WO2011114747A1 - 導電性ペースト、及び該ペーストから得られる導電接続部材 - Google Patents
導電性ペースト、及び該ペーストから得られる導電接続部材 Download PDFInfo
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- WO2011114747A1 WO2011114747A1 PCT/JP2011/001615 JP2011001615W WO2011114747A1 WO 2011114747 A1 WO2011114747 A1 WO 2011114747A1 JP 2011001615 W JP2011001615 W JP 2011001615W WO 2011114747 A1 WO2011114747 A1 WO 2011114747A1
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- conductive paste
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- fine particles
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Classifications
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Definitions
- the present invention relates to a conductive paste used for bonding semiconductor elements, circuit boards and the like, and conductive connecting members such as conductive bumps and conductive die bonding parts obtained by heat treatment of the conductive paste.
- the bumps formed by the plating method have a problem of generation of cracks and breakage which are considered to be caused by fatigue failure in the use process.
- flip chip bonding if the constituent materials of the semiconductor element and the circuit wiring substrate mounted on the semiconductor element are different, stress distortion is generated in the solder bump electrode due to the difference in thermal expansion coefficient. This stress strain destroys the solder bump electrode and reduces the reliability life.
- a porous body formed by firing a conductive paste containing metal fine particles is known.
- Patent Document 1 as a connection bump for electrically connecting a conductor wiring circuit and a substrate on a substrate, it is obtained by sintering metal fine particles having an average particle diameter of 0.1 ⁇ m to 50 ⁇ m of metal particles.
- a bump made of porous metal and having a density of 0.2 to 0.9 times that of bulk metal.
- Patent Document 2 proposes a bump made of a porous, relatively soft and elastic sintered material used for the bump. Due to the elasticity of the bumps, even if there is a variation in bump height, the porous body is shrunk by pressure and bonding becomes possible. In addition, distortion is less likely to remain inside, and the decrease in thermal stress is also small.
- Patent Document 3 a porous metal layer made of a third metal is interposed between the first metal layer and the second metal layer, and the first metal layer and the porous metal layer, and Disclosed is a bonding method in which a metal nanopaste in which metal ultrafine particles having an average diameter of 100 nm or less are dispersed in an organic solvent is placed between a second metal layer and the porous metal layer, and bonded by heating. It is done.
- a gold plating layer (first bump layer, height: 10 ⁇ m) is provided in the pores of a photoresist layer provided on a substrate, and gold paste is dropped and filled thereon as metal paste.
- a bump provided with a sintered body (second bump layer) by sintering.
- Patent Document 5 a sublimable substance is completely dissolved in an organic solvent, and the solution is jetted out of the pores into water to precipitate fine particles of the sublimable substance, and the resulting fine particles are added to ferrite powder.
- a method of producing a ferrite porous body which is mixed and fired after molding is disclosed.
- the metal porous body obtained by sintering metal particles of micron size (refer to the size of 1 ⁇ m or more and less than 1000 ⁇ m, the same applies hereinafter) disclosed in Patent Document 1 is nano size (nano size is less than 1 ⁇ m). That is, since the heat resistance stress is lower than that of the metal porous body described below, the problem is that the thermal cycle characteristics are relatively insufficient. That is, the porous body specifically disclosed in Patent Document 1 has a structure in which pores of micron size are present between combinations of micron-sized metal particles.
- the bump spacing (pitch) may be damaged.
- the adhesion at the die bond part which is a connection structure between the semiconductor element and the interposer, is low, mechanical stress (external stress, internal stress) or physical stress (thermal stress) causes the semiconductor die back surface or the interposer connection terminal to the conductive die bond.
- the bonding interface with the part may be partially exfoliated or completely exfoliated.
- a conductive connection member such as a conductive bump or conductive die bond having excellent thermal cycle characteristics is obtained by firing a conductive paste containing nano-sized metal fine particles so that the surfaces of the fine particles are combined and the nano-sized empty It is preferable to use a porous body in which pores are formed, but in the conductive paste, metal microparticles are unevenly distributed, or bubbles generated by evaporation or thermal decomposition of the organic dispersant during heat treatment grow. If coarse voids or cracks are formed inside the porous body, the mechanical strength and the thermal cycle characteristics are significantly reduced.
- conductive metal fine particles having an average primary particle size of 1 to 150 nm in a conductive paste have conductivity similar to that of the fine particles having an average primary particle size of 1 to 10 ⁇ m.
- Conductivity is excellent in bonding strength, with less uneven distribution of pores (voids) and absence of coarse voids or cracks, by blending specific metal fine particles in a certain ratio and using an organic solvent having reducibility as an organic dispersion medium
- conductive connecting members such as conductive bumps and conductive die bonding parts can be obtained, and the present invention has been completed. That is, the present invention is summarized as the inventions described in the following (1) to (17).
- Metal fine particles (P1) having an average primary particle size of 1 to 150 nm and one or more selected from metals and alloys, and metals having the same type as metal fine particles (P1) and having an average primary particle size
- metal fine particles (P) consisting of metal fine particles (P2) of 1 to 10 ⁇ m and having a blending ratio (P1 / P2) of 80 to 95% by mass / 20 to 5% by mass (total of 100% by mass) ,
- Organic solvent (S), or organic solvent (S) and organic dispersion medium (D) comprising organic binder (B), and the mixing ratio (P / D) of metal fine particles (P) to organic dispersion medium (D)
- a conductive paste hereinafter sometimes referred to as a first embodiment, characterized in that 50) to 85% by mass / 50 to 15% by mass) (total of 100% by mass).
- the organic dispersion medium (D) contains water, and the content of water is 75 to 99.9% by mass in the ratio (S / W) of the organic solvent (S) to the water (W)
- the organic solvent (S1) is ethylene glycol, diethylene glycol, 1,2-propanediol, 1,3-propanediol, 1,2-butanediol, 1,3-butanediol, 1,4-butanediol , 2-butene-1,4-diol, 2,3-butanediol, pentanediol, hexanediol, octanediol, glycerol, 1,1,1-trishydroxymethylethane, 2-ethyl-2-hydroxymethyl-1 2,3-propanediol, 1,2,6-hexanetriol, 1,2,3-hexanetriol, 1,2,4-butanetriol, threitol, erythritol, pentaerythritol, pentitol, hexitol and iminodiethanol Characterized in that it is one or more selected from The conductive paste according to
- the organic solvent (SA) is N-methylacetamide, N-methylformamide, N-methylpropanamide, formamide, N, N-dimethylacetamide, 1,3-dimethyl-2-imidazolidinone, N, It is characterized in that it is one or more selected from N-dimethylformamide, 1-methyl-2-pyrrolidone, hexamethylphosphoric triamide, 2-pyrrolidinone, ⁇ -caprolactam, and acetamide.
- the electroconductive paste as described in said (5).
- the organic binder (B) is a cellulose resin binder, an acetate resin binder, an acrylic resin binder, an urethane resin binder, a polyvinyl pyrrolidone resin binder, a polyamide resin binder, a butyral resin binder, and a terpene binder
- the cellulose resin based binder is acetyl cellulose, methyl cellulose, ethyl cellulose, butyl cellulose and nitrocellulose; acetate resin based binder is methyl glycol acetate, ethyl glycol acetate, butyl glycol acetate, ethyl diglycol acetate, and butyl diglycol acetate Acrylic resin binder is methyl methacrylate, ethyl methacrylate, and butyl methacrylate; urethane resin binder is 2,4-tolylene diisocyanate; and p-phenylene diisocyanate; polyvinyl pyrrolidone resin binder is polyvinyl pyrrolidone; and N-vinyl pyrrolidone; A polyamide resin based binder is polyamide 6, polyamide 66, and polyamide 11; The conductive according to (8), wherein the tilar resin-based binder is polyvinyl butyral; and
- a conductive paste according to any one of claims 1 to 10 is placed on a semiconductor element of an electronic component or an electrode terminal of a circuit board or a bonding surface of a conductive substrate, and then further connected on the conductive paste.
- a conductive connecting member comprising a metal porous body formed by arranging the bonding surface of the other electrode terminal or the conductive substrate and sintering it by heat treatment, Between the particles derived from the metal fine particles (P2) having an average particle size of 1 to 10 ⁇ m, the particles derived from the metal fine particles (P1) having an average particle size of 1 to 150 nm were partially bound on the surface
- a conductive connection member (hereinafter, may be referred to as a second aspect) which is present in a state and in which holes are dispersed among these metal fine particles.
- a conductive connecting member comprising the metal porous body according to any one of (11) to (14), wherein the heat treatment temperature of the conductive paste is 250 to 300 ° C.
- a conductive connecting member comprising the metal porous body according to any of (11) to (16), wherein the porosity of the metal porous body is 5 to 35%.
- conductive paste of the first aspect described in the above (1) there are two types of conductive paste comprising metal fine particles (P1) having an average primary particle diameter of 1 to 150 nm and metal fine particles (P2) of 1 to 10 ⁇ m.
- the metal fine particles in the paste are nanoparticles when the conductive paste is heat treated (sintered) to obtain a metal porous body by containing metal fine particles having a particle diameter and the organic solvent (S).
- the metal fine particles (P2) restrict free movement of the nano-sized metal fine particles (P1) in the paste compared with the case of only consisting of bubbles, and the bubbles generated at the time of firing grow to generate coarse voids and cracks.
- the organic solvent (S) is present in a liquid and / or gaseous state between the metal fine particles (P1) and the metal fine particles (P2) and between the metal fine particles (P1) to form a non-oxidizing atmosphere. It forms and suppresses the oxidation of these metal fine particles to promote sintering and promote the formation of dispersed pores.
- the conductive paste of the present invention is fired on the bonding surface of the electrode terminal to form a conductive connection member on the bonding surface of the electrode terminal for bonding electrically and mechanically, bonding strength can be improved.
- the metal fine particles (P) and the pores are dispersed without being unevenly distributed, and there are no coarse voids or cracks, so the thermal cycle characteristics are improved. It is excellent in crack resistance and joint strength.
- Example 7 is an electron micrograph of the cross section of the conductive bump obtained in Example 2.
- the “conductive paste” according to the first aspect is one or more selected from metals and alloys and has an average primary particle size It consists of metal particles (P1) of 1 to 150 nm and metal particles (P2) of the same metal as metal particles (P1) and having an average primary particle diameter of 1 to 10 ⁇ m, and the compounding ratio (P1 / P2) is 80 to 95 mass % / 20-5 mass% (the total of mass% is 100 mass%), and metal fine particles (P), Organic solvent (S), or organic solvent (S) and organic dispersion medium (D) comprising organic binder (B), and the mixing ratio (P / D) of metal fine particles (P) to organic dispersion medium (D) ) Is 50 to 85% by mass / 50 to 15% by mass (the total of mass% is 100% by mass).
