TW201021054A - Conductive powder and manufacturing method of conductive material and conductive particle containing the same - Google Patents

Abstract

The invention provides conductive powder having a particle diameter smaller than the conventional technique, better dispersibility and conductivity and made from conductive particle of nickel or nickel alloy coating on the surface of core particle. The conductive particle has a plurality of projections projected from the surface of the coating, combined with the coating to form a continuum and with the aspect ratio over 1. The number of the projections with the aspect ratio above 1 is over 40% of the total number of the projections. As to the conductive powder, the weight of the one-time particle of the above-mentioned conductive particle is over 85% of the weight of the conductive powder.

Description

201021054 VI. Description of the Invention: [Technical Field] The present invention relates to a conductive powder and a conductive material containing the conductive powder. Further, the present invention relates to a method for producing conductive particles. [Prior Art] 4 In the present case, four people have previously proposed electroless electroless plating powder having minute protrusions composed of recorded or recorded alloys on the surface (refer to Patent Document 1). The particles show good electrical properties due to the microprotrusions. The absence of the electricity (four) is to add the aqueous slurry of the spherical heart material to the electroless ore bath containing the recorded salt, the reducing agent, the wrong agent, etc., and the electroplating step (A step) And in the aqueous liquid filling of the spherical core material, the constituents of the electroless liquid dressing liquid are separated into at least two liquids, and they are simultaneously and simultaneously, and the electroless plating is added by -ni & Step (Step B) Manufactured. With regard to this manufacturing method, in the A-step release, the (ii) film of the core material particles forms (4), and the non-pregnant nucleus which forms the starting point of the formation of the protrusion grows in the middle of the step to form a protrusion. The electrolysis (4) which is completed by this is a conductive adhesive or the like which is suitable for connection circuits such as poems (4) and (4). In addition to this technique, the water-conducting film and the anisotropic conductive adhesive adhere to the surface of the core material particles of the patent document, and the nickel-core material having a particle size of 4 Å is adhered to the surface of the particle size of 5 〇 nm. The electroless ore of the connected electroless ore is completed, and the conductive particles having the protrusions are completed. However, in this method, 'the adhesion between the core material particles and the nickel core material 201021054 is weak, so the integration of the nickel layer and the protrusion portion on the surface of the core material particle is lacking, and in the case where the pressure is applied by the conductive particles, the protrusion portion is formed. Easy to break. In addition, it is very difficult to uniformly adhere a nickel core material having a particle diameter much smaller than 50 nm on the surface of the core material particle having a particle diameter of 4 m, because the nickel core substance is attached to the surface of the core particle. It is more likely that the nickel core materials are agglomerated with each other. As a result, the agglomerated particles having a large particle diameter in which the nickel core materials are aggregated adhere to the surface of the core material particles, and it is easy to form a very large projection. On the other hand, in recent years, with the further miniaturization of electronic devices, the circuit width and pitch of electronic circuits have become smaller and smaller. As a result, the electroless plating powder used for the above-mentioned conductive adhesive, an anisotropic conductive film anisotropic conductive adhesive or the like is required to have a small particle diameter. However, when the particle diameter of the particles is reduced, the particles are likely to aggregate with each other, and even if particles having a small particle diameter are used, the apparent particle diameter (secondary particle size) due to aggregation becomes large. Further, in the case of using a small particle diameter, it is difficult to increase the conductivity (reducing the electric resistance) than when a large particle is used. [Patent Document 1] JP-A-2000-243132 [Patent Document 2] JP-A-2006-228474 SUMMARY OF INVENTION [Problems to be Solved by the Invention] Accordingly, it is an object of the present invention to provide various functions as compared with the above-mentioned The conductive powder of the technology is also improved by the conductive powder. 201021054 [Means for Solving the Problem] In order to achieve the above object, the results of intensive research by the inventors of this case have been made to use conductive particles having the same degree of dispersibility as the conventional ones and having a particle diameter smaller than the conventional technique. In the case, the shape of the dog formed on the surface thereof is longer than the conventional technique, and the decrease in conductivity can be suppressed. The present invention provides a conductive powder based on the above research, and is applicable to the coffin. a conductive powder comprising a conductive particle of a nickel or a nickel alloy film formed on the surface of the particle, wherein the conductive particle has a surface protruding from the surface of the film and is a continuous body and a history of the film. a ratio of the number of protrusions in which the aspect ratio is i or more; the ratio of the number of the protrusions having an aspect ratio of one or more of the number of the upper portions is more than 40% of the total protrusion;

In the above-mentioned conductive powder, the weight of the heavy-duty helmet I·, +, and the broadcaster is 85 wt% or more of the weight of the conductive powder. The invention also provides a method for conducting electricity containing a ·························································································· At the time, the surface shape of the 4 core material particles is .· 咖 〜 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 The core material particles; and the above-mentioned 201021054 material particles α having an initial layer of iron and the aqueous polymer material containing the above dispersing agent are maintained in a range of pH values exhibiting the dispersion effect of the above dispersing agent, and are temporally-oriented. A nickel ion and a reducing agent are added in an amount such that the amount of precipitation per hour is 25] 00, and the same Bf of the pronuclear particles in which nickel is formed in the aqueous slurry is attached to the core. In the case of the material particles, the nucleus particles are grown by using the deposited nucleus particles as a starting point, and the protrusions 0 having an aspect ratio of $ i or more are formed. [Effect of the invention] The conductive powder of the present invention constitutes the conductivity thereof. Particle size ratio is known Surgery is still small, but the dispersion and good electrical conductivity. Further, according to the production method of the present invention, the above-mentioned conductive powder can be easily produced. [Embodiment] [Best Mode for Carrying Out the Invention] Hereinafter, the present invention will be described based on preferred embodiments of the present invention. The conductive powder of the present invention is formed by forming a nickel film or a nickel alloy film on the surface of the core material particles (hereinafter, these films are simply referred to as "nickel film"). One of the characteristics of the conductive powder of the present invention is that it has a plurality of protrusions protruding from the surface of the nickel film. Hereinafter, the protrusion will be described. The formation of a plurality of protrusions on the surface of the conductive powder is a well-known technique in the art as described in the prior art of the present specification. With respect to such a background art, in the present invention, the use of a specific shape as a projection is a point which is remarkably different from a conventional conductive powder. Specifically, the special 201021054 of the protrusions in the conductive powder of the present invention is characterized by an aspect ratio of 1 or more. The aspect ratio in the present specification means the ratio of the degree of the protrusion 突起 to the width D of the protrusion at the base of the protrusion, that is, the value defined by Η/D. From this definition, it can be understood that the aspect ratio is a measure of the degree of slenderness of the protrusion, and the significance is that the larger the value, the more the protrusion has an elongated shape. The aspect ratio of the protrusions in the conventional conductive powder having the protrusions is known from the inventors of the prior art in the patent document 1 described in the prior art item of the present specification, and it is not easy to make it Become i or above. The protrusions in the conventional conductive powder can be said to have a short fat shape (for example, refer to the 帛 2 diagram described later). (4) Here, the protrusions in the conductive powder of the present invention are elongated protrusions extending radially from the surface of the particles as shown in Fig. i to be described later. The inventors of this case have studied the aspect ratio of the Department: It is revealed that if the value is 乂, it will be: the shape of the dog is thinner than the conventional technology, and the conductivity becomes very In the case where the electrode is guided by the conductive powder of the present invention, it is considered that when a thin oxide film or the like is naturally formed on the surface of the electrode, or an oxide film of the electrode is intentionally formed, If the height and width of the protrusions are relatively large, the oxide film can be easily penetrated. In the case where the conductive powder is formed to form an anisotropic conductive film, the gate width of the protrusion is larger than that of the rudder. We believe that the conductivity is improved due to the high resin exclusion. For this reason, we also think that if the value of the aspect ratio of the protrusion is too large, the protrusion will be damaged, so the height and width of the door are better. Range is

