JP2004107728A - Joining material and joining method - Google Patents

Joining material and joining method Download PDF

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Publication number
JP2004107728A
JP2004107728A JP2002272364A JP2002272364A JP2004107728A JP 2004107728 A JP2004107728 A JP 2004107728A JP 2002272364 A JP2002272364 A JP 2002272364A JP 2002272364 A JP2002272364 A JP 2002272364A JP 2004107728 A JP2004107728 A JP 2004107728A
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Prior art keywords
metal
temperature
joining
bonding
material
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JP2002272364A
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Japanese (ja)
Inventor
Masayoshi Hirose
Naoaki Kogure
Kaori Mikojima
Hiroshi Nagasawa
小榑 直明
廣瀬 政義
神子島 かおり
長澤 浩
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Ebara Corp
株式会社荏原製作所
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Priority to JP2002272364A priority Critical patent/JP2004107728A/en
Priority claimed from TW092125572A external-priority patent/TWI284581B/en
Publication of JP2004107728A publication Critical patent/JP2004107728A/en
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    • H01L2224/26Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
    • H01L2224/28Structure, shape, material or disposition of the layer connectors prior to the connecting process
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    • H01L2224/29299Base material
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Abstract

An object of the present invention is to make it possible to use as a high-temperature solder substitute without using lead.
A composite metal nanoparticle in which the periphery of a core made of metal particles having an average particle diameter of about 100 nm or less is bonded and coated with an organic substance containing C, H and / or O as a main component is used as a main agent for bonding.
[Selection diagram] None

Description

[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to a bonding material and a bonding method used for bonding various parts such as various electronic parts and mechanical parts such as semiconductor elements to each other, and in particular, by using composite metal nanoparticles, two or more parts. The present invention relates to a joining material and a joining method used for joining components.
[0002]
[Prior art]
2. Description of the Related Art Conventionally, for example, face-down bonding using a solder alloy or the like is frequently used for electrical connection between a current-carrying terminal of an electronic component and a circuit pattern terminal on a circuit board. That is, a semiconductor element such as a chip, a pellet, a die, or the like, which is an active or passive element that is not packaged and is called a naked element, is mounted on a circuit board while being electrically bonded. In this case, a so-called face-down bonding method is used in which a solder bump is formed in advance on an electrode pad of a semiconductor element, and the solder bump is arranged facing down to a terminal electrode of a circuit board and is heated and fused at a high temperature. Is becoming widely adopted. The solder bumps are generally formed on a three-layer metal thin film (Under Bump Metals) made of, for example, Cr (chromium), Cu (copper), and Au (gold) by using a resist by plating or vapor deposition. You. This mounting method is considered to be an effective method for mounting a semiconductor element because the mechanical strength after bonding is high and the electrical connection between the electrode of the semiconductor element and the terminal electrode of the circuit board can be performed collectively.
[0003]
In addition to the above-described solder bumps, reflow soldering using a solder paste containing a tin-lead eutectic alloy is widely used for metal-to-metal bonding, such as mounting of electronic components on a printed wiring board. In this reflow soldering, the solder paste is brought into contact with the metal surface to be joined and heated and melted, causing some metal diffusion from the metal surface to be joined to the molten solder, and when cooling, Physical and electrical bonding is performed by forming an alloy or an intermetallic compound at the interface. This tin-lead eutectic alloy, which has been frequently used in the past, has an advantage that its melting temperature is low and there is little fear of causing erosion of a metal surface to be joined. Also, when fabricating structures by combining mechanical parts, joining by brazing including soldering is often used.
[0004]
[Problems to be solved by the invention]
However, in recent years, the use of lead has been severely restricted from the viewpoint of global environmental protection, and it has been necessary to avoid the leakage of lead into the environment when discarding used electrical equipment, and to use brazing during manufacturing. To avoid the problem of lead-evaporation due to the melting of the tin-lead solder material and the scatter of lead oxide that inevitably occur and contaminate the work environment, solder joints using materials that do not contain lead will be used. Development of the attachment method is underway. As a result, Sn-Ag based solder (melting point to about 250 ° C.) as a substitute for eutectic solder having a melting point of about 180 ° C. has been put to practical use.
[0005]
However, for example, if the first bonding is performed by the above-described face-down bonding method or the like, and another component is bonded to the packaged component again using the same type of solder as the first bonding, the solder bonded first time Is melted by the second heating, so that the first joint is damaged.
[0006]
Therefore, conventionally, high-temperature solder containing 96% of Pb and having a melting point of 300 ° C. is used for the first joining, and a means using ordinary eutectic solder or Sn—Ag based solder is used for the second joining. ing.
However, there has been no example of successful development of a lead-free high melting point solder material that can respond to the above-mentioned regulations on the use of lead. Therefore, a high melting point solder containing as much as 96% Pb is used as the first solder.
Therefore, if lead cannot be used, this mounting technique cannot be used.
[0007]
Also, for example, when joining components of a heat exchanger or an aircraft, brazing is frequently used. In the joining method by brazing, the temperature of the portion to be joined at the time of joining becomes extremely high as 450 to 1000 ° C., since the joining method inevitably involves heating to the melting point of the metal material (brazing material) or more. When exposed to temperatures as high as 1000 ° C. at maximum, it is generally inevitable that a wide range of thermal deformation and large-scale thermal stress / strain of the member will occur. For this reason, there is a strong demand for the development of a component capable of reliably joining the above-mentioned parts requiring precision in shape and dimensions at a relatively low temperature without causing inconvenience such as thermal deformation.
[0008]
A method of forming a ball with a metal paste having ultrafine metal particles and using the ball instead of the solder bump has also been proposed (see Japanese Patent Application Laid-Open No. 9-326416). However, the metal ultrafine particles used here are, for example, the metal is evaporated in the presence of some gas in a vacuum to condense the ultrafine particles consisting of only the metal from the gas phase, thereby forming an ultrafine metal. It is considered to be ultrafine particles of a single metal produced by a method of obtaining fine particles, and it is considered that there are problems in stability, physical properties and cost.