- Metal fine particles (P) are composed of metal fine particles (P1) having an average primary particle size of 1 to 150 nm, and metal fine particles (P2) having an average primary particle size of 1 to 10 ⁇ m and the same metal as the metal fine particles (P1).
- the blend ratio (P1 / P2) is 80 to 95% by mass / 20 to 5% by mass (the total of mass% is 100% by mass).
- the metal fine particles (P1) and the metal fine particles (P2) constituting the metal fine particles (P) are the same kind of metal, and are contained in the conductive paste as the metal fine particles (P), and after heat treatment as a conductive connecting member Can be used as long as it exhibits the function of (1), but is selected from copper, gold, silver, nickel, and cobalt in view of conductivity, heat treatment (sinterability), availability in the market, etc. It is preferable that it is 1 type, or 2 or more types.
- the average primary particle size of the metal fine particles (P1) is 1 to 150 nm. If the average primary particle size is less than 1 nm, it may be difficult to form a porous body having uniform particle size and pores by firing.
- the metal fine particles (P1) exist between the metal fine particles (P2) having an average primary particle size of 1 to 10 ⁇ m, so the average primary particle size of the metal fine particles (P1) is 150 nm. If the value exceeds the range, it is difficult to stably exist between the metal fine particles (P2), and the effect of the present invention may not be sufficiently exhibited.
- the average particle diameter of the primary particles means the diameter of the primary particles of the individual metal fine particles constituting the secondary particles.
- the primary particle size can be measured based on transmission electron microscope (TEM) observation. Further, the average particle size means the number average particle size of primary particles.
- the average primary particle size of the metal fine particles (P2) is 1 to 10 ⁇ m.
- the blending ratio (P1 / P2) of the metal fine particles (P1) to the metal fine particles (P2) in the metal fine particles (P) is 80 to 95% by mass / 20 to 5% by mass (the total of mass% is 100% by mass) It is. By setting the mixing ratio, uneven distribution of the metal fine particles (P2) is suppressed in the conductive connecting member made of the metal porous body, which is formed by heating the conductive paste, and the dispersibility is improved. It will be possible to
- Organic dispersion medium (D)
- the organic dispersion medium (D) comprises an organic solvent (S) or an organic solvent (S) and an organic binder (B).
- the organic dispersion medium (D) disperses the metal fine particles (P1) and the metal fine particles (P2) in the conductive paste to adjust the viscosity of the conductive paste, and conductive connection such as a bump precursor and a die bond portion precursor
- the shape of the member precursor is maintained, and in heat treatment, it functions as a reducing agent in the form of liquid and gas.
- the blend ratio (S / B) of the organic solvent (S) to the organic binder (B) in the organic dispersion medium (D) is 80 to 100% by mass / 20 to 0% by mass (the total of mass% is 100% by mass) Is preferred.
- the speed at which the organic binder (B) is thermally decomposed and scattered when the bump precursor is heat-treated becomes slow.
- the amount of carbon remaining in the conductive bump is increased, sintering is inhibited, which may cause problems such as cracking and peeling, which is not preferable.
- the metal fine particles (P1) and the metal fine particles (P2) are dispersed only with the solvent to adjust the viscosity of the conductive paste, and the conductive bump precursor and the conductive die bonding portion precursor
- a component consisting of only the organic solvent (S) can be used as the organic dispersion medium (D).
- Organic solvent (S) is (i) an organic solvent having a reducibility which is composed of an alcohol having a boiling point of 100 ° C. or higher at atmospheric pressure and having one or more hydroxyl groups in the molecule and / or a polyhydric alcohol S1) or (ii) an organic solvent having a reducibility (S1) comprising at least an alcohol having a boiling point of 100 ° C. or more at normal pressure and having one or more hydroxyl groups in the molecule and / or a polyhydric alcohol
- An organic solvent (S2) comprising 5 to 95% by volume, and 95 to 5% by volume of an organic solvent having an amide group (SA) is preferred.
- the organic dispersion medium (D) contains an organic solvent (S1) having reducibility
- the surface of the metal fine particles is first reduced when the conductive paste is heated, and then the surfaces of the fine particles are separated. Since bonding based on sintering is considered to be progressed, when the organic solvent (S1) evaporates continuously and is reduced and fired in the presence of liquid and vapor, sintering is promoted to have good conductivity. A conductive connection member is formed. Therefore, when the organic solvent (S1) is present in the organic dispersion medium (D), a non-oxidative atmosphere is formed during the heat treatment to promote reduction and bonding on the surface of the metal fine particles (P).
- the organic solvent (S2) is more preferably composed of 60 to 95% by volume of the organic solvent (S1) and 40 to 5% by volume of the organic solvent (SA) having an amide group.
- the organic dispersion medium (D) contains water, and the content of the water is 75 to 99.9% by mass in the ratio (S / W) of the organic solvent (S) to the water (W). It can also be 25 to 0.1 mass% (the total of mass% is 100 mass%).
- Many organic solvents (S) to be described later have good affinity to water, so they are easy to absorb water. Therefore, by adding water beforehand, it is suppressed that the viscosity change of the conductive paste occurs with time.
- the amide-based organic solvent (SA) is contained in the above proportion in the organic solvent (S2), mixing with the organic solvent (S1) is good, and when using an organic solvent having a high boiling point as the organic solvent (S1) In this case, the adhesion between the sintered particles after firing and the conductive substrate and the improvement of the connection strength can be expected because the evaporation of the particles is promoted to advance the sintering between the particles.
- organic solvent (S1) examples include ethylene glycol (boiling point 197 ° C.), diethylene glycol (boiling point 244 ° C.), 1,2-propanediol (boiling point 188 ° C.), 1,3-propanediol (boiling point 212 ° C.), 2-butanediol (boiling point 192 ° C.) 1,3-butanediol (boiling point 208 ° C.) 1,4-butanediol (boiling point 230 ° C.) 2-butene-1,4-diol (boiling point 235 ° C.) 2,3-butanediol, pentanediol (boiling point 239 ° C), hexanediol (boiling point 250 ° C), octanediol (boiling point 244 ° C),
- organic solvents (S1) threitol, erythritol (boiling point 331 ° C.), pentaerythritol, pentitol, xylitol (boiling point 216 ° C.), ribitol, arabitol, hexitol, mannitol, mannitol, sorbitol, dulcitol, glycerin aldehyde, dioxyacetone , Treose, erythrulose, erythrose, arabinose, ribose, ribulose, xylose, xylulose, glucose, fructose, mannose, idose, sorbose, gulose, talose, tagatose, galactose, allose, altrose, lactose, xylose, arabinose, isomaltose And sugars such as glucoheptose, he
- the organic solvent (S1) has two or more hydroxyl groups, and the carbon group portion to which the hydroxyl group is attached has a reducing function described later by a polyhydric alcohol having a (-CH (OH)-) structure. It is more preferable from the point which is easy to exhibit.
- the parenthesis shows the boiling point in a normal pressure.
- organic solvent examples include N-methylacetamide, N-methylformamide, N-methylpropanamide, formamide, N, N-dimethylacetamide, 1,3-dimethyl-2-imidazolidinone, N, N Dimethylformamide, 1-methyl-2-pyrrolidone, hexamethylphosphoric triamide, 2-pyrrolidinone, ⁇ -caprolactam, acetamide and the like.
- Organic binder (B) suppresses aggregation of the metal fine particles (P) in the conductive paste, controls the viscosity of the conductive paste, and conductive connecting member precursors such as conductive bump precursors and conductive die bonding portion precursors. Demonstrate the ability to maintain the shape of the As the organic binder (B) having such a function, a cellulose resin based binder, an acetate resin based binder, an acrylic resin based binder, an urethane resin based binder, a polyvinyl pyrrolidone resin based binder, a polyamide resin based binder, a butyral resin based binder, And one or more selected from terpene binders.
- organic binder (R) examples include acetyl cellulose, methyl cellulose, ethyl cellulose, butyl cellulose, and nitrocellulose as the cellulose resin based binder; methyl acetate, ethyl glycol acetate, butyl glycol acetate, ethyl diglycol as the acetate resin based binder Acetate, and butyl diglycol acetate; acrylic resin binder is methyl methacrylate, ethyl methacrylate, and butyl methacrylate; urethane resin binder is 2,4-tolylene diisocyanate, and p-phenylene diisocyanate; polyvinyl pyrrolidone resin binder is polyvinyl pyrrolidone And N-vinyl pyrrolidone; polyamide resin based binder is polyamide 6, polya De 66, and polyamide 11; butyral resin binder is polyvinyl butyral; terpene binder pin
- the conductive paste is a paste-like paste in which the metal fine particles (P) and the organic dispersion medium (D) are contained, and the metal fine particles (P) are uniformly dispersed in the organic dispersion medium (D).
- the metal fine particles (P) are contained in a proportion of 50 to 85% by mass and the organic dispersion medium (D) is contained in a proportion of 50 to 15% by mass (the total of the mass% is 100% by mass).
- the proportion of the metal fine particles (P) exceeds 85% by mass, the paste has a high viscosity, and in the heat treatment, the bonding between the surfaces of the metal fine particles (P) may be insufficient to lower the conductivity.
- the ratio (P / D) of the metal fine particles (P) to the organic dispersion medium (D) is preferably 55 to 80% by mass / 45 to 20% by mass (the total of mass% is 100% by mass).
- the conductive paste when the conductive paste is subjected to heat treatment, evaporation of the organic solvent (S) or evaporation of the organic solvent (S) and thermal decomposition of the organic binder (B) proceed when the temperature reaches a certain temperature, metal microparticles After the surfaces of (P) come in contact with each other, the principle of bonding (sintering) to each other is used.
- the organic dispersion medium (D) is added to the metal fine particles (P) to apply shearing stress, whereby the conductive paste can be prepared by kneading.
- a shear stress for example, a kneader, a kneader such as a three-roll mill, a closed-type kneader, or the like can be used. It is preferable to prevent the oxidation of the copper powder from excessively progressing during the kneading.
- the “conductive connection member” according to the second aspect includes the conductive paste described in the first aspect as an electrode of a semiconductor element or a circuit board in an electronic component.
- a metal porous body formed by placing the bonding surface of the other electrode terminal or conductive substrate to be connected further on the conductive paste after placing on the bonding surface of the terminal or conductive substrate and sintering by heat treatment
- a conductive connection member consisting of a body, Between the particles derived from the metal fine particles (P2) having an average particle size of 1 to 10 ⁇ m, the particles derived from the metal fine particles (P1) having an average particle size of 1 to 150 nm were partially bound on the surface It is characterized in that it exists in a state, and the pores are dispersed among these metal fine particles.