Uj4·. More preferably, it is U~3,5, and it is better to say that the height of the ridges of the protrusions having a large aspect ratio is large. The conductive particles of ruthenium can be produced, for example, by the method described in the following Japanese Patent No. 7, 201021054. In view of the individual particles in the conductive powder, it is preferable that the aspect ratios of the protrusions of each of the (four) sub-mass satisfy the above range, but the study of the inventors of the present case can understand the aspect ratio. The ratio "the ratio of the large-sized portion of the above-mentioned full circumference" is 40% or more with respect to the total number of the protrusions, and is preferably 45% or more, more preferably 5 % or more, more preferably 5 to 5% or more. Sex.

The above-mentioned aspect ratio tears, + L ❹ conductive powder " Each particle in the tantalum powder was magnified by an electron microscope. The base D and the height H of at least one of the protrusions were measured for each of the particles. In this case, the protrusion in the center of the particle in the observation image tends to be measured by the protrusion of the peripheral edge of the pre-existing edge. The above method/different particles are number-averaged for the object, and the value is used as the data of the aspect ratio=the same width ratio, because the protrusion “# 后 所述 后 后 后 后 ) ) ) ) ) The particle observation (the illusion is generally less of a concern). The resulting aspect ratio of the base D of the protrusion is as long as the length D itself and the protrusion "μ * the base of the part L0. 5" In particular, 'the length D of the base is 〇.05~〇.5... especially preferably 〇./.4(4), the long D in the high β aspect and the wide 4 (four) of the protrusion. The base of the protrusion is electrically conductive. The right side of the door is within this range, and the number of protrusions with an aspect ratio of 1 or more in each particle of the conductive powder is also related to the particle size of the particle, as will be described later. In the case where the particle diameter of the particles is 3/zm or less, it is 2 to 4, and particularly preferably 2 to 20, per particle, because the conductivity of the conductive powder is further improved. Each of the protrusions in the powder is continuous with the film on which the core material particles are coated. The protrusion and the film-like film are composed of a recording or chain alloy. The term "continuous body" as used herein means that the nickel film and the protrusion are composed of the same material, and the protrusion is composed of a single piece. - a step formed by the step of forming a film and a protrusion between the film and the protrusion portion. Therefore, for example, a film is formed on the surface of the core material particle, and is attached thereto for attachment thereon. The protrusions formed by the pronuclear particles forming the protrusions and the pronuclear particles as the starting point of growth are not formed in a single step by the protrusions, and are included in the continuum of the present invention. When the portion and the protrusion portion are in a continuous body, the strength of the protrusion portion is ensured. Even when the conductive powder is used, the protrusion portion is hardly broken. As a result, good conductivity can be obtained. If it is too thin, it is difficult for the conductive powder to exhibit sufficient conductivity. · Conversely, if it is too thick, it is easy to peel off from the surface of the core particle. «: Some views 'The thickness of the nickel film (in the absence of protrusions) The thickness of the portion is preferably 〇.0b 0.3 (four), more preferably 0.05 to 0.2. The thickness of the nickel film can be obtained by dissolving nickel from the conductive powder and quantifying the solution. If this method is used, it is not only the nickel film, but the nickel in the large part will also dissolve, but *, because the proportion of the dog in the nickel is always low, and the amount of nickel in the protrusion can be ignored. 9 201021054 In the conductive powder boat of the present invention, the shape of each particle is relatively shaped. The shape of the particle referred to herein means a shape other than the protrusion. Since the particle is spherical and has a protrusion, it is * The conductivity of the powder is very high. Conductivity of the moon In the conductive powder of the present invention, the specific use of the respective particles of the conductive powder is made of T, and the results of the invention are in the same case. The aspect ratio of the protrusions is small to the particle diameter of the conductive particles, but the conductivity is improved: The particle size of the electro-particles is Η. "" Don't be better for two:: more: I is better. Further, the particle size of the conductive particles = the particle diameter of the cerium particles, and the _ submicron = the particle diameter of the core material particles and the film = thickness, respectively, and the particle diameter of the conductive (tetra) is determined from these values. Conductive particles, which have a particle size of 峰Fengfengcheng, ▲ tend to aggregate easily. When agglomeration occurs, defects such as short-circuiting due to the use of conductive particles occur. Further, when the 胄 胄 film is easily treated by the ginseng, the nickel film is agglomerated and applied to pulverize, etc., and the reason is that the conductivity is lowered. From this point of view, it is important to report on the conductability of the present invention. In the present invention, the weight of the particles is one-time, and preferably nine, with respect to the guide μ (four). The weight% or more, more preferably 92 parts by weight, the weight of the high-conductivity particles m, for example. In order to lift the particles. Once "the method described in the following article is made. Conduction: = the weight of the electric weight is measured by the following method to put the i king object into the water of iuumL, to supersonic wave 10 201021054 (h〇mogenizer) The dispersion was measured for 1 minute. Next, the particle size distribution was measured by Coulter Counter method. From this result, the weight ratio of the primary particles was calculated. As described above, the nickel film and the protrusions in the conductive particles were It is composed of the same material, and specifically & is composed of a metal nickel or a nickel alloy. The nickel alloy is, for example, a nickel-phosphorus alloy. The nickel-phosphorus alloy is in the manufacture of a conductivity Thai body as described later. An alloy produced by using sodium hypophosphite as a reducing agent for nickel. Regarding the conductive powder of the present invention, the surface of each particle is composed of nickel or a nickel alloy, or nickel may be covered with a noble metal. Or the surface of a nickel alloy. Regarding the noble metal, gold or palladium of a highly conductive metal is used, and gold is preferably used. The coating of the noble metal can further improve the conductivity of the conductive powder. The thickness of the noble metal coating is generally about 0. 001 to 0.5 min. The thickness can be calculated from the amount of precious metal ions added, chemical analysis, etc. Next, the production of the conductive powder to which the present invention is applied is applied. The production method is roughly classified into (1) a step of forming a nickel initial film layer on the surface of the core material particles, and (2) using the particles completed in the step A as a raw material to form a target conductivity. The two steps of the step B of the particles are described below for each step. In step A, 'mixing the electroless bond containing the dispersant and the recorded ions is cold mixed with the core particles carrying the precious metal on the surface, in the core particles Table V is an initial film layer of nickel. The type of the core material particles is not particularly limited, and both organic matter and inorganic matter can be used. Considering the electroless electric boat 11 described later, 201021054 method 'heart material particles are preferably 5|~丨, 7, the horse is dispersed in the water. Therefore, the core material particles are preferably substantially insoluble 7tc, the water is better for the acid, alkali, etc. will not dissolve or deteriorate. Can be divided in water β 甘甲刀刀疋 means that a suspension which is substantially dispersed in the right middle can be formed by a usual dispersing method such as stirring, and the degree of dispersion = the extent to which a film can be formed on the surface of the core material particles. The shape of the conductive particles has a large influence on the shape of the conductive particles. As described above, since the thickness of the lock skin on the surface of the coated core particles is thin, the shape of the core particles is almost exactly reflected as conductivity. The shape of the particles. Since the conductive particles are preferably spherical, the shape of the core particles is preferably spherical. The core particles are spherical, and the surface of the core particles is The particle size of the conductive particles has a great influence. As described above, since the thickness of the film on the surface of the particles to be transferred is thin, the particle size of the core particles is reflected as conductive particles. Particle size. From this point of view, the particle size of the core material particles can be the same as the particle size of the conductive particles of the target material, specifically 1 to 10/zm, especially the better.