[0009]
The present invention has been made in view of the above circumstances, and an object of the present invention is to provide a bonding material and a bonding method that can be used as a high-temperature solder replacement without using lead.
[0010]
[Means for Solving the Problems]
The invention according to claim 1 is a composite type metal having a structure in which a metal core composed of metal particles having an average particle size of about 100 nm or less is bonded and covered with an organic substance containing C, H and / or O as a main component. It is a bonding material that uses nanoparticles as the main agent for bonding.
The invention according to claim 2 is a bonding material in which composite metal nanoparticles bonded and coated with an organic substance generated from an organic acid metal salt as a main agent for bonding.
The invention according to claim 3 is a bonding material in which a composite metal nanoparticle obtained by heat-synthesizing a metal salt and an organic substance in a non-aqueous solvent and then reducing the resultant by heating is used as a main agent for bonding. .
The invention according to claim 4 is a method of mixing a metal salt, a metal oxide, a metal hydroxide, and an organic substance, heating and synthesizing the resultant, and then reducing the composite by heating and reducing the composite metal nanoparticle. It is a bonding material that was used.
The invention according to claim 5 is that, after mixing and heat-synthesizing a metal salt and an alcohol-based organic substance, a composite metal nanoparticle obtained by adding a reducing agent to the mixture and reducing by heating is used as a main agent for bonding. It is a joining material.
The invention according to claim 6 is a method in which a composite metal nanoparticle obtained by heat-synthesizing a metal salt and an organic substance in a non-aqueous solvent, adding a reducing agent thereto and heat-reducing the metal salt and the organic substance is used as a main agent for bonding. It is a joining material.
[0011]
It is known that the melting start temperature of metal particles decreases as the particle size decreases, but the effect starts to appear at 100 nm or less, and the effect becomes significant at 20 nm or less. In particular, depending on the metal, when the thickness is less than 10 nm, the metal is mutually melt-bonded at a temperature considerably lower than the melting point of the metal in a bulk state.
[0012]
Further, prior to melting, a particle sintering phenomenon occurs, but the sintering onset temperature is also significantly lower than in the case of bulk, and bonding occurs by low-temperature sintering.
For example, in the case of Ag ultrafine particles having an average particle diameter of 20 nm, published data that sintering starts at a low temperature of 60 to 80 ° C. ) P. 26).
[0013]
In addition, the composite metal nanoparticles having a structure in which the surface of the metal nucleus is bonded and covered with an organic material can be stably formed in an organic solvent by allowing the organic material to function as a protective film for protecting the metal nucleus. It is uniformly dispersed and has high property stability as particles. Therefore, it is possible to provide a liquid bonding material in which a bonding material (composite metal nanoparticles) that can be sintered and melt-bonded at a low temperature is uniformly dispersed.
[0014]
For example, in the case of cluster ultrafine silver particles having a size of about 5 nm, the apparent melting start temperature is about 210 ° C. By heating above this temperature, the ultrafine silver particles are fused or sintered. be able to.
[0015]
On the other hand, an adhesive in which ultrafine particles having a particle length of 20 nm or less are mixed with another material and an adhesive method using the same have been proposed (see, for example, JP-A-5-54942).
In the present method, the ultrafine particles are present in the medium in the form of a metal alone and, unlike the present invention, have no organic coating. According to our experiments, it is known that such bare metal ultrafine particles tend to aggregate and coarsen each other and easily fall into an uneven dispersion state.
[0016]
If the ultrafine particles aggregate and the large particles become the main body, the melting start temperature and sintering temperature of the large particles will be higher than those of the ultrafine particles, so low-temperature bonding will be difficult or impossible. However, the advantages of the method will be greatly impaired.
[0017]
In the case of adding the aggregate according to the present invention, the presence of particles larger than the nanoparticles is similar to the case of the agglomerated / coarsened particles, but in the former, the original nanoparticles are still present, so that low-temperature sintering is performed. In contrast to the progress of sintering, the latter is largely different in that low-temperature sintering does not occur because nanoparticles are almost completely eliminated.
[0018]
In the present invention, unlike the case where the ultrafine metal particles are dispersed alone in the medium as described in claim 1, the composite metal nanoparticles in which the periphery of the metal nucleus is bound and covered with an organic substance are dispersed in the medium. As a result, the particles do not agglomerate and coarsen with each other, and maintain a state of uniform dispersion, so that the above-described inconvenience can be avoided.
[0019]
On the other hand, when the organic substance contains elements other than C, H or O, such as nitrogen (N) and sulfur (S), even if a step of decomposing and evaporating the organic substance by heating at the time of joining is performed, The N or S component contained therein may remain in the sintered metal.
[0020]
As a result, the conductivity of the bonding layer may be adversely affected. For example, it is considered that a decrease in conductivity in a portion where the current density during operation is high, such as a high-density mounted component, for such a reason causes a serious problem.
[0021]
On the other hand, in the metal joint realized by the present invention, since the composite metal nanoparticles used do not contain N or S, the phenomenon that N or S remains at the joint even after the decomposition and evaporation of organic matter occurs at all. There is no.
Therefore, when a high-density mounting component is manufactured by the method of the present invention, the conductivity does not decrease due to the residual N and S components.
[0022]
In the invention according to claim 7, when dispersing composite metal nanoparticles having an average particle diameter of the metal core of about 100 nm or less in an organic solvent, the state of the bonding material after dispersion is adjusted by adjusting the conditions of dispersion. It is a bonding material that is semi-solidified into a liquid, a slurry, a paste or a cream, or a solid or a jelly.
[0023]
In the case of the liquid, it is practically preferable that the weight ratio of the metal portion to the total liquid is 1% or more and 30% or less.
Examples of the organic solvent include toluene, xylene, hexane, octane, decane, cyclohexane, pinene, limonene and the like.
