the obtained nickel paste can be suitably used, for example, for an internal electrode of a highly multilayer ceramic capacitor, for which demands for miniaturization are increasing.
• Nickel paste is applied on a PET film to a thickness of 200 ⁇ m using an applicator, dried at 120 ° C. for 40 minutes, and the resulting film is cut out to be ⁇ 40 mm, and the area, film thickness, and mass are measured.
• the dry film density (g / cm 3 ) of the nickel paste was calculated from the measurement data.
• the entire amount of the vehicle containing the dispersion transfer accelerator was put into a planetary mixer (Hibismix 2P-1 type, manufactured by PRIMIX), and nickel powder water slurry (water content 80%) manufactured by Sumitomo Metal Mining Co., Ltd. ) (Ni ultrafine powder by wet reduction method, average particle size 0.07 ⁇ m) 500 g was added and kneaded at a rotation speed of 30 rpm for 15 minutes to remove water separated from the kneaded product. Thereafter, 500 g of the same nickel powdered water slurry (water content 80%) was added again and kneaded under the same conditions (rotation speed 30 rpm, 15 minutes) to remove the separated water. This operation was repeated, and a total of 1.5 kg of nickel powder water slurry (water content 80%) was added to obtain a kneaded material containing 300 g of nickel powder in total.
• a planetary mixer Hibismix 2P-1 type, manufactured by PRIMIX
• the residual moisture content of the nickel paste was as extremely low as 0.84% by mass.
• the dry film density was 5.5 g / cm 3 , and a high film density was obtained.
• the viscosity was 131.2 Pa ⁇ s, and it was a viscosity that could be used as a paste as it was.
• Example 2 With respect to the amount of the dispersion transfer accelerator added to the vehicle, except that the addition amount of N-oleyl-N-methylglycine (trade name: oleoylsarcosine 221P) as a dispersion transfer accelerator was changed to 4.5 g. A nickel paste was prepared in the same manner as in Example 1.
• Example 3 With respect to the amount of the dispersion transfer accelerator added to the vehicle, except that the addition amount of N-oleyl-N-methylglycine (trade name: oleoylsarcosine 221P) as a dispersion transfer accelerator was changed to 9.0 g. A nickel paste was prepared in the same manner as in Example 1.
• Example 4 First, 120 g of dihydroterpineol (manufactured by Nippon Fragrance Co., Ltd.) as an organic solvent and 10.5 g of acrylic resin (standard name: LC # 9176, manufactured by Toei Kasei Co., Ltd.) as a binder resin are charged and heated to 80 ° C. with stirring. Dissolved to prepare the vehicle. Next, 1.8 g of N-oleyl-N-methylglycine (trade name: oleoyl sarcosine 221P) as a dispersion transfer accelerator is dissolved in the prepared vehicle, and 132.3 g of the vehicle containing the dispersion transfer accelerator is dissolved. Obtained.
• N-oleyl-N-methylglycine trade name: oleoyl sarcosine 221P
• the entire amount of the vehicle containing the dispersion transfer accelerator was put into a planetary mixer (Hibismix 2P-1 type, manufactured by PRIMIX), and nickel powder water slurry (water content 80%) manufactured by Sumitomo Metal Mining Co., Ltd. ) (Ni ultrafine powder by wet reduction method, average particle size 0.1 ⁇ m) was charged, and kneaded at a rotation speed of 30 rpm for 15 minutes to remove water separated from the kneaded product. Thereafter, 500 g of the same nickel powder water slurry (water content 80%) was added again and kneaded under the same conditions (rotation speed: 30 rpm, 15 minutes) to remove the separated water. This operation was repeated, and a total of 1.5 kg of nickel powder water slurry (water content 80%) was added to obtain a kneaded material containing 300 g of nickel powder in total.
• a planetary mixer Hibismix 2P-1 type, manufactured by PRIMIX
• nickel powder water slurry water
• Example 5 With respect to the amount of the dispersion transfer accelerator added to the vehicle, except that the addition amount of N-oleyl-N-methylglycine (trade name: oleoylsarcosine 221P) as a dispersion transfer accelerator was changed to 4.5 g. A nickel paste was prepared in the same manner as in Example 4.
• N-oleyl-N-methylglycine trade name: oleoylsarcosine 221P
• Example 6 As the binder resin, N-oleyl-N-methylglycine (trade name), which is a dispersion transfer accelerator added to the vehicle, is changed to 10.5 g of an acrylic resin having a standard name of PC # 5984 manufactured by Toei Kasei Co., Ltd. : A nickel paste was prepared in the same manner as in Example 4 except that the amount of oleoylsarcosine 221P) was changed to 1.8 g.