The right is 1 to more especially the better name 1~3 # m. The particle size of the core material particles can be measured by a method similar to the particle size of the conductive particles. The particle size distribution of the core material powder measured by the above method has a width. Generally, the amplitude of the particle size distribution of the powder is expressed by a coefficient of variation shown by the following formula. On the other hand, if the core material particle variation coefficient (%) = (standard deviation / average particle diameter) xl 〇〇 if the coefficient of variation is large, the distribution width is large; and when the coefficient of variation is small, the particle size distribution is narrow. In the present invention, the 12 201021054 sub' is preferably such that the coefficient of variation is 3 Å, particularly preferably hereinafter, more preferably 10% or less. The reason for this is that when the conductive particles of the present invention are used as the conductive particles in the anisotropic conductive ruthenium, there is an advantage that the contribution ratio effective for the connection becomes high. Specific examples of the core material powder include metals (including alloys), glass, ceramics, bismuth oxide, carbon, metal or non-metal oxides (including Aqueous), metal citrate containing metal citrate, metal carbide, metal nitride, metal carbonate, metal sulphate, metal sulphate, metal sulphide, metal sulphate, metal dentate and carbon Wait. Examples of the organic substance include natural fiber, natural resin, polyethylene, polypropylene, polyethylene, polystyrene, polybutylene (polyamide), polyacrylic acid (polyamide), and polyacrylic acid (polyacryHc ester). ), polyacrylonitrile, p〇lyacetal, ionomer-containing polymer (ionomer), thermoplastic resin such as polyester; alkyd resin, phenol resin, urea resin, melamine resin , xylene resin, silicin resin, epoxy resin or diallylphthalate resin. These may be used singly or in combination of two or more. Further, the other physical properties of the core material particles are not particularly limited. However, when the core material particles are resin particles, it is preferred that the K value defined by the following formula (2) is 10 kgf/mm 2 to 1 000 〇 kgi at 20 C. The range of /imn2 and the recovery rate after compression deformation are in the range of 1% to 1%% at 20 °C. The reason for this is that the electrode can be sufficiently brought into contact with the electrode without satisfying the electrode when the electrodes are pressed against each other. 13 201021054 κ value (kgf/mm"=(3//2))FxS-3/2xR-w2 (2) F and S shown in formula (2) are micro compression tester MCTM-500 The value measured by (Island; manufactured by Seiko Co., Ltd.) is the microsphere here.

The load value (kgf) and compressive strain (nun) of 1〇% compression deformation, R is the radius of the microspheres (mW core particles preferably have the ability to capture precious metal ions on their surface, or are subject to surface modification It has the ability to capture noble metal ions. The noble metal ions are preferably ions such as silver and silver. They have the ability to capture noble metal ions, and the fingers can capture precious metal ions as chelate or salts. For example, in core particles. In the case where an amine group, an iminium group, a amide group, a quinone group, a cyano group, a hydroxyl group, a nitrile group, a carboxyl group or the like is present on the surface, the surface of the core material particle has a noble metal. In the case where the surface is modified to have the ability to capture noble metal ions, a method disclosed in, for example, JP-A-61-64882 can be used. The above-mentioned core material particles are used to carry a noble metal on the surface. Lv, the core material particles are dispersed in a slightly acidic aqueous solution of a noble metal salt such as vaporized palladium or silver nitrate, whereby the surface of the particles is trapped of noble metal ions. The concentration of the noble metal salt is per l. The particle surface area of m2 is 1χ1〇—7~1χ1〇_2 The range of Moir is sufficient. The core particles that have captured the noble metal ions are separated from the system and then washed. Next, the core particles are suspended in water and added thereto. The reduction agent is used to carry out the reduction treatment of the noble metal ions, whereby the surface of the core material particles carries the noble metal. Regarding the reducing agent, for example, sodium hypophosphite, sodium oxynitride, code hydrogenation, and dimethylaminoboron are used. Dimethylaminoborane; DMAB), hydrazines, fuma 14 201021054, etc. Before the surface of the core particle is captured by the noble metal ion, sensitization (sensi1; izing) treatment of adsorbing tin ions on the surface of the particle can be applied. When the surface of the particle is adsorbed with tin ions, for example, the core material subjected to the surface modification treatment may be introduced into an aqueous solution of vaporized stannous and stirred for a predetermined period of time. The core material particles subjected to the pretreatment described above and the dispersant are contained. It is mixed with an electroless plating bath of nickel ions. The electroless plating bath is a water-based solution. For the dispersant contained therein, for example, Ionic surfactants, zwitterionic surfactants, and water-soluble polymers. For nonionic surfactants, polyethylene glycol (polye1:hylene glyc〇i), polyoxyethylene alkyl ether, a polyoxyalkyl Iether lene ether-based surfactant such as p-butyloxyalkylphenyl ephenyl (her). For the zwitterionic surfactant, an alkyl dimethyl group can be used. An alkyldimethyl acetate betaine, an alkyl dimethyl carboxyl methyl acetate betaine, an alkyl dimethyl amino acetate betaine, or the like Betaine surfactant. As the water-soluble polymer, polyvinyl alcohol (polyvinyl aic〇 hQl; PVA), polyvinyl pyrrol idinone, hydroxy ethy 1 cellulose or the like can be used. The amount of the dispersant used is related to the type thereof, but it is generally 0.5 to 30 g/L with respect to the volume of the liquid (electroless plating bath). In particular, when the amount of the dispersant used is in the range of 1 to 10 g/L with respect to the volume of the liquid (electroless electroless bond bath), it is preferable to improve the adhesion of the film of the nickel skin 15 201021054.