[0024]
In the case of a slurry, paste or cream, it is practically preferable that the weight ratio of the metal portion to the total fluid is 15 to 90%.
Further, when the solidified or semi-solidified jelly is used, it is practically preferable that the weight ratio of the metal portion to the entire joining material be 20 to 95%.
[0025]
The invention according to claim 8 has a composite metal nanoparticle having a metal core bonded and coated with an organic substance, wherein the metal core portion has an average particle size of about 100 nm or less, and a bone having an average particle size of about 100 μm or less. A bonding material characterized by dispersing a material in an organic solvent and adjusting the viscosity to various values.
By adding the aggregate having an average particle diameter of about 100 μm or less as described above, various characteristics can be added unlike the case of the composite metal nanoparticles alone.
[0026]
According to a ninth aspect of the present invention, there is provided a bonding material in which the aggregate uses one or more of metal, plastic, and inorganic substances other than metal / plastic. The size of the aggregate is more preferably 0.1 to 1.0 μm.
[0027]
The invention according to claim 10 is a bonding material in which the inorganic substance includes, for example, various kinds of ceramics, carbon, diamond, and glass.
When the aggregate is a metal, the material is Al, Cu, Mg, Fe, Ni, Au, Ag, Pd, or a powder composed of a plurality of these elements. By adding an excellent metal powder as an aggregate, it is possible to secure stable strength and toughness of a joint portion and to improve conductivity.
[0028]
When the aggregate is plastic, the effect of reducing the weight of the joint is obtained. In particular, the use of a heat-resistant plastic powder, such as a polyimide, polyaramid, or polyetheretherketone powder, is convenient because the degree of deterioration and deterioration of the plastic is small even when exposed to the heating temperature at the time of joining.
Further, when the aggregate is any one of all inorganic substances other than metal and plastic, it is possible to simultaneously reduce the weight and increase the strength of the joint.
In addition, the above-mentioned aggregate may use only one kind of the substance alone, or may select a plurality of kinds of substances as necessary from many substances and use them in combination. .
[0029]
Next, Table 1 shows the content ratio of the above-mentioned aggregate to the whole joining material. However, in the case of a metal aggregate, it is indicated by a ratio of the total metal amount obtained by adding the amount of the metal core portion of the composite metal nanoparticles to the aggregate.
[Table 1]
Table 1 shows the upper limit of the content of the aggregate for each embodiment.
If the above content exceeds the upper limit, the fluidity during heating as a joining material is significantly reduced, so that when filling minute gaps with the joining material, an incompletely filled portion is likely to occur. Therefore, by setting the volume ratio of the aggregate to the entire joint material within the range shown in Table 1, the joint material (composite metal nanoparticles) that can be sintered and melt-bonded at a low temperature and the aggregate are mixed in an appropriate ratio. It is possible to provide a bonding material having desired fluidity.
[0030]
The invention according to claim 11 is a bonding material in which the material of the metal portion of the composite metal nanoparticle is one or more of Au, Ag, Pd, Pt, Cu, and Ni.
The invention according to claim 12 is a bonding material having composite metal nanoparticles in which two or more components are bonded and covered with an organic substance around a core made of metal particles having an average particle diameter of about 100 nm or less when bonding two or more parts. The entire surface or a part between the parts contact and intervene, applying energy to the whole or local, changing the form of the composite metal nanoparticles contained in the bonding material, between the composite metal nanoparticles, And / or bonding the composite metal nanoparticles to the surface of the component.
[0031]
The composite metal nanoparticles having changed morphology have the same properties as the metal in the bulk state, and in particular, the melting start temperature rises to the melting point in the bulk state. For example, in the case of silver whose metal core has a particle diameter of 5 nm, its melting point is about 210 ° C., but it is 961.93 ° C. in a bulk. Therefore, it becomes an ideal bonding material for repeated bonding required for high-temperature solder.
[0032]
In addition, according to the conventional joining method, there are cases where joining is difficult or impossible depending on the material type. However, according to this joining method, the same kind of material among metals, plastics, ceramics, etc., or a combination of different materials, etc. Basically, any material can be joined.
The bonding material can be brought into contact with or interposed on the entire surface or a part between the components by any method such as spraying, coating, dipping, spin coating, printing, dispensing, or inserting.
[0033]
A thirteenth aspect of the present invention is a bonding method in which the energy is applied by heating or by using both heating and pressurization.
Here, as the heating method, for example, means using combustion heat, electric heat, thermal fluid, energy beam irradiation, energization to the component itself, induction heating, dielectric heating, or plasma may be used.
[0034]
The invention according to claim 14 is a bonding method in which the heating temperature is set to a value within a range of 400 ° C. or less. The reason for limiting the temperature range by heating during joining will be described. The relationship between the particle size of ultra-fine particles of noble metal, which is often used practically, and the melting start temperature is studied. For example, FIG. 1 shows the relationship between the particle size of Au ultrafine particles and the melting onset temperature (see CRM Wronski, Brit. J. Appl. Phys., 18 (1967), p. 1731).
As is clear from FIG. 1, when the particle size is smaller than 10 nm, a sharp decrease in the melting start temperature appears. For example, when the particle diameter is 2 nm, the melting start temperature has dropped to around 120 ° C.
[0035]
For bonding, it is desirable to heat to as high a temperature as possible because atomic diffusion and sintering become active. However, in order to avoid deterioration of the semiconductor element due to high temperature, heating to a temperature exceeding 400 ° C. is allowed. Absent.
For the above reasons, the heating temperature for bonding according to the present invention is limited to 400 ° C. or less.
[0036]
The invention according to claim 15 is a bonding method in which the bonding is performed in air, dry air, an oxidizing gas atmosphere, an inert gas atmosphere, a vacuum, or an environment in which the amount of mist is reduced.