- the conductive connection member includes, but is not limited to, conductive bumps for bonding between semiconductor elements, conductive die bond parts for bonding between semiconductor elements and conductive substrate, and the like. .
- the conductive bump places the conductive paste on the bonding surface of the semiconductor element of the electronic component or the electrode terminal of the circuit board (including coating and printing, etc.), and bonds the other electrode terminal further connected on the conductive paste. After arranging the surface, it is formed by sintering by heat treatment or heat treatment under pressure.
- the other electrode terminal to be connected also includes a wire such as a gold wire when performing wire bonding. In addition, when arrange
- the conductive die bonding portion usually places the conductive paste on the bonding surface of the circuit board of the electronic component (including coating, printing, etc.), and arranges the bonding surface of the other electrode terminal to be further connected on the conductive paste. Then, it is formed by sintering by heat treatment or heat treatment under pressure.
- the heat treatment under pressure secures bonding between the conductive connecting member precursor and the both electrode terminal bonding surfaces or between the electrode terminal and the conductive substrate by pressing between both electrode terminals or between the electrode terminal and the substrate. While making it possible to cause appropriate deformation in the conductive connection member front body to perform reliable bonding with the electrode terminal bonding surface, the bonding area between the conductive connection member front body and the electrode terminal bonding surface becomes large, Bonding reliability can be further improved.
- the space between the semiconductor element and the conductive connection member precursor is sintered under pressure using a pressure type heat tool or the like, the sinterability at the joint portion is improved and a better joint portion can be obtained.
- the pressure between the both electrode terminals or between the electrode terminals and the substrate is preferably 0.5 to 15 MPa. When the pressure is 0.5 MPa or more, the effect of suppressing the formation of large voids in the bonding surface is improved. On the other hand, if it exceeds 15 MPa, the gaps between the conductive metal fine particles (P1) decrease and the porosity decreases. There is a risk of
- metal fine particles (P1) having an average primary particle diameter of 1 to 150 nm and the same metal fine particles as the metal fine particles (P1) consisting of one or more kinds selected from metals and alloys.
- Metal fine particles (P2) having an average primary particle diameter of 1 to 10 ⁇ m, and the compounding ratio (P1 / P2) thereof is 80 to 95% by mass / 20 to 5% by mass (the total of mass% is 100% by mass)
- Organic dispersion medium (D) consisting of 50 to 85% by mass of metal fine particles (P), organic solvent (S), or organic solvent (S) and organic binder (B) (total of 50% to 50% by mass (% by mass)
- a conductive paste consisting of (% by mass) can be used.
- the components of the metal fine particles (P1), the metal fine particles (P2), the organic solvent (S), and the organic binder (B) are as described in the first aspect. Further, as described in the first aspect, it is preferable that the organic dispersion medium (D) is composed of 80 to 100% by mass of the organic solvent (S) and 20 to 0% by mass of the organic binder (B).
- Examples of means for placing a conductive paste on an electrode terminal of a semiconductor element to form a conductive connection member precursor such as a conductive bump precursor or a conductive die bond portion precursor include, for example, known screen printing, a resist described later A method of forming an opening at the connection of the electrode terminal and applying a conductive paste to the opening can be mentioned.
- a screen plate provided with a plate film (resist) is disposed on an electrode terminal or the like of a semiconductor element, a conductive paste is placed thereon, and the paste is slid with a squeegee Then, the conductive paste passes through the screen of the portion without the resist and is transferred onto the electrode terminal etc., to form a conductive connecting member precursor such as a conductive bump precursor or a conductive die bond portion precursor. .
- a photolithographic method of forming a pattern on a photosensitive resin layer through an exposure and development process, high energy rays such as laser light, electron beam, ion beam and the like on the element There is a method of forming an opening in the resin layer by irradiating the insulating resin layer provided in the above and performing ablation by melting by heating or breaking molecular bonds of the resin.
- the photolithography method or the method of forming an opening by ablation using a laser beam is preferable in terms of practicality.
- the alignment for bringing the electrode terminals on the semiconductor element and the electrode terminals on the circuit board into contact so as to ensure electrical connection after the heat treatment (sintering) is, for example, the electrode terminals on the semiconductor element and a tape
- the connection electrode terminal portion of the conductive substrate transported by a reel or the like can be performed using an optical device or the like.
- the conductive connecting member precursor such as a bump precursor formed on the electrode terminal of the semiconductor element or the like and in contact with the pair of terminal electrodes is preferably 150 to 350 ° C., more preferably A heat treatment (sintering) is performed at a temperature of 250 to 300 ° C. to form a conductive connection member, whereby a terminal electrode or the like facing the electrode terminal or the like of the semiconductor element is electrically or mechanically through the conductive connection member. Bond to Although the time required for the heat treatment depends on the type of metal fine particles (P1) to be used and the type of organic dispersion medium (D), it is desirable that the time is about 5 to 30 minutes.
- P1 metal fine particles
- D organic dispersion medium
- the metal fine particles (P1) Since fine particles having an average primary particle diameter of 1 to 150 nm are used as the metal fine particles (P1), if the organic dispersion medium (D) is removed by heating, the energy of the surface lowers the melting point of the metal in bulk state. Bonding (sintering) between the surfaces of the fine particles proceeds to form conductive connecting members such as conductive bumps made of a metal porous body and conductive die bonding parts.
- the conductive paste according to the first aspect is applied to the semiconductor element of the electronic component or the electrode terminal of the circuit board or the bonding surface of the conductive substrate.
- a conductive connecting member comprising a metal porous body formed by placing the other electrode terminal to be further connected on the conductive paste or the bonding surface of the conductive substrate after mounting, and sintering by heat treatment, ,
- the particles derived from the metal fine particles (P2) having an average particle size of 1 to 10 ⁇ m the particles derived from the metal fine particles (P1) having an average particle size of 1 to 150 nm were partially bound on the surface It is characterized in that it exists in a state, and the pores are dispersed among these metal fine particles.
- the conductive connecting member obtained by the above heat treatment is in contact with the metal fine particles (P1) on the surface in a state where the deformation and stress are relaxed in the metal fine particles (P1) as compared with the conductive bumps obtained by the plating method.
- bonding sining
- the conductive connection member such as the conductive bump and the conductive die bond portion, which are obtained in this manner, has a porosity of 5 to 35% by volume, and since the pores are not unevenly distributed, mechanical and mechanical It has excellent electrical bondability, improved thermal cycle characteristics, and excellent crack resistance.
- the void ratio of the conductive bump shaped object or conductive die bond portion is determined by taking an electron micrograph of 1000 to 10000 magnification and observing the cross sectional image using a scanning electron microscope (SEM). be able to.
- conductive bump samples for evaluation were prepared, and in Examples 4 to 6 and Comparative Examples 6 to 10, conductive die bond part samples for evaluation were prepared, respectively. I made an evaluation. The preparation method of the sample for the evaluation test in a present Example and a comparative example is described below. In addition, the evaluation method of a conductive bump and a conductive die-bonding part etc. is mentioned later.
- Example 1 Silver fine particles having an average primary particle size of 60 nm and silver fine particles having an average primary particle size of 5 ⁇ m are mixed in a ratio of 95: 5 (mass ratio) After the addition so as to be%, they were thoroughly stirred to prepare a conductive paste.
- the conductive paste is screen-printed on a conductive substrate (DBC substrate Direct Bonding Copper substrate), and conductive bump precursors (size: 50 ⁇ m ⁇ , thickness: 150 ⁇ m) are provided at four points (4 mm on each side) Position) was applied.
- the gold sputtered surface of a Si chip (shape: a rectangular solid with a side of 4.5 mm) gold-sputtered on studs (50 ⁇ m ⁇ , thickness: 150 ⁇ m) to be paired on the precursor so that the gold sputtered surface faces the precursor surface I put it on.
- the conductive substrate on which the Si chip is mounted is heat treated at 200 ° C. to sinter the silver fine particles contained in the conductive paste, and the conductive substrate and the terminal of the Si chip are electrically and mechanically
- the conductive bump joined to was produced.
- Example 2 Copper fine particles having an average primary particle diameter of 120 nm prepared by electroless reduction from copper ions in an aqueous solution and copper fine particles having an average primary particle diameter of 7 ⁇ m prepared by the same electroless reduction are 90:10 (mass The conductive paste was prepared in the same manner as in Example 1 by mixing in a ratio and adding glycerol as an organic solvent having reducibility to the mixture so that the copper fine particle concentration became 80% by mass. The conductive substrate and the terminal of the Si chip are electrically and mechanically joined in the same manner as described in Example 1 except that the obtained conductive paste is used and the heat treatment temperature is set to 300 ° C. Conductive bumps were fabricated. Evaluation similar to Example 1 was performed about the obtained conductive bump. The evaluation results are shown in Table 1.
- Example 2 the electron micrograph of the electroconductive bump cross section obtained in Example 2 is shown in FIG. From FIG. 1, sintered particles derived from copper microparticles having an average primary particle diameter of 7 ⁇ m are dispersed and present in the conductive bumps, and derived from copper microparticles having an average primary particle diameter of 120 nm around the sintered particles. It is observed that sintered particles are present and no coarse voids or cracks are present.
- Example 3 Copper microparticles having an average primary particle size of 120 nm and copper microparticles having an average primary particle size of 7 ⁇ m are mixed at a ratio of 90:10 (mass ratio) as used in Example 2 and 80 vol% of glycerol and N as an organic solvent -A mixed solvent consisting of 20% by volume of methyl acetamide is used, and a conductive paste adjusted to have a copper fine particle concentration of 75% by mass is used, and the heat treatment temperature is set to 300 ° C.
- a conductive bump was produced in which the conductive substrate and the terminal of the Si chip were electrically and mechanically bonded. Evaluation similar to Example 1 was performed about the obtained conductive bump. The evaluation results are shown in Table 1.
- Comparative Example 1 A conductive paste prepared by adding glycerol as an organic solvent having reducibility to a copper fine particle having an average primary particle diameter of 120 nm similar to that used in Example 2 and adjusting the copper fine particle concentration to 50% by mass is used In the same manner as described in Example 1 except that the heat treatment temperature was set to 300 ° C., a conductive bump was produced in which the conductive substrate and the terminal of the Si chip were electrically and mechanically joined. . Evaluation similar to Example 1 was performed about the obtained conductive bump. The evaluation results are shown in Table 1.
- Comparative Example 2 Copper fine particles having an average primary particle size of 120 nm similar to those used in Example 2 and copper fine particles having an average primary particle size of 10 ⁇ m prepared by electroless reduction from copper ions in an aqueous solution of 75:25 (mass Conductive paste prepared by adding glycerol as an organic solvent having reducibility and adjusting the concentration of copper fine particles to 50% by mass, and using a heat treatment temperature of 300 ° C., In the same manner as described in Example 1, a conductive bump was produced in which the conductive substrate and the terminal of the Si chip were electrically and mechanically bonded. Evaluation similar to Example 1 was performed about the obtained conductive bump. The evaluation results are shown in Table 1.