The 鉾龅 B contained in the electroless plating bath is used as the knot M ion, and the water-soluble nickel is used as the H-origin. As for the water-soluble salt, it can be used, but it is not limited to this. Electroless ‘,,,,, 〇·_Η, Mohr/L, and +1 contain recorded ion inversions in liters per liter. It is better to raise the special 疋. 005 在 在 In the electroless electroplating bath, the above-mentioned composition is contained. With regard to the reducing agent, the reducing agent can be used to reduce the same reducing agent. Helmet Thunder City

Approximately .0 moor/eight liters: The concentration of reducing agent in the medium is 4X liters.尔 / 升, especially preferably 2. 〇χΠΓΜ). 2 Moor / Gong In the electroless plating bath, can be more m, Η -,, more 3 have a wrong agent. The advantageous effect of the carboxylic acid hydrazine JLai#, which inhibits the decomposition of the plating solution, is achieved by the inclusion of a distoring agent. It can be exemplified that organic defiant A (such as lemon acid), western π # 幺 acetic acid (hydr〇xyacetic or its metal salt, :: di = gluconic acid - (4), etc., can be used one or two The concentration of the staggering agent in the electroless electrothermal ore bath is 〇〇〇5 liters, especially preferably 〇, 〇 3 3 摩尔/liter liter, er, and The method of mixing the electroless plating bath is not particularly limited. The illusion can be first heated to an electroless plating bath to a nickel-reducible, itch, dish, and in this state, the core that has been treated before The material particles are put into the suilei two..., in the electric mine bath. By this operation, 'reducing the nickel ions', the original film layer is formed on the surface of the core material particles by the reduction of the &&&& The initial film; s & 曰, the formation thickness is preferably 0.1~l〇nm, more preferably 16 201021054 0·1~5mn. At this time point, no protrusion is formed. The focus of step A is electroless plating. The relationship between the amount of the monument ion contained in the bath and the amount of the core material to be charged. In other words, it has been adjusted to a concentration of nickel ions of 〇.000 〇.008 摩尔/liter, and a liter of an electroless electrolysis bath of preferably 0.0001 to 0.005 mole/liter of 1 liter. The total surface area used is a core material particle of 15 m 2 , particularly preferably 2 to 8 melons, whereby an initial thin φ film layer having the above thickness can be easily formed. Further, by the amount of nickel ions The amount of the core material particles is as described above. The aggregation of the core material particles in which the initial film layer has been formed can be effectively prevented. In this case, when the particle diameter of the core material particles is small, for example, the particle diameter is 3 The following conditions are particularly effective. After the reduction of the recorded ions is completed, the step B is performed next. The step B is carried out in the subsequent step A, and the core material particles having the nickel initial film completed in the step a are not separated from the liquid, etc. Therefore, in the aqueous slurry containing the core material particles having the nickel initial film, the dispersant added in the step 8 is still left. In the step B, it is the initial stage of the nickel completed in the step A. Film core pellet In the aqueous slurry containing the dispersant used in the step A, nickel ions and a reducing agent are added over time. The meaning of "addition 1±addition" means that not all of the recorded ions and the reducing agent are added at a time. Rather, it is necessary to continuously or intermittently add nickel and a reducing agent for a fixed period of time. In this case, the time at which the recording ions and the reducing agent are added may be all the same; or it may be added first. Nickel ions, followed by the addition of a reducing agent; may also be in the reverse order described above. Also, with respect to the end point of the addition, the addition of nickel ions may be terminated first, followed by the addition of the reducing agent 17 201021054, or the reverse order described above. . Regarding the ion source of the nickel ions used in the step B, the same ion source as used in the step A can be used. The same applies to the reducing agent.乂

In the step B, by the reduction of nickel ions, firstly, the micronuclear particles are formed in the liquid, and the pronuclear particles are attached to the surface of the core material particles having the nickel initial film completed in the step A, and The raised particles are grown by using the attached nuclear particles as a starting point to form protrusions. By adopting this method, aggregation of particles can be effectively prevented, and protrusions having an aspect ratio of 1 or more can be easily formed. On the other hand, the (four) reading towel described in the prior art item of the present specification first forms a recorded film on the surface of the riding particle, and forms a pregnancy (step-step) as a starting point of generation of the protrusion; Next, the nucleus is grown in the next step to form a protrusion (first step). In this method, since it is necessary to make the concentration of the nickel ions in the first step relatively high, the formation of particles is condensed and thus the particles are likely to be coagulated. In addition, it is difficult to form a protrusion having a high aspect ratio.

Regarding the reduction of the recorded ions in the step B, it is important to maintain the aqueous dip in the pH range of the dispersing effect of the dispersing agent added in the step A (the additive remains in the step B). Thereby, aggregation of particles with each other can be effectively prevented. For the adjustment of the pH, it is sufficient to add a variety of inorganic acids or the like, or a base such as sodium hydroxide to the aqueous slurry while superimposing the slurry (iv). The adjustment range of the pH value may be an appropriate value as long as it is a used powder. In the case of using, for example, a nonionic interface <RTIgt; lingual agent as a dispersing agent', it is preferred to maintain the pH of the aqueous slurry in the range of 5 to 1 Torr. In the case where a zwitterionic surfactant is used as the dispersant in the case of 2010 201054, it is preferred to range the water. The use of a water-based polymer as a binary value: holding: w is good to maintain the value of the aqueous slurry in the range of 5 to 8 'the same as the amount of nickel ion ions in the step B is added to Nickel 1 X of the aqueous slurry and 1 of the reducing agent are also important points. By forming the protrusions with high aspect ratio well, "from beginning to end,,., about the specific conditions, adding nickel per hour to the aqueous slurry over time,

For 4 〇, the amount of ions required for nra and: 25~1〇_, the relative addition conditions, relative to the initial J layer and by the use of the above nickel precipitation will occur preferentially in the nucleus particles, and It is easy to form a protrusion having a high aspect ratio. With regard to the addition of nickel ions and a reducing agent, the aqueous slurry can be heated to a predetermined temperature to smooth the reduction of nickel ions caused by the reducing agent. For the addition of the lock ion and the reducing agent, the aqueous slurry can be stirred first. The adhesion of reduced nickel occurs in the hook. As described above, the target conductive particles are completed. This conductive particle can be post-processed as needed. As the post-treatment, there may be mentioned an electroless gold plating step or an electroless palladium plating step. By adding this step, a gold plating layer or a palladium plating layer is formed on the surface of the conductive particles. The formation of the gold plating layer can be carried out according to a conventional electroless plating method. For example, in an aqueous suspension of conductive particles, tetrasodium ethylenediamine (e1:raaceta1;e), disodium citrate, and gold potassium cyanide are added to adjust the pH by adding sodium hydroxide. An electroless plating solution can form a bond gold layer. In addition, the formation of the ore layer can be based on the conventional electroless electrowinning method. 19 201021054 For example, in an aqueous suspension of conductive particles, a water-soluble compound such as vaporized palladium is added; hypophosphorous acid, phosphorous acid, formic acid, acetic acid, hydrazines, hydrogenated butterfly, and amine-based consortium (amjne) a reducing agent such as a compound or a salt thereof; and a commonly used electroless palladium plating solution such as a distorting agent; and a dispersing agent, a stabilizer, and a pH buffering agent are added as needed. Then, the pH is adjusted with an acid such as hydrochloric acid or sulfuric acid or a base such as sodium hydroxide, and a reduction-type electroless plating is simultaneously performed to form a palladium plating layer. In another method, a palladium ion source miscluster such as tetraammine palladium salt or a dispersant according to requirements may be added to an aqueous suspension of conductive particles, and a substitution reaction between palladium ions and nickel ions may be used. Displacement type electroless plating is performed to form a palladium plating layer. In order to form the above-mentioned plating layer, in the case of electroless plating, for example, acid). Further, the palladium plating layer is preferably substantially free of phosphorus or has a phosphorus content of 3% by weight or less because it contributes to electrical conductivity and electrical reliability. For example, a replacement type electroless plating or reduction may be used, and a phosphorus-free reducing agent may be used (for example, in the replacement type #t胄 plating or reduction type 纟 electrolytic heat 1: deplating