The above environment can be used to avoid contamination, alteration, deterioration, and the like of the surface to be bonded and to perform reliable bonding on a clean surface.
[0037]
The invention according to claim 16 is performed to improve the reliability of the bonding by making the surface roughness, activity, cleanliness and the like appropriate by performing the surface treatment of the surface to be bonded before performing the bonding. .
As means for surface treatment, for example, cleaning, pure water cleaning, chemical solution etching, corona discharge treatment, flame treatment, plasma treatment, ultraviolet irradiation, laser irradiation, ion beam etching, sputter etching, anodic oxidation, mechanical grinding, fluid grinding Alternatively, it is conceivable to perform at least one operation such as blasting.
[0038]
The method according to claim 17, wherein another component is joined to the structure joined by changing the form of the composite metal nanoparticles contained in the joining material, by the joining method or by another method. This is a joining method characterized by joining.
[0039]
This is because in the conventional soldering and brazing, the joining temperature is equal to the melting point of the solder and brazing material, so if the point once joined is heated again to the same temperature or more, it will melt and fluidize. In the case of the above, a completely different part, the melting start temperature and the sintering temperature drop phenomenon due to ultra-fine metal particles are used, so the previously joined part cannot be re-melted by the heat applied when joining later. Absent. That is, for example, in the case of a composite silver nanoparticle having a diameter of 5 nm, it is heated at 210 ° C. or higher and once bonded, the melting point of the bonded portion rises to 960 ° C. or higher which is the melting point of bulk metallic silver. Therefore, unless the temperature reaches 960 ° C. or more by reheating, re-melting does not occur, so that a one-way joining method can be practically performed. This is a greatly different feature from the fact that it is difficult to perform brazing a plurality of times unless different brazing materials having different temperatures are sequentially used depending on the reflow method for warming the entire part.
[0040]
That is, in this method, brazing can be repeatedly performed using the same bonding material. Therefore, not only the components manufactured by the present method can be joined to the components by the present method, but also the joined components can be joined to each other.
As a result, components that have been previously joined by the reflow method can be joined again and again by the reflow method, which is a very effective method especially for mounting electronic components.
[0041]
The invention according to claim 18 is a method for joining a structure comprising two or more independently formed parts, wherein the size of the metal core portion is an average particle size on the entire surface or a part between the structures. Bonding the structure by contacting and interposing a bonding material having a composite metal nanoparticle having a diameter of about 100 nm or less as a main agent for bonding, and changing the form of the composite metal nanoparticle contained in the bonding material. It is a joining method characterized by the following.
[0042]
The invention according to claim 19 is a bonding material that is heated and solidified to a temperature equal to or higher than a bonding temperature to bond the members, wherein the bonding material is chemically bonded to a metal core made of metal and the metal core, A joining material comprising an organic material that coats the outer shell of the metal nucleus, and having a temperature at which re-melting after solidification is at least twice as high as the joining temperature.
[0043]
The invention according to claim 20 is a bonding material in a solid or powder form at room temperature, which is heated and solidified to a temperature higher than the bonding temperature to bond the members, and the temperature at which the material is remelted after the solidification is twice the bonding temperature. It is a bonding material characterized by being higher than the above.
[0044]
The invention according to claim 21 is a bonding material that is heated and solidified to a temperature equal to or higher than a bonding temperature to bond the members, wherein the bonding material includes a metal core made of a metal and an organic material covering the outer shell. The bonding material is characterized in that the organic material does not contain nitrogen and sulfur, and the temperature at which the organic material remelts after solidification is at least twice as high as the bonding temperature.
[0045]
The invention according to claim 22 is the bonding material according to any one of claims 19 to 21, wherein the diameter of the metal core is 0.5 to 100 nm.
The invention according to claim 23 is characterized in that the material of the metal nucleus is one or more of Au, Ag, Pd, Pt, Cu or Ni. It is a joining material of description.
[0046]
The bonding material according to any one of claims 19 to 23, wherein the bonding material further includes an aggregate having an average particle size of 0.1 to 100 µm. It is.
The invention according to claim 25 is the joining material according to claim 24, wherein the aggregate is one or a combination of metals, plastics, and inorganic substances.
The invention according to claim 26 is the bonding material according to claim 25, wherein the inorganic substance is ceramic, carbon, diamond, or glass.
[0047]
The invention according to claim 27 is a joining material that joins members by being heated and solidified to a joining temperature or higher, wherein the joining material is a mixture of a metal salt in which a metal and an inorganic substance are bonded, and an organic substance. By heating the mixture, the inorganic substance is separated from the metal salt, and the metal core having a particle diameter of 0.5 to 100 nm made of the metal contains metal nanoparticles coated with the organic substance. It is a bonding material to be used.
[0048]
The invention according to claim 28 is the bonding material according to claim 27, wherein the organic substance is an alcohol-based organic substance.
The invention according to claim 29 is the bonding material according to claim 27 or 28, wherein the mixing and heating are performed in a non-aqueous solvent.
[0049]
The invention according to claim 30 is characterized in that a metal material having a diameter of 0.5 nm or more and 100 nm or less made of a metal is bonded between two or more parts to be bonded with a bonding material including metal nanoparticles coated with an organic substance. It is heated to a temperature that is equal to or higher than the decomposition start temperature of the organic substance and is equal to or lower than the melting temperature of the metal constituting the metal core as a bulk, and decomposes the organic substance of the bonding material applied between the members from the metal core. A metal core is fused to form a bulk metal, and the two or more parts are joined together, the joining material is applied between the joined member and another member, and at a temperature not lower than the decomposition start temperature of the organic substance. Yes, heated to a temperature below the melting temperature of the metal constituting the metal core as a bulk, without melting the bulk metal, the organic material of the bonding material applied between the bonded member and another member Decomposes and melts metal nuclei It is a bonding method of bonding a member and another member after the joining by.