- Comparative Example 3 Copper microparticles similar to those used in Example 2 with an average primary particle size of 120 nm, prepared by electroless reduction from copper ions in aqueous solution, prepared by electroless reduction from copper ions in aqueous solution, A conductive paste prepared by mixing copper fine particles having an average primary particle diameter of 10 ⁇ m at 70:30 (mass ratio) and adding glycerol as an organic solvent having reducibility so that the copper fine particle concentration is 50% by mass. Using the same method as described in Example 1 except that the heat treatment temperature was set to 300.degree. C., a conductive bump in which the conductive substrate and the terminal of the Si chip are electrically and mechanically bonded to each other. Made. Evaluation similar to Example 1 was performed about the obtained conductive bump. The evaluation results are shown in Table 1.
- Comparative Example 4 Copper fine particles having an average primary particle size of 120 nm and copper fine particles having an average primary particle size of 15 ⁇ m, prepared by electroless reduction from copper ions in an aqueous solution as in Example 2, 95: 5 ( The conductive paste is mixed at a mass ratio), glycerol is added as an organic solvent having reducibility, and the copper fine particle concentration is adjusted to 50 mass%, and the heat treatment temperature is set to 300 ° C.
- a conductive bump was produced in which the conductive substrate and the terminal of the Si chip were electrically and mechanically bonded. Evaluation similar to Example 1 was performed about the obtained conductive bump. The evaluation results are shown in Table 1.
- Comparative Example 5 Copper microparticles having an average primary particle size of 120 nm and copper microparticles having an average primary particle size of 6 ⁇ m prepared by electroless reduction from copper ions in an aqueous solution in the same manner as used in Example 2 95: 5 ( Using a conductive paste prepared by mixing in a mass ratio) and preparing glycerol as the organic solvent having reducibility so that the copper fine particle concentration becomes 90% by mass, except that the heat treatment temperature is set to 300 ° C. In the same manner as described in Example 1, a conductive bump was produced in which the conductive substrate and the terminal of the Si chip were electrically and mechanically bonded. Evaluation similar to Example 1 was performed about the obtained conductive bump. The evaluation results are shown in Table 1.
- the evaluation criteria in Table 1 for the above Examples 1 to 3 and Comparative Examples 1 to 5 were as follows.
- (I) Volume Void The volume A of the conductive bump is A if it is 5 to 35%, B if it is more than 35%, and C if it is less than 5%.
- (Ii) Average Bonding Strength Test A force applied when peeling a Si chip from a substrate with a die shear tester using a die shear tester is a Si chip connection sample for bonding strength test in which a substrate and a Si chip are bonded by a conductive bump The bonding strength per unit area [N / mm 2 ] was determined by dividing by the bonding area.
- Example 4 Silver fine particles having an average primary particle size of 60 nm and silver fine particles having an average primary particle size of 5 ⁇ m are mixed in a ratio of 95: 5 (mass ratio) After the addition so as to be%, they were thoroughly stirred to prepare a conductive paste. Apply 150 ⁇ m thick tape (vinyl chloride tape) on conductive substrate (DBC substrate Direct Bonding Copper substrate), apply conductive paste (shape: rectangular 4 mm on side) with metal spatula, and apply pair on it The gold sputtered surface of the gold-sputtered Si chip (shape: a rectangular solid having a side of 3.5 mm) was mounted so as to face the conductive paste surface.
- the conductive substrate, the conductive paste, and the Si chip portion are heat treated at 200 ° C. while pressing the conductive substrate on which the Si chip is mounted in the direction of the conductive paste at a pressure of 2 MPa.
- Example 5 Copper fine particles having an average primary particle size of 120 nm similar to those used in Example 2 and copper fine particles having an average primary particle size of 7 ⁇ m prepared by electroless reduction from copper ions in an aqueous solution 90:10 (mass The mixture was mixed in a ratio, glycerol was added as an organic solvent having reducibility to the mixture so that the concentration of copper fine particles was 80% by mass, and then sufficiently stirred to prepare a conductive paste.
- the conductive substrate and the terminal of the Si chip are electrically and mechanically joined in the same manner as described in Example 4 except that the conductive paste is used and the heat treatment temperature is set to 300 ° C. A conductive die bond part was produced. Evaluation similar to Example 4 was performed about this die-bonding part. The evaluation results are shown in Table 2.
- Example 6 Copper fine particles having an average primary particle size of 120 nm and copper fine particles having an average primary particle size of 7 ⁇ m are mixed in a ratio of 90:10 (mass ratio) as used in Example 5 with glycerol 80 as an organic solvent. A mixed solvent consisting of% by volume and 20% by volume of N-methylacetamide was added to a copper fine particle concentration of 75% by mass and then sufficiently stirred to prepare a conductive paste.
- the conductive substrate and the terminal of the Si chip are electrically and mechanically joined in the same manner as described in Example 1 except that the conductive paste is used and the heat treatment temperature is set to 300 ° C. A conductive die bond part was produced. Evaluation similar to Example 4 was performed about this electroconductive die-bonding part. The evaluation results are shown in Table 2.
- Comparative Example 6 After adding glycerol as an organic solvent having reducibility to a copper fine particle having an average primary particle diameter of 120 nm similar to that used in Example 5 so that the copper fine particle concentration is 50 mass%, the conductive paste is sufficiently stirred Was prepared.
- the conductive substrate and the terminal of the Si chip are electrically and mechanically joined in the same manner as described in Example 1 except that the conductive paste is used and the heat treatment temperature is set to 300 ° C. A conductive die bond part was produced. Evaluation similar to Example 4 was performed about this electroconductive die-bonding part. The evaluation results are shown in Table 2.
- Comparative Example 7 Copper fine particles having an average primary particle size of 120 nm similar to those used in Example 5 and copper fine particles having an average primary particle size of 10 ⁇ m prepared by electroless reduction from copper ions in an aqueous solution of 75:25 (mass The mixture was mixed in a ratio, glycerol was added as an organic solvent having reducibility to the mixture so that the copper fine particle concentration became 50% by mass, and then sufficiently stirred to prepare a conductive paste.
- the conductive substrate and the terminal of the Si chip are electrically and mechanically joined in the same manner as described in Example 1 except that the conductive paste is used and the heat treatment temperature is set to 300 ° C. A conductive die bond part was produced. Evaluation similar to Example 4 was performed about this electroconductive die-bonding part. The evaluation results are shown in Table 2.
- Comparative Example 8 Copper fine particles having an average primary particle diameter of 120 nm similar to that used in Example 5 and copper fine particles having an average primary particle diameter of 10 ⁇ m prepared by electroless reduction from copper ions in an aqueous solution at 70:30 (mass The mixture was mixed in a ratio, glycerol was added as an organic solvent having reducibility to the mixture so that the copper fine particle concentration became 50% by mass, and then sufficiently stirred to prepare a conductive paste.
- the conductive substrate and the terminal of the Si chip are electrically and mechanically joined in the same manner as described in Example 1 except that the conductive paste is used and the heat treatment temperature is set to 300 ° C. A conductive die bond part was produced. Evaluation similar to Example 4 was performed about this electroconductive die-bonding part. The evaluation results are shown in Table 2.
- Comparative Example 9 Copper fine particles having an average primary particle size of 120 nm similar to those used in Example 5 and copper fine particles having an average primary particle size of 15 ⁇ m prepared by electroless reduction from copper ions in an aqueous solution of 95: 5 (mass The mixture was mixed in a ratio, glycerol was added as an organic solvent having reducibility to the mixture so that the copper fine particle concentration became 50% by mass, and then sufficiently stirred to prepare a conductive paste.
- the conductive substrate and the terminal of the Si chip are electrically and mechanically joined in the same manner as described in Example 1 except that the conductive paste is used and the heat treatment temperature is set to 300 ° C.
- a conductive die bond part was produced. The bonding strength test of the conductive die bonding portion was performed. Evaluation similar to Example 4 was performed about this electroconductive die-bonding part. The evaluation results are shown in Table 2.
- Comparative Example 10 Copper fine particles having an average primary particle diameter of 250 nm similar to that used in Example 5 and copper fine particles having an average primary particle diameter of 6 ⁇ m prepared by electroless reduction from copper ions in an aqueous solution of 95: 5 (mass The mixture was mixed in a ratio, glycerol was added as an organic solvent having reducibility to the mixture so that the copper fine particle concentration became 50% by mass, and then sufficiently stirred to prepare a conductive paste.
- the conductive substrate and the terminal of the Si chip are electrically and mechanically joined in the same manner as described in Example 1 except that the conductive paste is used and the heat treatment temperature is set to 300 ° C. A conductive die bond part was produced. Evaluation similar to Example 4 was performed about this electroconductive die-bonding part. The evaluation results are shown in Table 2.
- the evaluation criteria in Table 2 were as follows.
- (I) Volume porosity The porosity of the conductive bump was determined by taking an electron micrograph at an observation magnification of 1000 to 10000 times using a scanning electron microscope (SEM) and analyzing its cross-sectional image.
- the volume porosity of the conductive die bonding portion is 3 to 25%, A is more than 25%, 35% or less is B, more than 35% is C, and less than 3% is D.