20 201021054 It is more convenient to set the weight of the disposable particles relative to the weight of the control body to the above range. The conductive AM·.# rain-powered particle of the present invention thus completed is suitable for, for example, an anisotropic conductive film (ACF), a heat-sealed connection ttCp. _ ytieat seal connector; SC), for smashing a liquid crystal display The electrode is connected to a conductive material or the like of the circuit board of the LSI wafer for driving. τ is specifically intended to be used as a conductive filler which is conductively incident on the conductive powder of the present invention. ❿ The conductive adhesive agent described above is preferably used as an anisotropic conductive adhesive which is disposed between two substrates on which a conductive substrate is formed and which is heated and then connected to the conductive substrate. . The anisotropic conductive adhesive contains the conductive particles of the present invention and an adhesive resin. The binder resin can be used without any particular limitation as long as it is insulative and can be used as a successor, and a thermoplastic resin or a thermosetting (tetra) grease can be used, and it is preferred to exhibit a function of heating by heating. The above-mentioned adhesive resin is, for example, a thermoplastic type, a thermosetting type, an ultraviolet curing type or the like. There are also so-called semi-thermosetting type, thermosetting type and ultraviolet type composite type which exhibit intermediate properties of a thermoplastic type and a thermosetting type. These adhesive resins can be appropriately selected in accordance with the surface characteristics, the use form, and the like of the circuit board to be adhered. It is particularly preferable that the binder resin is composed of a thermosetting resin because the material strength after the subsequent one is excellent. The adhesive resin' is specifically selected from the group consisting of ethylene-vinyl acetate copolymer, carboxy modified (carb xy pm 〇 f ethylene) copolymer, and isobutyl acryl. Pseudo) copolymer, polyamine, polyimine, polyester, polyethylene ether (p0lKinyl 21 201021054 ether), polyvinyl butyral (PVB), polyurethane, SBS block copolymer (sbs block copolymer), carboxyl modified SBS copolymer, SIS copolymer (SIS copolymer), SEBS copolymer, maleic acid modified SEBS copolymer, polybutylene rubber (p〇1 ybutadiene rubber) ), chloroprene rubber, carboxyl modified chloroprene rubber, styrene-butadiene rubber, isobutylene-isopentadiene (18 0 "6116" copolymer, acrylonitrile A polybutylene rubber (hereinafter referred to as ^^), carboxyl modified NBR, amine modified NBR, epoxy resin, epoxy resin (ep〇xy ® ester resin), acrylic resin, resin or One or more of Jushixi oxygen tree wax, etc. The composition obtained by the combination is prepared as a main component. Among the above, the thermoplastic resin is preferably styrene-butadiene rubber, SEBS or the like because of its excellent reworkability, and the thermosetting resin is preferably an epoxy resin. Among these, from the viewpoints of high adhesion, excellent heat resistance, excellent insulation, and low melt viscosity, which can be connected under low pressure, the epoxy resin is preferred. As the epoxy resin, as long as it is a polyvalent epoxy resin having two or more epoxy groups in one molecule, an epoxy tree generally used can be used. For specific examples, such as varnish resins such as novolac (novolac) and cresol (cres〇1 N〇v〇lac); bisphenol A, bisphenol F, bisphenol AD, resorcinol (res〇rcin), polyphenols such as tushydroxydiphenyl ether; ethylene glycol (ethylene glyC〇i), neopentyl glycol (ne〇pentyl, glycerin, dimethylolpropane) (trimethyl〇1叩叩(10)e), polypropylene 22 201021054 Polyols such as polyol glycol; ethylenediamine, triethylenetetramine Polyamine-based compound such as 1 ine); polyvalent carboxyl compound such as adipic acid, phthalic acid or isophthalic acid, and epichlorohydrin or Epoxypropyl φ (glycidyl) type epoxy resin obtained by the reaction of 2-methylepichlorohydrin (2-me1: hylepichlorohydrin), and dicyciopentadiene epoxide, Fat such as epoxidized butadiene dimer die P〇xide And a cycloaliphatic epoxy resin or the like. The above-mentioned materials may be used singly or in combination of two or more kinds thereof. The above-mentioned various kinds of the following resins are preferably used such that the impurities (Na, n, etc.) are reduced, and water-decomposable gas or the like is used. The high-purity product can prevent ion migration. The conductive particles of the present invention in the anisotropic conductive adhesive are used in the weight-retaining weight of the adhesive component, usually 0. H0 weight injury, preferably 0. 5 to 25 parts by weight, the amount of conductive particles used is 2 parts by weight, and the adhesion, melting viscosity, and the like are improved, and the connection is increased: by: suppressing the anisotropy of the contact electrical connection. It is sufficient to ensure that in addition to the above-mentioned conductive particles, it can be added within the range known in the art. In addition to the imparting agent, the auxiliary reaction, the anisotropic conductivity, and then the sword and the adhesive resin, The additive of the present technology, the addition amount of 9 can also be used in the present technology for other additives, exemplified by 23 201021054 agent, epoxy resin hardener, metal oxide, photoinitiator, sensitizer, hardener, sulfurization Agent Agents, heat-resistant additives, heat transfer enhancers, softeners, pigments, various couplants, metal passivators, etc. Examples of the viscous agent can be exemplified by rosin (sin), rosin derivatives, terpene resins ( Terpene resins), terpene-phenol resin, petroleum resin, coumarone-indene resin, styrene resin, isoprene resin, alkylphenol resins ), xylene resin, and the like. The co-reagent, that is, the crosslinking agent, may, for example, be a polyalcohol (p〇ly〇1), an isocyanate, a melamine resin, a urea resin, a urotropine, an amine, an acid anhydride, or the like. Peroxide and the like. The epoxy resin hardener is not particularly limited as long as it has two or more active hydrogens in one molecule. Specific examples of the particles include diethylene triamine, triethylenetetramine, metaphenylenediamine, and dicyandiamide (<11〇)^11(^31111(16). Polyamine-based compound such as polyamidoamine (卩〇1}^11^(1〇31^!16); phthalic anhydride, methylnadic anhydride, An organic acid anhydride such as a hexahydrophthalic anhydride or a pyromellitic anhydride; a varnish resin such as a varnish or a phenol varnish; and the like may be used alone or in combination of two or more. A latent hardener can also be used depending on the application, demand, etc. Examples of the latent hardener which can be used include, for example, imidazole, hydrazide, boron trifluoride-amine, 201021054. Compound, strontium salt (ph〇SPh〇niuffi salt, amine i] nide), polyamine salt, dicyandiamide, etc. and the above modified substances. Or use as a mixture of two or more. The conductive conductive adhesive is a manufacturing apparatus which is generally used between those having ordinary knowledge in the technical field to which the present invention pertains, and modulates the conductive particles and the adhesive particles of the present invention, and also uses a hardener as required. And various additives, etc., when the adhesive resin is a thermosetting resin φ, it is produced by mixing in an organic solvent; when the adhesive is a thermoplastic resin, the temperature is higher than the softening point, and specifically, it is preferably about 50 to 130 C. Further, it is preferably produced by melt-kneading at a temperature of about 60 to 110 ° C. The anisotropic conductive adhesive thus obtained can be used for coating or a film. [Examples] The present invention will be described in more detail by way of examples. However, the scope of the present invention is not limited to these examples. Φ [Examples 1 to 4] (1) Step A uses the particle diameter shown in Table 1, true A spheroidal styrene-cerium dioxide composite resin having a specific gravity of 1.1 (manufactured by Nippon Shokubai Co., Ltd., trade name: SOL 10STAR) is used as an anger material particle, and 4 〇g of this core material particle is cast while being mixed. Into 400 mL of a condii (ioner) aqueous solution ("CLEANER-CONDITIONER231" by Röhm and Haas Electronic Materials KK). The concentration of the tempering aqueous solution is 40 ml/L. Next, the liquid temperature at 60 °C. While applying ultrasonic waves, the mixture was mixed with 25 201021054 for 30 minutes to carry out surface modification and dispersion treatment of the core particles. The aqueous solution was filtered and subjected to a repulp water-washed core material particle to obtain a slurry of the second test. 200 ml of an aqueous solution of vaporized stannous solution was placed in the slurry. The degree of this aqueous solution is 5xl{r3mQl/L. The mixture was incubated for 5 minutes under a constant overflow to sensitize the surface of the rag particles to the tin ions. Next, the aqueous solution was filtered and washed once with water. Next, the core material particles were made into 400 ml of the mass material 'maintained at 6 Gt. - And use ultrasonic waves, face-to-face mixing slurry, and add 2 mL of 气·1 im〇i /l gasification fluid solution on one side. This pull-up type was maintained for 5 minutes, and an active treatment for capturing palladium ions on the surface of the core particles was carried out. Next, 20 g/L of sodium tartrate, 5.4 g/L of sodium hypophosphite, nickel sulfate hexahydrate of the concentration shown in Table 1, and a dispersing agent of the type and concentration shown in the above table were dissolved to form an aqueous solution, and the aqueous solution was dissolved. The formed 3 liter electrolytic bath was heated to enthalpy, and the core material particles of the structure were put into the electroless plating bath in the amounts shown in the same table, and the A step was started. In addition, the specific contents of the dispersing agent shown in Table 1 are shown in Table 2. After stirring for 5 minutes and confirming that the helium gas bubbles have stopped, the step A is ended. Lu (2) Step B uses a mixed aqueous solution of 30 0 mL of 224 g/L of nickel sulphate solution and 210 g/L of sodium hypophosphite and 8 〇g/L of sodium hydroxide by means of a quantitative pump. The above aqueous solution is continuously added to the slurry of the core material particles completed in the step a, respectively, and the electroless plating step is started. The addition rate was 2·5 mL/min. The specific conditions of this step are shown in Table 3. After adding the liquid, keep it at 7 (rc temperature, continue stirring 26 201021054 minutes. Next, filter the liquid, and the gentleman will clean the material for three times, v