[0050]
The invention according to claim 31 is characterized in that a metal material having a diameter of 0.5 nm or more and 100 nm or less made of a metal is bonded between two or more parts to be bonded with a bonding material including metal nanoparticles coated with an organic substance. Coating is performed so that an interval between the joining members adjacent to each other is 10 to 10,000 times the size of a metal nucleus included in the joining member, and is equal to or higher than the decomposition start temperature of the organic substance; Heating to a temperature equal to or lower than the melting temperature of the bulk of the constituent metal, decomposing the organic material of the bonding material applied between the members from the metal nucleus, fusing the metal nucleus to form a bulk metal, and forming the bulk metal. This is a joining method for joining parts.
[0051]
BEST MODE FOR CARRYING OUT THE INVENTION
Hereinafter, embodiments of the present invention will be described with reference to the drawings.
First, as shown in FIG. 2, a composite having a structure including a metal core 10 substantially composed of a metal component and a bonding / coating layer (organic substance layer) 12 composed of an organic substance containing C, H or O as a main component. Form the metal nanoparticles 14. Such a composite metal nanoparticle 14 is stable because the metal core 10 is covered with the binding / coating layer 12 made of an organic compound, and has a small tendency to aggregate in a solvent.
[0052]
The composite metal nanoparticles 14 are composed of an organic compound and a metal salt as a starting material, for example, a metal component derived from a carbonate, formate or acetate. A binding organic compound surrounds. At this time, the organic compound and the metal component are present in a state in which a part or all of them are integrated in a state of being chemically bonded, and the conventional nanoparticles stabilized by being coated with a surfactant. Differently, it is more stable and stable at higher metal concentrations.
[0053]
The average particle size of the metal cores 10 of the composite metal nanoparticles 14 is about 100 nm or less, preferably 20 nm or less, more preferably 10 nm or less. The minimum value of the average particle size of the metal core 10 is not particularly limited as much as possible, but is generally about 0.5 nm, preferably about 1.0 nm. With this configuration, the metal core 10 can be melted at a temperature considerably lower than the melting start temperature of the metal constituting the metal core 10, thereby enabling low-temperature sintering. For example, in the case of cluster ultrafine silver particles having a size of about 5 nm, the melting start temperature is about 210 ° C. By heating above this temperature, the ultrafine silver particles can be sintered and melt-bonded. .
[0054]
The composite metal nanoparticles 14 are used, for example, in a non-aqueous solvent and in the presence of a binding organic substance to convert a metal salt, for example, a carbonate, formate or acetate, to a temperature not lower than its decomposition reduction temperature and not higher than the decomposition temperature of the binding organic substance. And can be produced by heating. Ag, Au or Pd is used as the metal component, and as the binding organic substance, for example, a fatty acid having 5 or more carbon atoms and a higher alcohol having 8 or more carbon atoms are used.
[0055]
The heating temperature is equal to or higher than the decomposition reduction temperature of a metal salt, for example, a carbonate, formate or acetate, and is equal to or lower than the decomposition temperature of a binding organic substance. For example, in the case of silver acetate, the decomposition onset temperature is 200 ° C. The temperature may be maintained at a temperature of not less than 0 ° C. and a temperature at which the above-mentioned binding organic substance is not decomposed. In this case, the heating atmosphere is preferably an inert gas atmosphere in order to make it difficult for the binding organic substance to be decomposed. However, heating can be performed even in the atmosphere by selecting a non-aqueous solvent.
[0056]
When heating, various alcohols can be added, and the reaction can be promoted. The alcohol is not particularly limited as long as the above effects are obtained, and examples thereof include lauryl alcohol, glycerin, and ethylene glycol. The amount of the alcohol to be added can be appropriately determined according to the type of the alcohol to be used and the like, but is usually 5 to 20 parts by weight, preferably 5 to 10 relative to 100 parts by weight of metal salt.
After the heating is completed, purification is performed by a known purification method. The purification may be performed by, for example, centrifugation, membrane purification, solvent extraction, or the like.
[0057]
Then, the composite metal nanoparticles 14 are dispersed in a predetermined organic solvent such as toluene, xylene, hexane, octane, decane, cyclohexane, pinene or limonene to prepare a bonding material. The composite metal nanoparticles 14 having a structure in which the surface of the metal core 10 is covered with a bonding / coating layer (organic material layer) 12 made of an organic material serve as a protective film for protecting the metal core 10 on the organic material layer 12. By doing so, it is stably dispersed in a solvent, and has high property stability as particles. Therefore, it is possible to obtain a liquid bonding material in which a bonding material (composite metal nanoparticles 14) that can be sintered and melt-bonded at a low temperature is uniformly dispersed.
[0058]
Here, the composite metal nanoparticles 14 are dispersed in an organic solvent so that the weight ratio of the metal portion to the total liquid is preferably 1% or more and 85% or less, and a dispersant or a gelling agent is appropriately added thereto. By liquefaction, it is possible to obtain a liquid bonding material having desired fluidity at the time of heating in which a bonding material (composite metal nanoparticles 14) capable of being sintered and melt-bonded at a low temperature is uniformly dispersed. it can. When the weight ratio of the metal portion of the composite metal nanoparticles 14 to the total liquid exceeds 85%, the fluidity of the liquid bonding material is significantly reduced, so that when filling the fine gaps with the liquid bonding material, Imperfect part is likely to occur.
Further, when the weight ratio of the metal portion of the composite metal nanoparticles 14 to the total liquid is 1% or less, the amount of organic components contained in the bonding material is too large, so that degassing during firing becomes insufficient, and This ratio is limited to the above range because defects are likely to occur.
[0059]
The composite metal nanoparticles 14 are dispersed in an organic solvent so that the weight ratio of the metal portion to the total fluid is preferably 15 to 90%, and a dispersant or a gelling agent is appropriately added thereto to liquefy, A slurry or paste having desired fluidity at the time of heating, in which a joining material (composite-type metal nanoparticles 14) capable of being sintered and melt-bonded at a low temperature is uniformly dispersed by adjusting to a slurry, paste or cream form. Alternatively, a creamy bonding material can be obtained.