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Abstract
Description
フリップチップボンディングは半導体素子等上に形成されたバンプ(突起状物)を、回路基板等へ接合するものであるが、そのバンプの形成にはメッキ法が主に採用されている。
メッキ法によるバンプの形成では、微細なパターンの形成が可能であり、条件設定によりバンプ高さ制御が試みられてはいるものの、バンプの高さに多少のバラつきが生じるのを避けられないという問題点がある。電極の接触不良を防止するために、このようなバンプ高さのバラつきに対する対策としては、接合時の加圧手段により全てのバンプを密着させる方法を採用することも可能であるが、過度に加圧するとバンプ内部に歪が残存したり、耐熱応力が低下したりして破損につながるおそれがある。従って、金属製の微細パターン接続用バンプの構造を加圧時に変形し易い柔らかさを有する構造にすることが好ましい。
特許文献2には、バンプに使用する材料を多孔質で比較的柔らかく弾力性を有する焼結体からなるバンプが提案されている。バンプが弾力性を有することによりバンプ高さにバラつきがあっても、加圧により多孔質体に収縮が生じて接合が可能となる。また、内部に歪が残存することも少なく、耐熱応力の低下も少ない。
特許文献3には、第一の金属層と、第二の金属層との間に第三の金属からなる多孔質金属層を介在させて、第一の金属層と該多孔質金属層、及び第二の金属層と該多孔質金属層との間に、平均直径が100nm以下の金属超微粒子を有機系溶媒中に分散させた金属ナノペーストを設置して、加熱により接合する接合方法が開示されている。
特許文献4には、基板上に設けたフォトレジスト層の細孔内に金メッキ層(第1バンプ層、高さ:10μm)を設け、その上に金属ペーストとして金ペーストを滴下して充填した後焼結して焼結体(第2バンプ層)を設けたバンプが開示されている。
特許文献5には、昇華性物質を有機溶媒に完全に溶解し、その溶解液を細孔から水中に噴出させて昇華性物質の微粒子を析出させ、得られる微粒子をフェライト粉体に添加して混合し、成形後に焼成するフェライト多孔体の製造方法が開示されている。
金属材料中のクラック(亀裂)の伝播の理論によれば、クラックを空孔ととらえ、空孔サイズが十分に小さいとき大きい応力が働いても空孔(クラック)が拡大しないことが知られている(日本材料学会編、疲労設計便覧、1995年1月20日、養賢堂発行、148~195頁参照)。この場合、例えばナノサイズの空孔を持つバンプは、ミクロンサイズの空孔を持つバンプよりおよそ100倍程度の耐応力性があると推測される。
上記特許文献2に開示の焼結体からなるバンプを適用する場合には、上記のような問題はないが、バンプに弾性を持たせたために、実装の際に横方向の変形のおそれがあり、バンプ間隔(ピッチ)を損ねることがある。
上記特許文献3、及び特許文献4に開示のナノサイズからなる金属微粒子を焼結する際には、焼結温度近辺まで固体粉末が残存し分散媒から発生するガスの取り込みによる粗大ボイドの形成、膨れやクラックを形成し易いという問題点がある。
半導体素子とインターポーザとの接続構造部であるダイボンド部における接着性が低いと機械的ストレス(外部応力、内部応力)や物理応力(熱ストレス)によって、半導体素子の裏面またはインターポーザ接続端子と導電性ダイボンド部との接着界面が、部分剥離したり完全剥離したりすることがある。
優れた熱サイクル特性を有する導電性バンプ、導電性ダイボンド部等の導電接続部材は、ナノサイズの金属微粒子を含有する導電性ペーストを焼成して、該微粒子の表面が結合すると共にナノサイズの空孔が形成されている多孔質体とすることが好ましいが、導電性ペーストにおいて、金属微粒子が偏在していたり、加熱処理する際に有機分散剤が蒸発又は熱分解して生じた気泡が成長して、多孔質体内部に粗大ボイドやクラックを形成すると、機械的強度や熱サイクル特性が著しく低下する。
即ち、本発明は、以下の(1)~(17)に記載する発明を要旨とする。
(1)金属、及び合金から選択された1種又は2種以上からなる、平均一次粒子径が1~150nmの金属微粒子(P1)と、金属微粒子(P1)と同種金属で平均一次粒子径が1~10μmの金属微粒子(P2)からなり、その配合割合(P1/P2)が80~95質量%/20~5質量%(質量%の合計は100質量%)である金属微粒子(P)と、
有機溶媒(S)、又は有機溶媒(S)と有機バインダー(B)からなる有機分散媒(D)とを含み、金属微粒子(P)と有機分散媒(D)との配合割合(P/D)が50~85質量%/50~15質量%(質量%の合計は100質量%)である、ことを特徴とする導電性ペースト(以下、第1の態様ということがある)。
(2)前記金属微粒子(P)が、銅、金、銀、ニッケル、及びコバルトの中から選択される1種又は2種以上である、ことを特徴とする前記(1)に記載の導電性ペースト。
(3)前記有機分散媒(D)における有機溶媒(S)と有機バインダー(B)の配合割合(S/B)が80~100質量%/20~0質量%(質量%の合計は100質量%)である、ことを特徴とする前記(1)又は(2)に記載の導電性ペースト。
(4)前記有機分散媒(D)が水を含有しており、該水の含有量が有機溶媒(S)と水(W)との割合(S/W)で75~99.9質量%/25~0.1質量%(質量%の合計は100質量%)である、ことを特徴とする前記(1)から(3)のいずれかに記載の導電性ペースト。
(6)前記有機溶媒(S1)が、エチレングリコール、ジエチレングリコール、1,2-プロパンジオール、1,3-プロパンジオール、1,2-ブタンジオール、1,3-ブタンジオール、1,4-ブタンジオール、2-ブテン-1,4-ジオール、2,3-ブタンジオール、ペンタンジオール、ヘキサンジオール、オクタンジオール、グリセロール、1,1,1-トリスヒドロキシメチルエタン、2-エチル-2-ヒドロキシメチル-1,3-プロパンジオール、1,2,6-ヘキサントリオール、1,2,3-ヘキサントリオール、1,2,4-ブタントリオール、トレイトール、エリトリトール、ペンタエリスリトール、ペンチトール、ヘキシトール及びイミノジエタノールの中から選択される1種又は2種以上である、ことを特徴とする前記(5)に記載の導電性ペースト。
(7)前記有機溶媒(SA)が、N-メチルアセトアミド、N-メチルホルムアミド、N-メチルプロパンアミド、ホルムアミド、N,N-ジメチルアセトアミド、1,3-ジメチル-2-イミダゾリジノン、N,N-ジメチルホルムアミド、1-メチル-2-ピロリドン、ヘキサメチルホスホリックトリアミド、2-ピロリジノン、ε-カプロラクタム、及びアセトアミドの中から選択される1種又は2種以上である、ことを特徴とする、前記(5)に記載の導電性ペースト。
(8)前記有機バインダー(B)がセルロース樹脂系バインダー、アセテート樹脂系バインダー、アクリル樹脂系バインダー、ウレタン樹脂系バインダー、ポリビニルピロリドン樹脂系バインダー、ポリアミド樹脂系バインダー、ブチラール樹脂系バインダー、及びテルペン系バインダーの中から選択される1種又は2種以上である、ことを特徴とする前記(1)から(7)のいずれかに記載の導電性ペースト。
(10)前記導電性ペーストを加熱処理して金属多孔質体を形成する際に、有機溶媒(S)と有機バインダー(B)が蒸発又は熱分解する、ことを特徴とする前記(1)から(9)のいずれかに記載の導電性ペースト。
該金属多孔質体が平均粒子径1~10μmの金属微粒子(P2)に由来する粒子間に、平均粒子径1~150nmの金属微粒子(P1)に由来する粒子がその表面で部分的に結合した状態で存在していて、これらの金属微粒子間に空孔が分散している、ことを特徴とする導電接続部材(以下、第2の態様ということがある)。
(12)前記導電接続部材が半導体素子間を接合するための導電性バンプであることを特徴とする前記(11)に記載の導電接続部材。
(13)前記導電接続部材が半導体素子と導電性基板間を接合するための導電性ダイボンド部である、ことを特徴とする前記(11)に記載の導電接続部材。
(14)前記加熱処理が両電極端子間、又は電極端子と基板間を0.5~15MPaで加圧した状態で行われる、ことを特徴とする前記(11)から(13)に記載の導電接続部材。
(15)前記導電性ペーストの加熱処理温度が150~350℃である、ことを特徴とする前記(11)から(14)に記載の金属多孔質体からなる導電接続部材。
(16)前記導電性ペーストの加熱処理温度が250~300℃である、ことを特徴とする前記(11)から(14)に記載の金属多孔質体からなる導電接続部材。
(17)前記金属多孔質体の空隙率が5~35%である、ことを特徴とする前記(11)から(16)に記載の金属多孔質体からなる導電接続部材。
(ii)上記(11)に記載した第2の態様の導電接続部材は、金属微粒子(P)と空孔が偏在しないで分散しており、粗大ボイドやクラックが存在しないので熱サイクル特性が向上して耐クラック性、及び接合強度に優れている。
〔1〕第1の態様である「導電性ペースト」について
第1の態様である「導電性ペースト」は、金属、及び合金から選択された1種又は2種以上からなる、平均一次粒子径が1~150nmの金属微粒子(P1)と、金属微粒子(P1)と同種金属で平均一次粒子径が1~10μmの金属微粒子(P2)からなり、その配合割合(P1/P2)が80~95質量%/20~5質量%(質量%の合計は100質量%)である金属微粒子(P)と、
有機溶媒(S)、又は有機溶媒(S)と有機バインダー(B)からなる有機分散媒(D)とを含み、金属微粒子(P)と有機分散媒(D)との配合割合(P/D)が50~85質量%/50~15質量%(質量%の合計は100質量%)であることを特徴とする。
金属微粒子(P)は、平均一次粒子径が1~150nmの金属微粒子(P1)と、金属微粒子(P1)と同種金属で平均一次粒子径が1~10μmの金属微粒子(P2)からなり、その配合割合(P1/P2)が80~95質量%/20~5質量%(質量%の合計は100質量%)である。金属微粒子(P)を構成する金属微粒子(P1)と金属微粒子(P2)とは同種の金属であり、金属微粒子(P)としては導電性ペーストに含有されていて、加熱処理後導電接続部材としての機能を発揮するものであれば使用可能であるが、導電性、加熱処理(焼結性)、市場における入手の容易性等から、銅、金、銀、ニッケル、及びコバルトの中から選択される1種又は2種以上であることが好ましい。
金属微粒子(P1)の平均一次粒子径は、1~150nmである。該平均一次粒子径が1nm未満では、焼成により均質な粒子径と空孔を有する多孔質体を形成することが困難になるおそれがある。一方、導電性ペーストを加熱処理する際に金属微粒子(P1)は平均一次粒子径が1~10μmである金属微粒子(P2)間に存在するので、金属微粒子(P1)の平均一次粒子径が150nmを超えると、金属微粒子(P2)間に安定的に存在しづらくなり、本発明の効果を充分に発揮できなくなるおそれがある。