A 100C vacuum dryer was used for drying, followed by M conductive particles. The image of the scanning electron microscope (SEM) of the conductive particles formed in the skin of the example was shown to be a continuous body of the nickel film and the protrusions in the evaluation type electric particles. [Examples 5 to 23] Conductive particles were completed in the same manner as in Example 1 except that the human step and the B step were carried out under the conditions shown in Tables 1 and 3. However, in the step B of Example 19, the amount of addition of the aqueous solution of the #p, -7 township, and the mixed aqueous solution containing sodium hypophosphite and sodium oxychloride is said. Further, in the step B of Example 20, the amount of the mixed solution of the material and the mixed aqueous solution of sodium ytterbium and sodium oxyhydroxide was divided into 39 QmL. Further, the addition amount and the lowering speed of the aqueous solution of the sulfuric acid recorded in Examples 21 to 23 and the mixed aqueous solution containing sodium sub-sodium sulphate and sodium sulphate were respectively 15 Å, and the test was carried out; H1.9H/min. Thus, the conductive particles having the recording-disc alloy film were completed. [Example 24] Modification of EDTA-4Na of l〇g/L, citric acid-2Na of l〇g/L, and gold potassium cyanide of 2.9 g/L (2〇g/L in the case of Au) An electroless gold plating bath is constructed. Two liters of this gold plating solution was heated to 79 〇c, and 10 g of the conductive particles prepared in Example 2 were added while stirring the gold plating solution. Thereby, electroless plating treatment is performed on the surface of the particles, and the treatment time is 2 〇 minutes. After the treatment was completed, the liquid was filtered, and the filtrate was repulped three times. Next, it was dried by a vacuum dryer of no °c. In this way, the nickel-27 201021054 phosphor alloy coating is coated with a gold plating layer. [Examples 25 to 27] A solution of 10 g/L of EDTA-4Na, 10 g/L of citric acid-2Na and 20 g/L of tetraammine palladium hydrochloride (Pd(NH3)4Cl2) was prepared. 2. An electroless palladium plating bath composed of Og/L), 100 ppm of carboxymethylcellulose (having a molecular weight of 250,000 and an etherification degree of 90). 65 liters (Example 25), 1.3 liters (Example 16), and 2.6 liters (Example 27) of this palladium plating solution were heated to 7 (TC ' while stirring the palladium ore solution while adding 10 g of the conductive particles prepared in Example 2. The electroless plating treatment was performed on the surface of the particles, and the treatment time was 6 minutes. After the treatment was completed, the liquid was filtered, and the filtrate was subjected to 3 times. Next, it was dried by a vacuum dryer of litre. As a result, a palladium plating layer was applied on the nickel-phosphorus alloy film, and phosphorus was not contained in the palladium film. [Comparative Examples 1 to 7] /17 In the same way as the embodiment, the method of "fourth"-scale alloy film and conductive particles is completed. However, in the step B of Comparative Example 3, the aqueous solution of the sulfuric acid chain and the sub-containing sodium and sodium hydroxide are contained. The amount of the mixed aqueous solution added was 2 Hz. In addition, the addition amount of the aqueous solution of the sulfuric acid solution of Comparative Examples 5 to 6, the mixed aqueous solution of the sub-sub-disc and sodium hydroxide, and the low-speed distraction 38, 120 0 mL; 3, 1〇〇mi / 八# So, complete with nickel 1 alloy skin Conductive particles. The image of the comparison is shown in Fig. 2. Conductivity (1) completed in 1 [Comparative Example 8] 201021054 The same plating gold as in Example 24 was applied to the conductive particles produced in Comparative Example 2. The coating treatment was carried out. [Physical property evaluation] The particle diameter of the conductive particles, the thickness of the nickel film, the thickness of the gold film, the thickness of the palladium film, the surface state, and the nickel film were measured and evaluated in each of the examples and the comparative examples. Adhesiveness and electrical conductivity. In addition, the application of the gold plating layer was evaluated, and the adhesion of the gold film was evaluated. The adhesion of the palladium coating was evaluated by the application of the palladium coating. The evaluation of each physical property is based on the following. In addition, the ratio of the aspect ratio of the protrusions, the ratio of the protrusions 高 having an aspect ratio of i or more, the ratio of the primary particles in the conductive powder, and the particle diameter of the conductive particles are respectively described by the above method. The above results are shown in Tables 4 and 5. [Thickness of Nickel Film] The conductive particles are impregnated with aqua regia to dissolve the nickel film, and the film components are analyzed by ICP or chemical analysis, and the following formula (1), (2) Calculate the skin A=[(r + t)3-r3]d, /r3d2 (1) A=W/(l〇〇-f) (2) where r is the radius of the core particle and the thickness of the nickel film, Dl is the specific gravity of the nickel film, d2 is the specific gravity of the core material particles, and w is the ratio of nickel content (weight [thickness of gold film and palladium film]. The conductive particles are immersed in aqua regia to dissolve gold or palladium film and nickel barium. The composition of the film is analyzed by ICP or chemical analysis. Then, the thickness of the gold or palladium film is calculated from (3) and (4) of 29 201021054. B=[(r+t + u)3-(r + t)3]d3/(r+t)3d4 (3) B=X(100-X) (4) where 'u is the thickness of gold or palladium film, d3 is the specific gravity of gold or palladium film, di is chain The specific gravity of the product, X is the content of gold or the weight (% by weight). Here, the gravity of the nickel product is calculated using the formula. The specific gravity is calculated using the formula of (5) below. D4=W/[(W/di)+(l〇〇-W)/d2] (5) where d! is the specific gravity of the nickel film, & is the specific gravity of the core material particles, and w Θ is nickel-containing Proportion (% by weight). [Surface state] Using SEM, the conductive particles were magnified three times, and one field of view was observed, and the average value of the number of the protrusions of one conductive particle was calculated. 10,400 records are 〇, and 10 or less are recorded as △. In addition,