[0060]
The composite metal nanoparticles 14 are dispersed in an organic solvent so that the weight ratio of the metal portion to the total bonding material is preferably 20 to 95%, and a dispersant or a gelling agent is appropriately added thereto to liquefy. For example, a bonding material (composite metal nanoparticle 14) that can be sintered and melt-bonded at a low temperature by being formed into various shapes such as a rod shape, a string shape or a ball shape and solidified, or semi-solidified in a jelly shape. Can be obtained, and a solidified or semi-solidified bonding material having desired fluidity during heating can be obtained.
[0061]
At this time, if necessary, 0.1 to 10 μm, more preferably about 0.1 to 1.0 μm, for example, metal powder, plastic powder, inorganic powder other than metal and plastic alone, etc., Alternatively, an aggregate obtained by combining them may be added to be uniformly dispersed in the joining material. Thus, by adding the aggregate, various characteristics can be added unlike the case of the composite metal nanoparticles alone.
[0062]
As the aggregate, for example, a metal powder made of Al, Cu, Mg, Fe, Ni, Au, Ag, or Pd can be used. Thus, stable electric conductivity can be secured by adding various metal powders having excellent electric conductivity as aggregates.
[0063]
The content of the aggregate in the respective joining materials is determined by the upper limit value as shown in Table 1 depending on the mode of the joining material. If the above content exceeds the upper limit, the fluidity of the joining material during heating is significantly reduced, so that when filling the fine gaps with the liquid joining material, an incompletely filled portion is likely to occur. Therefore, by setting the volume ratio to the entirety of the aggregate within the range shown in Table 1, it is desirable to mix the bonding material (composite metal nanoparticles) that can be sintered and melt-bonded at a low temperature and the aggregate in an appropriate ratio. It is possible to provide a bonding material having fluidity.
[0064]
Next, a case where a semiconductor element (semiconductor chip) is bonded to a ceramic circuit board by a face-down bonding method using the above-described bonding material will be described with reference to FIG. Here, an example is shown in which composite silver ultrafine particles having metal nuclei 10 composed of cluster ultrafine silver particles having a size of 5 nm are used as composite metal nanoparticles 14.
[0065]
First, as shown in FIG. 3A, for example, a paste-like bonding material is applied (printed) to a predetermined position of the terminal electrode 22 of the ceramic circuit board 20, and the high-pressure material mainly composed of the composite metal nanoparticles 14 is applied. A composite metal bump 24 having a thickness of about 2 μm is formed.
Such composite metal bumps 24 are almost transparent when the composite metal nanoparticles 14 which are dispersed particles are very fine because the composite metal nanoparticles 14 are very fine. By appropriately selecting the concentration of the metal nanoparticles, the temperature, and the like, physical properties such as surface tension and viscosity can be adjusted.
[0066]
Next, as shown in FIG. 3B, a so-called flip chip is used in which the electrode pad portion provided on the semiconductor element 30 and the composite metal bump 24 are aligned using a face-down method with the semiconductor element 30 facing downward. The electrode pad portion of the semiconductor element 30 is bonded on the composite metal bump by a method, and leveling is performed according to the weight of the semiconductor element 30 as necessary. Of course, the face-up method may be used.
[0067]
In this state, for example, when composite silver ultrafine particles are used, since the melting start temperature is about 210 ° C., low-temperature sintering is performed at 210 to 250 ° C. for about 30 minutes using a hot air oven to obtain FIG. As shown in (c), the electrode pad portion of the semiconductor element 30 and the terminal electrode 22 of the circuit board 20 are joined via a joining layer 32 made of a silver layer. That is, the solvent such as toluene contained in the composite metal bumps 24 is evaporated, and the composite metal nanoparticles 14 which are the main components of the composite metal bumps 24 are further combined with the bonding / coating layer (organic material layer) 12 (see FIG. 2). The bonding / coating layer 12 is detached from the metal nucleus 10 by heating to a temperature at which the bonding / coating layer 12 itself decomposes or a temperature higher than the decomposition temperature of the bonding / coating layer 12 itself. The coating layer 12 is decomposed and evaporated. As a result, the metal nuclei (ultrafine silver particles) 10 are brought into direct contact with each other and sintered to form a silver layer. The bonding layer 32 made of the silver layer and the electrode pads of the semiconductor element 30 and the terminal electrodes 22 of the circuit board 20 are formed. Are brought into direct contact with each other to cause adhesion, and as a result, the electrode pad portion of the semiconductor element 30 and the terminal electrode 22 of the circuit board 20 are joined via the joining layer 32 made of a silver layer.
[0068]
In this way, by bonding the semiconductor element and the circuit board by firing at a low temperature in a temperature range of, for example, 210 to 250 ° C., lead-free bonding that can replace conventional solder bonding can be performed.
Moreover, as mentioned above, the re-melting temperature of the joint is much higher than the joining temperature, so once the joint has been made, another part can be joined at the same temperature or as many times as necessary, even if necessary. It has a great effect that it can be done.
[0069]
At this time, as described above, by using, as an aggregate, a bonding material to which a metal powder having a high conductivity is added, a high conductivity is secured through the metal powder, and the reliability of the semiconductor element mounting is improved. You can also. As described above, when the bonding material to which the metal powder is added is used, the composite metal nanoparticles and the surface of the aggregate (metal powder) come into direct contact with the change in the form of the composite metal nanoparticles described above. Join. The same applies to the case where inorganic powder such as plastic powder or ceramic is used as the aggregate.