尚、本発明において、一次粒子の平均粒径とは、二次粒子を構成する個々の金属微粒子の一次粒子の直径の意味である。該一次粒子径は、透過型電子顕微鏡(TEM)観察に基づいて測定することができる。また、平均粒径とは、一次粒子の数平均粒径を意味する。
有機分散媒(D)は、有機溶媒(S)、又は有機溶媒(S)と有機バインダー(B)とからなる。有機分散媒(D)は、導電性ペースト中で金属微粒子(P1)と金属微粒子(P2)とを分散させ、導電性ペーストの粘度の調節、及びバンプ前躯体、ダイボンド部前躯体等の導電接続部材前躯体の形状を維持し、かつ加熱処理の際に液状及びガス状で還元剤としての機能を発揮する。前記有機分散媒(D)における有機溶媒(S)と有機バインダー(B)の配合割合(S/B)が80~100質量%/20~0質量%(質量%の合計は100質量%)であることが好ましい。有機分散媒(D)中の有機バインダー(B)の配合割合が20質量%を超えると、バンプ前躯体を加熱処理する際に有機バインダー(B)が熱分解して飛散する速度が遅くなり、また導電性バンプ中に残留カーボン量が増えると焼結が阻害されて、クラック、剥離等の問題が生ずる可能性があり好ましくない。有機溶媒(S)の選択により、該溶剤のみで金属微粒子(P1)と金属微粒子(P2)とを分散させ、導電性ペーストの粘度を調節し、導電性バンプ前躯体、導電性ダイボンド部前躯体等の導電接続部材前駆体の形状を維持できる機能を発揮できる場合には、有機分散媒(D)として有機溶媒(S)のみからなる成分を使用できる。
前記有機溶媒(S)は、(i)常圧における沸点が100℃以上で、かつ分子中に1又は2以上のヒドロキシル基を有するアルコール及び/又は多価アルコールからなる還元性を有する有機溶媒(S1)、又は(ii)少なくとも、常圧における沸点が100℃以上で、かつ分子中に1又は2以上のヒドロキシル基を有するアルコール及び/又は多価アルコールからなる還元性を有する有機溶媒(S1)5~95体積%、並びにアミド基を有する有機溶媒(SA)95~5体積%からなる有機溶媒(S2)が好ましい。
有機分散媒(D)中に還元性を有する有機溶媒(S1)が含有されていると、導電性ペーストを加熱処理する際に、先ず金属微粒子表面が還元され、その後に該微粒子の表面間で焼結に基づく結合が進行すると考えられるので、有機溶媒(S1)が連続的に蒸発して、液体および蒸気が存在する雰囲気で還元・焼成すると、焼結が促進されて良好な導電性を有する導電接続部材が形成される。従って、有機分散媒(D)中に有機溶媒(S1)が存在すると、加熱処理の際に非酸化性雰囲気が形成されて、金属微粒子(P)表面における還元、結合が促進される。
かかる観点から、有機溶媒(S2)は有機溶媒(S1)60~95体積%、及びアミド基を有する有機溶媒(SA)40~5体積%からなることがより好ましい。
有機溶媒(SA)の具体例として、N-メチルアセトアミド、N-メチルホルムアミド、N-メチルプロパンアミド、ホルムアミド、N,N-ジメチルアセトアミド、1,3-ジメチル-2-イミダゾリジノン、N,N-ジメチルホルムアミド、1-メチル-2-ピロリドン、ヘキサメチルホスホリックトリアミド、2-ピロリジノン、ε-カプロラクタム、及びアセトアミド等が挙げられる。
有機バインダー(B)は、導電性ペースト中で金属微粒子(P)の凝集の抑制、導電性ペーストの粘度の調節、及び導電性バンプ前躯体、導電性ダイボンド部前躯体等の導電接続部材前駆体の形状を維持する機能を発揮する。このような機能を有する有機バインダー(B)としては、セルロース樹脂系バインダー、アセテート樹脂系バインダー、アクリル樹脂系バインダー、ウレタン樹脂系バインダー、ポリビニルピロリドン樹脂系バインダー、ポリアミド樹脂系バインダー、ブチラール樹脂系バインダー、及びテルペン系バインダーの中から選択される1種又は2種以上が好ましい。
有機バインダー(R)の具体例として、前記セルロース樹脂系バインダーがアセチルセルロース、メチルセルロース、エチルセルロース、ブチルセルロース、及びニトロセルロース;アセテート樹脂系バインダーがメチルグリコールアセテート、エチルグリコールアセテート、ブチルグリコールアセテート、エチルジグリコールアセテート、及びブチルジグリコールアセテート;アクリル樹脂系バインダーがメチルメタクリレート、エチルメタクリレート、及びブチルメタクリレート;ウレタン樹脂系バインダーが2,4-トリレンジイソシアネート、及びp-フェニレンジイソシアネート;ポリビニルピロリドン樹脂系バインダーがポリビニルピロリドン、及びN-ビニルピロリドン;ポリアミド樹脂系バインダーがポリアミド6、ポリアミド66、及びポリアミド11;ブチラール樹脂系バインダーがポリビニルブチラール;テルペン系バインダーがピネン、シネオール、リモネン、及びテルピネオール等が挙げられる。
導電性ペーストは、金属微粒子(P)と有機分散媒(D)を含み、金属微粒子(P)が有機分散媒(D)中に均一に分散されたペースト状のものであり、金属微粒子(P)が50~85質量%と、有機分散媒(D)が50~15質量%(質量%の合計は100質量%)の割合で含有されている。金属微粒子(P)の割合が前記85質量%を超えるとペーストが高粘度となり、加熱処理において金属微粒子(P)表面間の結合不足が生じて導電性が低下するおそれがある。一方、金属微粒子(P)の割合が前記50質量%未満では、ペーストの粘度が低下して半導体素子の電極端子又は回路基板の電極端子の接合面に塗布された導電接続部材前駆体の形状維持が困難となるおそれがあり、また、加熱処理の際に金属多孔質体が収縮するという不具合が生ずるおそれがある。かかる観点から前記金属微粒子(P)と有機分散媒(D)との割合(P/D)は55~80質量%/45~20質量%(質量%の合計は100質量%)が好ましい。
本発明においては、導電性ペーストを加熱処理すると、ある温度に達すると有機溶媒(S)の蒸発、又は有機溶媒(S)の蒸発と有機バインダー(B)の熱分解が進行して、金属微粒子(P)の表面同士が接触した後に、互いに結合(焼結)する原理を利用するものである。本発明の導電性ペーストには、本発明の効果を損なわない範囲において、前記した成分に必要に応じて消泡剤、分散剤、可塑剤、界面活性剤、増粘剤等、また他の金属粒子等を加えることができる。
導電性ペーストを製造するに際し、前記金属微粒子(P)に有機分散媒(D)を添加してせん断応力を付加することにより、混練し、導電性ペーストを調製することができる。
せん断応力を付加する方法としては、例えば、ニーダー、三本ロール等の混練装置、密閉系で混練可能なライカイ器等を用いることができる。混練の際、銅粉の酸化が過度に進行しないようにすることが好ましい。
第2の態様の「導電接続部材」は、前記第1の態様に記載された導電性ペーストを電子部品における半導体素子もしくは回路基板の電極端子又は導電性基板の接合面に載せた後、該導電性ペースト上に更に接続する他方の電極端子又は導電性基板の接合面を配置して加熱処理により焼結して形成された金属多孔質体からなる導電接続部材であって、
該金属多孔質体が平均粒子径1~10μmの金属微粒子(P2)に由来する粒子間に、平均粒子径1~150nmの金属微粒子(P1)に由来する粒子がその表面で部分的に結合した状態で存在していて、これらの金属微粒子間に空孔が分散していることを特徴とする。
導電接続部材としては半導体素子間を接合するための導電性バンプ、半導体素子と導電性基板間を接合するための導電性ダイボンド部等が挙げられるがこれらに限定されない。
導電性バンプは、導電性ペーストを電子部品における半導体素子もしくは回路基板の電極端子の接合面に載せ(塗布、印刷等も含まれる)、該導電性ペースト上に更に接続する他方の電極端子の接合面を配置した後、加熱処理、又は加圧下に加熱処理により焼結して形成される。前記接続する他方の電極端子にはワイヤボンディングを行う場合の金ワイヤ等のワイヤも含まれる。尚、前記導電性ペースト上に更に接続する他方の電極端子の接合面を配置する際に位置合わせを行うことが望ましい。
導電性ダイボンド部は、通常、導電性ペーストを電子部品における回路基板の接合面に載せ(塗布、印刷等も含まれる)、該導電性ペースト上に更に接続する他方の電極端子の接合面を配置した後、加熱処理、又は加圧下に加熱処理により焼結して形成される。
前記加圧下の加熱処理は、両電極端子間、又は電極端子と基板間の加圧により導電接続部材前躯体と両電極端子接合面、又は電極端子と導電性基板間との接合を確実にするか、または導電接続部材前躯体に適切な変形を生じさせて電極端子接合面との確実な接合を行うことができるとともに、導電接続部材前躯体と電極端子接合面との接合面積が大きくなり、接合信頼性を一層向上することができる。また、半導体素子と導電接続部材前躯体間を加圧型ヒートツ-ル等を用いて加圧下で焼成すると、接合部での焼結性が向上してより良好な接合部が得られる。
前記両電極端子間、又は電極端子と基板間の加圧は、0.5~15MPaが好ましい。該加圧が0.5MPa以上の加圧で接合面の大きなボイド形成の抑制効果が向上し、一方、15MPaを超えると導電性金属微粒子(P1)間の空隙が減少して、空隙率が低下するおそれがある。
上記金属微粒子(P1)、金属微粒子(P2)、有機溶媒(S)、及び有機バインダー(B)の成分については、第1の態様に記載した通りである。又、有機分散媒(D)が有機溶媒(S)80~100質量%と、有機バインダー(B)20~0質量%からなることが好ましいことも第1の態様に記載した通りである。
導電性ペーストを充填するための開口部形成方法としては、露光・現像工程を経て感光性樹脂層にパターンを形成するフォトリソグラフィー方法、レーザー光、電子線、イオンビーム等の高エネルギー線を素子上に設けた絶縁樹脂層に照射して、加熱による溶融もしくは樹脂の分子結合を切断するアブレーションにより該樹脂層に開口部を形成する方法がある。これらの中で、実用性の点からフォトリソグラフィー法、又はレーザー光を用いたアブレーションによる開口部形成方法が好ましい。加熱処理(焼結)後に、半導体素子上の電極端子と、回路基板の電極端子とが電気的接続を確保できるように接触させるための位置合わせは、例えば、半導体素子上の電極端子と、テープリール等で搬送されてきた導電性基板の接続電極端子部とを光学装置等を用いて行うことができる。
前記加熱処理に要する時間は、使用する金属微粒子(P1)の種類、有機分散媒(D)の種類にもよるが、5~30分間程度が望ましい。金属微粒子(P1)として平均一次粒子径が1~150nmの微粒子を使用するので、加熱により有機分散媒(D)が除去されれば、その表面のエネルギーによってバルク状態の金属の融点より低温で金属微粒子表面間での結合(焼結)が進み、金属多孔質体からなる導電性バンプ、導電性ダイボンド部等の導電接続部材が形成される。