Record the abnormal analysis of A (4) record as x. The abnormality analysis refers to, for example, a case where nickel is not precipitated on the surface of the core particle and precipitates in the liquid. ^ [Adhesiveness of the film] ... π... The oxidizing particles of 90 g and the diameter of lmln were placed in a beaker of lGGmL and 1 (1 mL) of toluene was further added. After the cartridge is removed, the oxidized material is mixed with the slurry (4) and dried. 1 The conductive particles after drying were magnified, and the average value of the number of peeling sheets produced by stirring in 1 G of observations was observed. Peeling "Unsatisfactory 1G bellows records as 〇, 1G~3Q records as △ and records as X. 30 201021054 [Electrical conductivity] 100 parts of epoxy resin, 150 parts of hardener, 70 parts of stupid Kunming's modulation of the edge and the edge of the agent. The 胄15 money 胄 electrical particles are mixed with the insulating adhesive to complete the paste. Using a bar coater, the paste is applied to the sputum. Oxygen-treated polyester film and dried. The finished coating film was used to climb between the fully-evaporated aluminum glass and the copper-imprinted polyimide film substrate having a pitch of 50 Am. The conductivity of the conductive particles is evaluated by measuring the on-resistance between the electrodes. The evaluation is as follows: those with a resistance value of 2 Ω or less are recorded as 〇, and those with a value of 2 Ω are recorded as Δ, and 5 Ω or more are recorded as . The first one records whether there is a short circuit. [Table 1] ΑStep core material particle distribution ---- ---- MI concentration (ε/ΤΛ NiS〇4 (g/L) Ϊ Example particle size (#m) Mixing amount ( g) sum of surface areas (m2) type 1 5.0 15.0 16.3 A 5 η αγ. 2 3.0 9.0 16.3 A 5 U. 40 n 3 2.5 7.5 16.3 A 5 U. *i O Π AK 4 2.0 6 16.3 A U. 4D 0.45 5 2.5 7.5 16.3 B~ K 0.45 " 6 2.5 7.5 16.3 C ϋ -- 5 n V 2.5 7.5 16.3 D 5 U. rtJ Π AK 8 2.5 7.5 16.3 E 5 U 40 Ω 9 2.5 7.5 16.3 F ~~~~5_ 0. 45 _10 2.5 7.5 16.3 5 π 11 2.5 7.5 16.3 H 5_ U. 0.45 12 2.5 7.5 16.3 5_ 0.45 13 2.5 7.5 16.3 1 14 2.5 7.5 16.3 A 10 U. 40 n AK lb 2.5 7.5 16.3 A 5_ u. ftJ 0. 23 16 2.5 7.5 16.3 ——--- A 3f) π AK IV 2.5 7.5 16.3 A U. 40 0.9 31 201021054 18 2.5 7.5 16.3 A 5 1.8 19 2.5 7.5 16.3 A 5 0.45 20 2.5 7.5 16.3 A 5 0.45 21 2.5 3.8 8.2 A 5 0.45 22 2.5 5.7 12.3 A 5 0.45 23 2.5 15 32.7 A 5 0.45 1 2.5 7.5 16.3 No 0 4.5 2 2.5 7.5 16.3 A 5 4.5 Ratio 3 2.5 7.5 16.3 A 5 4.5 vs. 4 2.5 7.5 16.3 A 5 0 Case 5 2.5 1.0 2.2 A 5 0.45 6 2.5 30 65.4 A 5 0.45 7 2.5 7.5 16.3 No 0 0.45

[Table 2] A polyethylene glycol B 'polyethylene glycol alkyl ether C polyethylene glycol alkyl phenol ether D alkyl dimethyl carboxy methyl acetate betaine E alkyl dimethyl acetate betaine F alkane Glycidylaminoacetate betaine G polyvinyl alcohol H polyvinylpyrrolidone I hydroxyethyl woven vitamin [Table 3] Step B

Pr Permeation of nickel per hour (nm) Real 1 5. 7-6. 2 49 Application 2 5. 8-6.2 48 Example 3 5. 7-6.1 49 4 5. 6-6.1 48 5 5. 6-6. 2 48.5 6 5. 6-6.1 48 32 201021054