[0070]
Then, as shown in FIG. 3D, when the semiconductor element 30a is also joined to the back surface side of the ceramic circuit board 20, for example, a paste-like joining material is applied to the terminal electrodes of the ceramic circuit board 20 in the same manner as described above. The composite metal bumps 24a are formed by applying to predetermined positions of the composite metal bumps 22a. In this state, when using composite silver nanoparticles, for example, at a temperature of 210 to 250 ° C. for about 30 minutes, a low temperature Perform baking. Thereby, the electrode pad portion of the semiconductor element 30a and the terminal electrode 22a of the circuit board 20 are joined via the joining layer 32a made of a silver layer.
[0071]
At this time, the composite metal nanoparticle in which the form has changed, that is, the bonding layer 32 made of the silver layer formed earlier has changed to the same properties as the metal in the bulk state, and particularly, the bonding layer has the same melting point as the bulk state, that is, It has a temperature of 961.93 ° C, and once fused, it cannot be re-melted unless it is 961.93 ° C or higher. Therefore, it is not melted by the heating at the time of joining to the back surface, and provides an ideal joining material required for high-temperature solder for repeated joining.
[0072]
The paste-like joining material can be supplied by any method such as spraying, brushing, dip, spin coating, dispensing, screen printing, and transfer, without being limited to a simple coating method.
In addition, according to this joining method, basically, all kinds of parts can be joined, such as parts of the same kind of materials such as metals, plastics, and ceramics, or combinations of parts of different kinds of materials.
[0073]
In this example, the application of energy for changing the form of the composite metal nanoparticles contained in the bonding material is performed by heating with a hot blast stove (low-temperature sintering). Any method such as energization between components, induction heating or dielectric heating of components may be used. When the morphology of the composite metal nanoparticles is changed by these methods, the composite metal nanoparticles are bonded to each other or between the added metal powder or other additives and various materials to be bonded by sintering and / or melting.
[0074]
The present invention is a bonding method for setting the heating temperature to a value within a range of 400 ° C. or less. The reason for limiting the temperature range by heating during joining will be described. The relationship between the particle size of ultrafine particles of a noble metal, which is often used practically, and the melting start temperature will be examined with reference to FIG.
According to FIG. 1, when the particle size of the Au ultrafine particles is smaller than 10 nm, a sharp decrease in the melting start temperature point appears. For example, if the particle size is 2 nm, this temperature has dropped to 120 ° C.
On the other hand, when the heating temperature exceeds 400 ° C., deterioration and damage of semiconductor elements and the like used in electronic components become remarkable.
As a result of the above considerations, the upper limit of the heating temperature is set to 400 ° C.
[0075]
Here, the bonding can be performed in the air, in dry air, in an inert gas atmosphere, in a vacuum, or in an environment in which the amount of mist is reduced. In particular, for example, by performing the bonding in a clean atmosphere, it is possible to prevent the surfaces to be bonded from being contaminated with mist such as mineral oil, oil and fat, a solvent, and water that are scattered or floated in the air before the bonding.
[0076]
Further, surface treatment of the surface to be joined of the component prior to joining includes cleaning / degreasing with an organic solvent or pure water, ultrasonic cleaning, chemical solution etching, corona discharge treatment, flame treatment, plasma treatment, ultraviolet irradiation, laser irradiation. And at least one operation of ion beam etching, sputter etching, anodic oxidation, mechanical grinding, fluid grinding or blasting.
This makes it possible to create a surface morphology suitable for joining by removing contamination and foreign matter on the surface of the member to be joined and changing the roughness of the surface prior to the joining step.
[0077]
【The invention's effect】
As described above, according to the present invention, it is possible to provide a bonding material and a bonding method that can be used as a high-temperature solder substitute without using lead.
[Brief description of the drawings]
FIG. 1 is a diagram showing the relationship between the particle size of Au ultrafine particles and the melting start temperature.
FIG. 2 is a view schematically showing a composite metal nanoparticle having a bonding / coating structure with an organic substance used in the present invention.
FIG. 3 is a view showing a bonding method according to one embodiment of the present invention in the order of steps.
[Explanation of symbols]
10 Metal core
12 Bonding and coating layers
14 Composite metal nanoparticles
20 circuit board
22, 22a Terminal electrode
24 Composite Metal Bump
30, 30a Semiconductor element
32, 32a bonding layer

Claims (31)

  1. A bonding material mainly composed of composite metal nanoparticles in which the periphery of a core made of metal particles having an average particle diameter of about 100 nm or less is bonded and coated with an organic substance containing C, H and / or O as a main component.
  2. The bonding material according to claim 1, wherein the organic substance is generated from an organic acid metal salt.
  3. 2. The bonding material according to claim 1, wherein the composite metal nanoparticles are produced by heat-synthesizing a metal salt and an organic substance in a non-aqueous solvent, and then reducing the resultant by heating. 3.
  4. The composite metal nanoparticles are produced by mixing and heating and synthesizing a metal salt, a metal oxide, a metal hydroxide, and an organic substance, and then reducing the mixture by heating. The bonding material according to 1.
  5. The composite metal nanoparticles are produced by mixing and heating a metal salt and an alcoholic organic substance, adding a reducing agent thereto, and reducing the mixture by heating. Joining material.
  6. 2. The composite metal nanoparticles are produced by heat-synthesizing a metal salt and an organic substance in a non-aqueous solvent, and then adding a reducing agent thereto and reducing by heating. Joining material.
  7. The composite metal nanoparticles are liquefied by being dispersed in an organic solvent and used for bonding, or the liquefied one is further used as a slurry, paste or cream to be used for bonding, or liquefied. The joining material according to any one of claims 1 to 6, wherein the joining material is formed into various shapes and solidified or semi-solidified in a jelly shape and used for joining.
  8. The bonding material according to any one of claims 1 to 7, wherein the bonding material further contains an aggregate having an average particle diameter of about 100 µm or less, in addition to the composite metal nanoparticles.
  9. 9. The bonding material according to claim 8, wherein the aggregate is one or a combination of any one of a metal, a plastic, and an inorganic substance other than a metal / plastic.
  10. 10. The bonding material according to claim 9, wherein the inorganic substance includes, for example, various kinds of ceramics, carbon, diamond, and glass.