第2の態様の導電接続部材は、前述の通り、第1の態様に記載の導電性ペーストを電子部品における半導体素子もしくは回路基板の電極端子又は導電性基板の接合面に載せた後、該導電性ペースト上に更に接続する他方の電極端子又は導電性基板の接合面を配置して加熱処理により焼結して形成された金属多孔質体からなる導電接続部材であって、
該金属多孔質体が平均粒子径1~10μmの金属微粒子(P2)に由来する粒子間に、平均粒子径1~150nmの金属微粒子(P1)に由来する粒子がその表面で部分的に結合した状態で存在していて、これらの金属微粒子間に空孔が分散していることを特徴とする。
上記加熱処理により得られる導電接続部材は、めっき法で得られる導電性バンプ等と対比すると金属微粒子(P1)に変形や応力が緩和された状態で金属微粒子(P1)同士が表面で接触して、結合(焼結)されることで、適度な弾力性と柔らかさを有し、かつ、良好な導電性が得られる。
このようにして得られる金属多孔質体からなる導電性バンプ、導電性ダイボンド部等の導電接続部材は、空隙率が5~35体積%であり、かつ空孔が偏在していないので機械的及び電気的接合性に優れ、熱サイクル特性が向上して耐クラック性に優れている。尚、導電性バンプ形状物または導電性ダイボンド部の空隙率は、走査型電子顕微鏡(SEM)を用いて、観察倍率1000~10000倍の電子顕微鏡写真を撮り、その断面像を解析することにより求めることができる。
尚、導電性バンプと導電性ダイボンド部の評価方法等については後述する。
平均一次粒子径が60nmの銀微粒子と、平均一次粒子径が5μmの銀微粒子を95:5(質量比)で混合し、該混合物に還元性を有する有機溶媒としてエチレングリコールを銀微粒子濃度60質量%になるように添加後十分に撹拌して導電性ペーストを調製した。
該導電性ペーストを、導電性基板(DBC基板 Direct Bonding Copper 基板)にスクリーン印刷により、導電性バンプ前駆体(サイズ:50μmφ、厚み:150μm)を4箇所(1辺が4mmの正方形の頂点に対応する位置)塗布した。該前駆体上に対になるようにスタッド(50μmφ、厚み:150μm)に金スパッタされたSiチップ(形状:1辺が4.5mmの直方体)の金スパッタ面が該前駆体面と相対するように載せた。Siチップが搭載された導電性基板を200℃で加熱処理して、導電性ペースト中に含有されている銀微粒子を焼結させて、導電性基板とSiチップの端子とが電気的、機械的に接合している導電性バンプを作製した。得られた導電性バンプについて後述する接合強度試験(測定の平均値(N=10))等の評価を行った。その評価結果を表1に示す。
水溶液中で銅イオンからの無電解還元により調製された、平均一次粒子径が120nmの銅微粒子と、同様の無電解還元により調製された平均一次粒子径が7μmの銅微粒子を90:10(質量比)で混合し、該混合物に還元性を有する有機溶媒としてグリセロールを銅微粒子濃度が80質量%になるように添加して、実施例1と同様にして導電性ペーストを調製した。
得られた導電性ペーストを使用し、加熱処理温度を300℃とした以外は、実施例1に記載したと同様にして、導電性基板とSiチップの端子とが電気的、機械的に接合している導電性バンプを作製した。得られた導電性バンプについて実施例1と同様の評価を行った。その評価結果を表1に示す。また、実施例2で得られた導電性バンプ断面の電子顕微鏡写真を図1に示す。図1から、平均一次粒子径が7μmの銅微粒子に由来する焼結粒子が導電性バンプ中に分散して存在し、該焼結粒子の周囲に、平均一次粒子径が120nmの銅微粒子に由来する焼結粒子が存在していて、粗大ボイドやクラックが存在していないことが観察される。
実施例2で使用したと同様の平均一次粒子径が120nmの銅微粒子と、平均一次粒子径が7μmの銅微粒子を90:10(質量比)で混合し、有機溶媒としてグリセロール80体積%とN-メチルアセトアミド20体積%からなる混合溶剤を添加し、銅微粒子濃度が75質量%になるように調節した導電性ペーストを使用し、加熱処理温度を300℃とした以外は、実施例1に記載したと同様にして、導電性基板とSiチップの端子とが電気的、機械的に接合している導電性バンプを作製した。得られた導電性バンプについて実施例1と同様の評価を行った。その評価結果を表1に示す。
実施例2で使用したと同様の平均一次粒子径が120nmの銅微粒子に、還元性を有する有機溶媒としてグリセロールを添加し、銅微粒子濃度が50質量%になるように調節した導電性ペーストを使用し、加熱処理温度を300℃とした以外は、実施例1に記載したと同様にして、導電性基板とSiチップの端子とが電気的、機械的に接合している導電性バンプを作製した。得られた導電性バンプについて実施例1と同様の評価を行った。その評価結果を表1に示す。
[比較例2]
実施例2で使用したと同様の平均一次粒子径が120nmの銅微粒子と、水溶液中で銅イオンからの無電解還元により調製された、平均一次粒子径が10μmの銅微粒子を75:25(質量比)で混合し、還元性を有する有機溶媒としてグリセロールを添加して、銅微粒子濃度が50質量%になるように調節した導電性ペーストを使用し、加熱処理温度を300℃とした以外は、実施例1に記載したと同様にして、導電性基板とSiチップの端子とが電気的、機械的に接合している導電性バンプを作製した。得られた導電性バンプについて実施例1と同様の評価を行った。その評価結果を表1に示す。
実施例2で使用したと同様の平均一次粒子径が120nmの銅微粒子と、水溶液中で銅イオンからの無電解還元により調製された、水溶液中で銅イオンからの無電解還元により調製された、平均一次粒子径が10μmの銅微粒子を70:30(質量比)で混合し、還元性を有する有機溶媒としてグリセロールを添加して、銅微粒子濃度が50質量%になるように調節した導電性ペーストを使用し、加熱処理温度を300℃とした以外は、実施例1に記載したと同様にして、導電性基板とSiチップの端子とが電気的、機械的に接合している導電性バンプを作製した。得られた導電性バンプについて実施例1と同様の評価を行った。その評価結果を表1に示す。
実施例2で使用したと同様の、平均一次粒子径が120nmの銅微粒子と、水溶液中で銅イオンからの無電解還元により調製された、平均一次粒子径が15μmの銅微粒子を95:5(質量比)で混合し、還元性を有する有機溶媒としてグリセロールを添加して、銅微粒子濃度が50質量%になるように調節した導電性ペーストを使用し、加熱処理温度を300℃とした以外は、実施例1に記載したと同様にして、導電性基板とSiチップの端子とが電気的、機械的に接合している導電性バンプを作製した。得られた導電性バンプについて実施例1と同様の評価を行った。その評価結果を表1に示す。
実施例2で使用したと同様の、平均一次粒子径が120nmの銅微粒子と、水溶液中で銅イオンからの無電解還元により調製された、平均一次粒子径が6μmの銅微粒子を95:5(質量比)で混合し、該混合物に還元性を有する有機溶媒としてグリセロールを銅微粒子濃度が90質量%になるように調製した導電性ペーストを使用し、加熱処理温度を300℃とした以外は、実施例1に記載したと同様にして、導電性基板とSiチップの端子とが電気的、機械的に接合している導電性バンプを作製した。得られた導電性バンプについて実施例1と同様の評価を行った。その評価結果を表1に示す。
(i)体積空隙率
導電性バンプの体積空隙率が5~35%の場合はA、35%超の場合はB、5%未満の場合はCとした。
(ii)平均接合強度試験
基板とSiチップが導電性バンプにより接合された接合強度試験用のSiチップ接続サンプルをダイシェア試験機で基板からSiチップを剥離させる際にかかった力を導電性バンプの接合面積で除して、単位面積当りの接合強度[N/mm2]を求めた。
(iii)粗大ボイドの有無
導電性バンプに10μm以上の粗大ボイドが観察されない場合はA、観察された場合はBとした。
(iv)クラックの有無
導電性バンプ、及びその接合面にクラックが観察されない場合はA、観察された場合はBとした。
平均一次粒子径が60nmの銀微粒子と、平均一次粒子径が5μmの銀微粒子を95:5(質量比)で混合し、該混合物に還元性を有する有機溶媒としてエチレングリコールを銀微粒子濃度60質量%になるように添加後十分に撹拌して導電性ペーストを調製した。
導電性基板(DBC基板 Direct Bonding Copper 基板)上に150ミクロン厚のテープ(塩化ビニールテープを貼り、金属ヘラにより導電性ペースト(形状:1辺が4mmの直方体)を塗布し、その上に対になるように金スパッタされたSiチップ(形状:1辺が3.5mmの直方体)の金スパッタ面が導電性ペースト面と相対するように載せた。
次に、Siチップが搭載された導電性基板を導電性ペースト方向に2MPaの圧力で加圧しながら、導電性基板、導電性ペースト、及びSiチップ部分を200℃で加熱処理して、導電性ペースト中に含有されている金属微粒子を焼結させて、該導電性基板とSiチップが導電性ダイボンド部により電気的、機械的に接合された接合強度試験用のSiチップ接続サンプルを作製した。該導電性ダイボンド部について後述する接合強度試験(測定の平均値(N=10))等の評価を行った。その評価結果を表2に示す。
実施例2で使用したと同様の平均一次粒子径が120nmの銅微粒子と、水溶液中で銅イオンからの無電解還元により調製された、平均一次粒子径が7μmの銅微粒子を90:10(質量比)で混合し、該混合物に還元性を有する有機溶媒としてグリセロールを銅微粒子濃度が80質量%になるように添加後十分に撹拌して導電性ペーストを調製した。
該導電性ペーストを使用し、加熱処理温度を300℃とした以外は、実施例4に記載したと同様にして、導電性基板とSiチップの端子とが電気的、機械的に接合している導電性ダイボンド部を作製した。該ダイボンド部について実施例4と同様の評価を行った。その評価結果を表2に示す。
実施例5で使用したと同様の、平均一次粒子径が120nmの銅微粒子と、平均一次粒子径が7μmの銅微粒子を90:10(質量比)で混合し、該混合物に有機溶媒としてグリセロール80体積%とN-メチルアセトアミド20体積%からなる混合溶剤を銅微粒子濃度が75質量%になるように添加後十分に撹拌して導電性ペーストを調製した。
該導電性ペーストを使用し、加熱処理温度を300℃とした以外は、実施例1に記載したと同様にして、導電性基板とSiチップの端子とが電気的、機械的に接合している導電性ダイボンド部を作製した。該導電性ダイボンド部について実施例4と同様の評価を行った。その評価結果を表2に示す。