7 5. 6-6. 2 48 8 5. 7-6. 3 48 9 5. 7-6. 2 48 10 5.7-6.2 48 11 5. 6-6. 3 48 12 5. 7-6. 3 48 13 5. 7-6.2 47.5 14 5. 6-6.1 48. 5 15 5. 7-6.2 48 16 5. 7-6. 5 30 17 5.5-6.2 48.5 18 5.3-6.2 48 19 5. 6-6. 2 48.5 20 5.7-6.2 47.5 21 5. 8-6. 3 46 22 5. 7-6. 2 48.5 23 5.7-6.2 47.5 1 4.2-6.1 47.5 2 4.2-6.2 48.5 Ratio 3 4.1-6.3 47.5 4 4. -6. 3 47.5 Example 5 5. 8-6.2 46 6 5. 8-6. 2 48 7 5. 5-6.1 47.5 * The range of pH is the transition from the start of dripping to the end of dripping. 33 201021054 [2] j ratio of primary particles to sub-particles (%) CD OO CT> LO CJ5 CO 〇i CO 03⁄4 ΙΛ σ> ΙΛ 〇> LO σ> LO CD CT> Od σ> 55 CO 〇d σ» CD 03⁄4 CO CD tn 03 σ» σ> OO CO σ> g CN1 σ>L〇σ> CO 〇> LO σ> 05 protrusion|aspect ratio 1 or more ratio j case (%) in in LO § 03 CO 〇> §§ CO CO CO CO § in LO 5 C^I CO OO m 00 CO s CO § in L〇in CO CQ ir> ΙΛ CO s 03 LO OO 呀LT3 LO 1—( CO CNI T~H ΙΛ <NI OJ CO 〇ϊ-H CO C>3 CO CO C<I c- O CO LO 1—H CO LT5 ΙΛ CO rH m CSl r^ CO T—^ CO C<l CO CO CNI CO LO LO o High 1 (βΐπ) 0.232 0.202 〇i—lo C<l CO Gf tn CM o 0.094 0. 082 0.091 0.130 0.133 o 0.124 0. 248 0.192 1 0.088 0.193 1 0.184 1 0.136 0.207 0.175 0.264 0.178 0. 224 0.213 0.244 1 0.245 ^ix W 0.160 0.164 (>3 12 O oa CO o CO (M ot-H c> 0. 085 0.075 0.074 0.112 0.108 0.095 丨0.113 0.162 0.123 ! 0. 065 | 0.155 I 0.163 | 0.108 0.183 0.108 | 0.163 0.135 0.200 0.185 0.212 1 0.223 Discs, discs, discs, discs, discs, discs, discs, discs, discs, discs, discs - conductive recordings The adhesion of the film 〇〇〇〇〇〇〇〇〇〇〇〇〇〇〇<3 〇〇〇〇〇〇〇〇〇〇〇椹 )) 〇〇〇〇〇〇〇〇〇〇〇〇〇〇 〇〇〇〇〇〇〇〇〇〇〇δ* p \o 1 Thickness of palladium flag (nm) CD 〇ooo ◦ O 〇〇> oo CD o O 〇〇O oo C3 O oo cr>c=> CO s Thickness of gold flag (nm) I 〇o 〇> ooo c>cr> ooo 〇ooooo C5 o 〇ooo in CNI c? oo Thickness of nickel 骐 (nm) I OO 05 CD Oi 〇0 05 CD σ» CD O) CD 05 CD 05 CO σϊ CO CJ5 CO 03⁄4 ΙΛ CT> CO cn g & CO 03⁄4 LO c- T--1—< OJ cs [>* C3>ir> 〇a LO LO Lft CD 00 CO particle size (βΰί) Cvl ir: CO cc o. az (N oc CN OC OJ OC CN GC <N 〇0 C<1 〇0 CS] OO c<l oc <N OC CN (N t - C1) oc <NI t - < N1 02 OJ Bu 03 00 CNJ 00 (N! 00 is OO CM* CS cn Ϊ ^ « LT > CC > OC > cr Os CC i_n 4 »—H cc 卜 σ; c <>3 r—<<NI<N OJ OZ (N1 <N ir. CN CC CO C- Cvl 1_If._ .蜣珑 众 ^ ^ ± 1- bead silver «chain 刼 ^ electric 麇 · · ^.来坡一·众slai-xiong wedge transport 璀刼Φ蘧2* e^e 201021054 [Table 5] Particle size (private m) Thickness of nickel film (nm) Thickness of gold film (nm) Thickness of palladium film ( Nm) Surface state Nickel film adhesion Conductivity Short-circuited protrusion primary particle ratio (3⁄4) Base length D (//m) Height (^m) Aspect ratio Aspect ratio of 1 or more (%) 1 7.8 95 0 0 〇X Λ has 0. 250 〇. 151 0. 60 15 47 2 4.3 97 0 0 〇X Λ There are 0. 265 〇. 138 0.52 12 68 to 3 3.6 73 0 0 〇X Δ has 0.213 〇. 148 0. 69 30 70 compared to 4 3.3 95 0 0 Δ XX no _*1 -*1 -*1 _*1 76 Example 5 3.3 92 0 0 Δ XX None-*1 *1 78 6 3.4 96 0 0 XX - - _*2 _*2 76 7 5. 5 95 0 0 Δ XX No _*1 _*1 7fi 8 7.8 扪: 74 25 0 〇X Δ There is 0.286 0.189 0.66 15 47 *2 : Nickel is abnormally precipitated and cannot be As is clear from the results of Table 4 and Table 5, the projections of the conductive powder (the present invention) which were completed in each of the examples were clearly observed as compared with the conductive powders obtained in the comparative examples. High and wide, and primary particles A higher proportion. Further, in comparison with the conductive powder prepared in the comparative example, it was apparent that the conductive powder obtained in each of the examples had high conductivity and high adhesion of the nickel film. BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is an SEM image of conductive particles completed in Example 3. Fig. 2 is an SEM image of the conductive particles completed in Comparative Example 1. [Main component symbol description] None 35

Claims (1)

201021054 VII. Patent application scope: 1.-Electrical powders are suitable for forming conductive powders composed of conductive particles of nickel or gold film on the surface of core particles, which are characterized by: The particles have a plurality of protrusions that protrude from the surface of the film and are one or more of the skin and the continuous body and have an aspect ratio "speci: plus"; The ratio of the number of the protrusions having a back-width ratio of 1 or more is 40% or more of the total number of the protrusions; and in the conductive powder, the weight of the primary particles in the conductive particles is the conductive powder The weight of the body is 85% by weight or more. 2. The conductive powder according to claim 1, wherein the core material particles have an average particle diameter of 1 to 3 μm. The conductive powder according to the above-mentioned item, wherein the surface of the film containing the protrusions is covered with gold or palladium. A conductive material of any one of the above-mentioned items of the present invention, which is a conductive material and an insulating resin. A method for producing conductive particles, comprising: a step of mixing an electroless plating bath containing a dispersing agent and nickel ions with a core material particle having a surface-dependent metal, wherein a surface of the core particle is shaped At the time of the initial film layer, the electroless mineral bath of 0.000 H.GG8 Mohr/liter is adjusted to a concentration of 1 liter of the phase material, and the core material particles having a surface area and an amount equivalent to 15 m2 are used; and the step A is performed. The finished core 36 201021054 material particles having the nickel initial film layer, and the slurry containing the dispersant are maintained in a range of pfl values exhibiting the dispersion remaining dispersion effect, and are added hour by hour. (4) the amount of iron ions and a reducing agent in an amount of 25 to 100 ηπ, and the generation of the nucleus particles of nickel in the aqueous pulp, and the generated nucleus particles are attached to the core material particles. The core particles are used as a starting point to grow the pronuclear particles, and a protrusion having an aspect ratio of i or more is formed. 6. The method of manufacturing the conductive particles according to claim 5, wherein the + A # step is performed so that the thickness of the initial nickel of the nickel is 0. 1 Onm 〇 7. If the patent application scope The method for producing conductive particles according to Item 5 or 6, wherein a nonionic surfactant, a zwitterionic surfactant or a water-soluble polymer is used as the dispersant. 37