• Example 7 The dispersion transfer accelerator to be added to the vehicle was changed to 1.5 g of a polymer dispersant having a structure having an acid group at the terminal (Solsperse 55000, manufactured by Nippon Lubrizol Co., Ltd.), and a nickel powder water slurry (water content 80%)
• the nickel paste was prepared in the same manner as in Example 1 except that the material was changed to one containing Ni ultrafine powder having an average particle size of 0.2 ⁇ m by a wet reduction method manufactured by Sumitomo Metal Mining Co., Ltd.
• Example 8 Nickel in the same manner as in Example 7 except that the dispersion transfer accelerator added to the vehicle was changed to 1.5 g of a polymer dispersant having a structure having an acid group at its terminal (Solsperse 21000, manufactured by Nippon Lubrizol Co., Ltd.). A paste was prepared.
• Example 9 A nickel paste was prepared in the same manner as in Example 8 except that 270 g of dihydroterpineol (manufactured by Nippon Fragrance Co., Ltd.) was used for the amount of the organic solvent.
• Example 10 As a binder resin, the standard name: STD4 made by Dow Chemical Co. is changed to 10.5 g of ethyl cellulose, and the dispersion transfer accelerator added to the vehicle is Lauroyl, an anionic surfactant made by Kawaken Fine Chemical Co., Ltd. Sarcosine (trade name: Soypon SLA) was changed to 0.48 g.
• the nickel powder water slurry (water content 20%) was changed to one containing Ni ultrafine powder having an average particle diameter of 0.3 ⁇ m by a wet reduction method manufactured by Sumitomo Metal Mining Co., Ltd. A nickel paste was produced in the same manner as in Example 1 except for the above.
• Example 11 Except that the dispersion transfer accelerator added to the vehicle was changed to 1.8 g of lauroyl sarcosine (trade name: Soypon SLA), an anionic surfactant manufactured by Kawaken Fine Chemical Co., Ltd., in the same manner as in Example 10. A nickel paste was prepared.
• lauroyl sarcosine trade name: Soypon SLA
• anionic surfactant manufactured by Kawaken Fine Chemical Co., Ltd. in the same manner as in Example 10.
• a nickel paste was prepared.
• Example 12 A nickel paste was prepared in the same manner as in Example 1 except that the binder resin was changed to 10.5 g of ethyl cellulose having the standard name of STD200 manufactured by Dow Chemical Company.
• Example 13 A nickel paste was prepared in the same manner as in Example 1 except that the binder resin was changed to 10.5 g of ethyl cellulose having the standard name manufactured by Dow Chemical Company: STD20.
• Example 14 A nickel paste was prepared in the same manner as in Example 1 except that the binder resin was changed to 10.5 g of ethyl cellulose having the standard name of STD4 manufactured by Dow Chemical Company.
• Ni concentration was too high at 83.6% by mass, making it difficult to separate and remove water, making it impossible to produce a nickel paste.
• the Ni concentration was as low as 36.36% by mass, and it was difficult to apply torque during kneading. Therefore, separation and removal of water from the kneaded material is insufficient, and the amount of residual moisture in the produced nickel paste is large.
• the dry film density was also low.
• Example 3 A nickel paste was prepared in the same manner as in Example 4 except that the binder resin was changed to 10.5 g of an acrylic resin having the standard name YZ # 5125 manufactured by Toei Kasei Co., Ltd.
• Example 4 As in Example 10, except that the dispersion transfer accelerator added to the vehicle was changed to 0.27 g of lauroyl sarcosine (trade name: Soypon SLA), an anionic surfactant manufactured by Kawaken Fine Chemical Co., Ltd. An attempt was made to make a nickel paste.
• lauroyl sarcosine trade name: Soypon SLA
• the amount of the dispersion transfer accelerator was too small, the nickel powder water slurry could not be kneaded and a nickel paste could not be produced.
• Table 2 shows the evaluation results of the nickel paste in each example and comparative example.
• Comparative Example 1 Comparative Example 3, and Comparative Example 4, since the nickel paste could not be produced, the dry film density and viscosity were not evaluated. Further, in Comparative Example 4, since the nickel powder water slurry could not be kneaded, the residual water content was not measured.

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