実施例5で使用したと同様の平均一次粒子径が120nmの銅微粒子に、還元性を有する有機溶媒としてグリセロールを銅微粒子濃度が50質量%になるように添加後十分に撹拌して導電性ペーストを調製した。
該導電性ペーストを使用し、加熱処理温度を300℃とした以外は、実施例1に記載したと同様にして、導電性基板とSiチップの端子とが電気的、機械的に接合している導電性ダイボンド部を作製した。該導電性ダイボンド部について実施例4と同様の評価を行った。その評価結果を表2に示す。
[比較例7]
実施例5で使用したと同様の平均一次粒子径が120nmの銅微粒子と、水溶液中で銅イオンからの無電解還元により調製された、平均一次粒子径が10μmの銅微粒子を75:25(質量比)で混合し、該混合物に還元性を有する有機溶媒としてグリセロールを銅微粒子濃度が50質量%になるように添加後十分に撹拌して導電性ペーストを調製した。
該導電性ペーストを使用し、加熱処理温度を300℃とした以外は、実施例1に記載したと同様にして、導電性基板とSiチップの端子とが電気的、機械的に接合している導電性ダイボンド部を作製した。該導電性ダイボンド部について実施例4と同様の評価を行った。その評価結果を表2に示す。
実施例5で使用したと同様の平均一次粒子径が120nmの銅微粒子と、水溶液中で銅イオンからの無電解還元により調製された、平均一次粒子径が10μmの銅微粒子を70:30(質量比)で混合し、該混合物に還元性を有する有機溶媒としてグリセロールを銅微粒子濃度が50質量%になるように添加後十分に撹拌して導電性ペーストを調製した。
該導電性ペーストを使用し、加熱処理温度を300℃とした以外は、実施例1に記載したと同様にして、導電性基板とSiチップの端子とが電気的、機械的に接合している導電性ダイボンド部を作製した。該導電性ダイボンド部について実施例4と同様の評価を行った。その評価結果を表2に示す。
実施例5で使用したと同様の平均一次粒子径が120nmの銅微粒子と、水溶液中で銅イオンからの無電解還元により調製された、平均一次粒子径が15μmの銅微粒子を95:5(質量比)で混合し、該混合物に還元性を有する有機溶媒としてグリセロールを銅微粒子濃度が50質量%になるように添加後十分に撹拌して導電性ペーストを調製した。
該導電性ペーストを使用し、加熱処理温度を300℃とした以外は、実施例1に記載したと同様にして、導電性基板とSiチップの端子とが電気的、機械的に接合している導電性ダイボンド部を作製した。該導電性ダイボンド部の接合強度試験を行った。該導電性ダイボンド部について実施例4と同様の評価を行った。その評価結果を表2に示す。
実施例5で使用したと同様の平均一次粒子径が250nmの銅微粒子と、水溶液中で銅イオンからの無電解還元により調製された、平均一次粒子径が6μmの銅微粒子を95:5(質量比)で混合し、該混合物に還元性を有する有機溶媒としてグリセロールを銅微粒子濃度が50質量%になるように添加後十分に撹拌して導電性ペーストを調製した。
該導電性ペーストを使用し、加熱処理温度を300℃とした以外は、実施例1に記載したと同様にして、導電性基板とSiチップの端子とが電気的、機械的に接合している導電性ダイボンド部を作製した。該導電性ダイボンド部について実施例4と同様の評価を行った。その評価結果を表2に示す。
(i)体積空隙率
導電性バンプの空隙率は、走査型電子顕微鏡(SEM)を用いて、観察倍率1000~10000倍の電子顕微鏡写真を撮り、その断面像を解析することにより求めた。
導電性ダイボンド部の体積空隙率3~25%はA、25%超で35%以下はB、35%超はC、3%未満はDとした。
(ii)平均接合強度試験
導電性基板とSiチップが導電性ダイボンド部により電気的、機械的に接合された接合強度試験用のSiチップ接続サンプルをダイシェア試験機で導電性基板からSiチップを剥離させる際にかかった力を導電性ダイボンド部の接合面積で除して、単位面積当りの接合強度[N/mm2]を求めた。
(iii)粗大ボイドの有無
導電性ダイボンド部に5μm以上の粗大ボイドが観察されない場合はA、観察された場合はBとした。
(ニ)クラックの有無
導電性ダイボンド部、及びその接合面にクラックが観察されない場合はA、観察された場合はBとした。
Claims (17)
- 金属、及び合金から選択された1種又は2種以上からなる、平均一次粒子径が1~150nmの金属微粒子(P1)と、金属微粒子(P1)と同種金属で平均一次粒子径が1~10μmの金属微粒子(P2)からなり、
その配合割合(P1/P2)が80~95質量%/20~5質量%(質量%の合計は100質量%)である金属微粒子(P)と、有機溶媒(S)、又は有機溶媒(S)と有機バインダー(B)からなる有機分散媒(D)とを含み、金属微粒子(P)と有機分散媒(D)との配合割合(P/D)が50~85質量%/50~15質量%(質量%の合計は100質量%)であることを特徴とする導電性ペースト。 - 前記金属微粒子(P1)が、銅、金、銀、ニッケル、及びコバルトの中から選択される1種又は2種以上である、ことを特徴とする請求項1に記載の導電性ペースト。
- 前記有機分散媒(D)における有機溶媒(S)と有機バインダー(B)の配合割合(S/B)が80~100質量%/20~0質量%(質量%の合計は100質量%)である、ことを特徴とする請求項1又は2に記載の導電性ペースト。
- 前記有機分散媒(D)が水を含有しており、該水の含有量が有機溶媒(S)と水(W)との割合(S/W)で75~99.9質量%/25~0.1質量%(質量%の合計は100質量%)であることを特徴とする、請求項1から3のいずれかに記載の導電性ペースト。
- 前記有機溶媒(S)が、(i)常圧における沸点が100℃以上で、かつ分子中に1又は2以上のヒドロキシル基を有するアルコール及び/又は多価アルコールからなる有機溶媒(S1)、又は(ii)少なくとも、常圧における沸点が100℃以上で、かつ分子中に1又は2以上のヒドロキシル基を有するアルコール及び/又は多価アルコールからなる有機溶媒(S1)5~95体積%、並びにアミド基を有する有機溶媒(SA)95~5体積%からなる有機溶媒(S2)、である、ことを特徴とする請求項1から4のいずれかに記載の導電性ペースト。
- 前記有機溶媒(S1)が、エチレングリコール、ジエチレングリコール、1,2-プロパンジオール、1,3-プロパンジオール、1,2-ブタンジオール、1,3-ブタンジオール、1,4-ブタンジオール、2-ブテン-1,4-ジオール、2,3-ブタンジオール、ペンタンジオール、ヘキサンジオール、オクタンジオール、グリセロール、1,1,1-トリスヒドロキシメチルエタン、2-エチル-2-ヒドロキシメチル-1,3-プロパンジオール、1,2,6-ヘキサントリオール、1,2,3-ヘキサントリオール、1,2,4-ブタントリオール、トレイトール、エリトリトール、ペンタエリスリトール、ペンチトール、ヘキシトール及びイミノジエタノールの中から選択される1種又は2種以上である、ことを特徴とする請求項5に記載の導電性ペースト。
- 前記有機溶媒(SA)が、N-メチルアセトアミド、N-メチルホルムアミド、N-メチルプロパンアミド、ホルムアミド、N,N-ジメチルアセトアミド、1,3-ジメチル-2-イミダゾリジノン、N,N-ジメチルホルムアミド、1-メチル-2-ピロリドン、ヘキサメチルホスホリックトリアミド、2-ピロリジノン、ε-カプロラクタム、及びアセトアミドの中から選択される1種又は2種以上である、ことを特徴とする請求項5に記載の導電性ペースト。
- 前記有機バインダー(B)がセルロース樹脂系バインダー、アセテート樹脂系バインダー、アクリル樹脂系バインダー、ウレタン樹脂系バインダー、ポリビニルピロリドン樹脂系バインダー、ポリアミド樹脂系バインダー、ブチラール樹脂系バインダー、及びテルペン系バインダーの中から選択される1種又は2種以上である、ことを特徴とする請求項1から7のいずれかに記載の導電性ペースト。
- 前記セルロース樹脂系バインダーがアセチルセルロース、メチルセルロース、エチルセルロース、ブチルセルロース、及びニトロセルロース;アセテート樹脂系バインダーがメチルグリコールアセテート、エチルグリコールアセテート、ブチルグリコールアセテート、エチルジグリコールアセテート、及びブチルジグリコールアセテート;アクリル樹脂系バインダーがメチルメタクリレート、エチルメタクリレート、及びブチルメタクリレート;ウレタン樹脂系バインダーが2,4-トリレンジイソシアネート、及びp-フェニレンジイソシアネート;ポリビニルピロリドン樹脂系バインダーがポリビニルピロリドン、及びN-ビニルピロリドン;ポリアミド樹脂系バインダーがポリアミド6、ポリアミド66、及びポリアミド11;ブチラール樹脂系バインダーがポリビニルブチラール;テルペン系バインダーがピネン、シネオール、リモネン、及びテルピネオール、の中から選択される1種又は2種以上である、ことを特徴とする請求項8に記載の導電性ペースト。
- 前記導電性ペーストを加熱処理して金属多孔質体を形成する際に、有機溶媒(S)と有機バインダー(B)が蒸発又は熱分解する、ことを特徴とする請求項1から9のいずれかに記載の導電性ペースト。
- 請求項1から10のいずれかに記載の導電性ペーストを電子部品における半導体素子もしくは回路基板の電極端子又は導電性基板の接合面に載せた後、該導電性ペースト上に更に接続する他方の電極端子又は導電性基板の接合面を配置して加熱処理により焼結して形成された金属多孔質体からなる導電接続部材であって、
該金属多孔質体が平均粒子径1~10μmの金属微粒子(P2)に由来する粒子間に、平均粒子径1~150nmの金属微粒子(P1)に由来する粒子がその表面で部分的に結合した状態で存在していて、これらの金属微粒子間に空孔が分散している、ことを特徴とする導電接続部材。 - 前記導電接続部材が半導体素子間を接合するための導電性バンプである、ことを特徴とする請求項11に記載の導電接続部材。
- 前記導電接続部材が半導体素子と導電性基板間を接合するための導電性ダイボンド部である、ことを特徴とする請求項11に記載の導電接続部材。
- 前記加熱処理が両電極端子間、又は電極端子と基板間を0.5~15MPaで加圧した状態で行われる、ことを特徴とする請求項11から13のいずれかに記載の導電接続部材。
- 前記導電性ペーストの加熱処理温度が150~350℃である、ことを特徴とする請求項11から14に記載の金属多孔質体からなる導電接続部材。
- 前記導電性ペーストの加熱処理温度が250~300℃である、ことを特徴とする請求項11から14に記載の金属多孔質体からなる導電接続部材。
- 前記金属多孔質体の空隙率が5~35%である、ことを特徴とする請求項11から16に記載の金属多孔質体からなる導電接続部材。
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