  11. The joint according to any one of claims 1 to 10, wherein the material of the metal core portion of the composite metal nanoparticle is one or more of Au, Ag, Pd, Pt, Cu, and Ni. material.
  12. In joining two or more components, the joining material according to any one of claims 1 to 11 is brought into contact with or interposed on the entire surface or a part between the components, and imparts energy entirely or locally. Bonding, by changing the form of the composite metal nanoparticles contained in the bonding material, to bond between the particles, the particles and the surface of the aggregate, and / or the particles and the surface of the component. Method.
  13. 13. The joining method according to claim 12, wherein the application of the energy is performed by heating, or by using both heating and pressurizing.
  14. 14. The joining method according to claim 12, wherein an object to be joined is heated to a temperature within a range of 400 ° C. or less by the means according to claim 13.
  15. The method according to any one of claims 12 to 14, wherein the bonding is performed in air, dry air, an oxidizing gas atmosphere, an inert gas atmosphere, a vacuum, or an environment in which the amount of mist is reduced. Joining method.
  16. The bonding method according to any one of claims 12 to 15, wherein the surface to be bonded is subjected to a surface treatment prior to the bonding.
  17. 17. The method according to claim 12, wherein the composite metal nanoparticles contained in the bonding material are changed in morphology, and the structure is bonded to the bonded structure by the necessary number of times. The joining method according to any one of claims 12 to 16, wherein the joining is performed by using.
  18. The joining method according to any one of claims 12 to 17, wherein the part to be joined according to claim 12 is a structure including two or more independently formed parts.
  19. A bonding material that is heated and solidified to a temperature higher than a bonding temperature to bond the members, wherein the bonding material is a metal nucleus made of metal, and is chemically bonded to the metal nucleus, and covers an outer shell of the metal nucleus. A bonding material comprising an organic material, wherein a temperature at which the material is remelted after solidification is at least twice as high as the bonding temperature.
  20. A joining material in a solid or powder form at room temperature, which is heated and solidified to a temperature higher than the joining temperature to join the members, wherein the temperature at which the material is remelted after solidification is at least twice as high as the joining temperature. .
  21. A bonding material that is heated to a temperature equal to or higher than a bonding temperature and solidifies to bond the members, wherein the bonding material includes a metal core made of a metal and an organic material covering the outer shell, and the organic material contains nitrogen and sulfur. And a temperature at which re-melting after solidification is at least twice as high as the bonding temperature.
  22. 22. The bonding material according to claim 19, wherein the diameter of the metal core is 0.5 to 100 nm.
  23. 23. The bonding material according to claim 19, wherein a material of the metal nucleus is one or more of Au, Ag, Pd, Pt, Cu, and Ni.
  24. 24. The bonding material according to claim 19, wherein the bonding material further includes an aggregate having an average particle size of 0.1 to 100 [mu] m.
  25. The joining material according to claim 24, wherein the aggregate is one or a combination of metals, plastics, and inorganic substances.
  26. The joining material according to claim 25, wherein the inorganic substance is ceramic, carbon, diamond, or glass.
  27. A bonding material that is heated to a temperature equal to or higher than a bonding temperature and solidifies to bond the members, wherein the bonding material is obtained by mixing a metal salt in which a metal and an inorganic substance are bonded, and an organic substance, and heating the mixture to form the metal. A bonding material, which separates an inorganic substance from a salt and includes metal nanoparticles coated with the organic substance in the outer shell of a metal core having a particle diameter of 0.5 to 100 nm made of the metal.
  28. The bonding material according to claim 27, wherein the organic substance is an alcohol-based organic substance.
  29. 29. The bonding material according to claim 27, wherein the mixing and heating are performed in a non-aqueous solvent.
  30. An outer shell of a metal nucleus having a diameter of 0.5 nm or more and 100 nm or less made of a metal is applied between two or more components to be joined with a joining material including metal nanoparticles coated with an organic substance,
    It is heated to a temperature that is equal to or higher than the decomposition start temperature of the organic substance and is equal to or lower than the melting temperature of the metal constituting the metal core as a bulk, and decomposes the organic substance of the bonding material applied between the members from the metal core to form the metal core. Fusing to form a bulk metal and joining the two or more parts;
    Applying the joining material between the joined member and another member,
    It is heated to a temperature equal to or higher than the decomposition start temperature of the organic substance and equal to or lower than the melting temperature of the metal constituting the metal nucleus as a bulk, without melting the bulk metal, between the joined member and another member. A bonding method for decomposing an organic substance of a bonding material applied to a metal core from a metal core and fusing the metal core to bond the joined member to another member.
  31. Between two or more parts to be joined with a joining material containing metal nanoparticles in which the outer shell of a metal nucleus made of metal having a diameter of 0.5 nm or more and 100 nm or less is coated with an organic substance, between the joining members adjacent to each other. The interval is applied so as to be 10 to 10,000 times the size of the metal core included in the joining member,
    It is heated to a temperature that is equal to or higher than the decomposition start temperature of the organic substance and is equal to or lower than the melting temperature of the metal constituting the metal core as a bulk, and decomposes the organic substance of the bonding material applied between the members from the metal core to form the metal core. A joining method for joining the two or more components by fusing to form a bulk metal.
JP2002272364A 2002-09-18 2002-09-18 Joining material and joining method Pending JP2004107728A (en)

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US10/484,454 US20040245648A1 (en) 2002-09-18 2003-09-17 Bonding material and bonding method
CNB038009056A CN100337782C (en) 2002-09-18 2003-09-17 Joining material and joining method
PCT/JP2003/011797 WO2004026526A1 (en) 2002-09-18 2003-09-17 Bonding material and bonding method
EP03788702A EP1578559B1 (en) 2002-09-18 2003-09-17 Bonding method
DE60326760A DE60326760D1 (en) 2002-09-18 2003-09-17 Process for connecting
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