CN116079277A - In-Cu@Ag solder pre-prepared sheet and preparation method thereof - Google Patents

In-Cu@Ag solder pre-prepared sheet and preparation method thereof Download PDF

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Publication number
CN116079277A
CN116079277A CN202310045341.XA CN202310045341A CN116079277A CN 116079277 A CN116079277 A CN 116079277A CN 202310045341 A CN202310045341 A CN 202310045341A CN 116079277 A CN116079277 A CN 116079277A
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China
Prior art keywords
nano
particles
solder preform
core
solder
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Pending
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CN202310045341.XA
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Chinese (zh)
Inventor
李益兵
孙小航
顾小军
刘威
高阳
温志成
张鑫月
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Nanjing Hengdian Advanced Microwave Technology Research Institute Co ltd
Nanjing Hengdian Electronics Co ltd
Harbin Institute of Technology
Original Assignee
Nanjing Hengdian Advanced Microwave Technology Research Institute Co ltd
Nanjing Hengdian Electronics Co ltd
Harbin Institute of Technology
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Priority to CN202310045341.XA priority Critical patent/CN116079277A/en
Publication of CN116079277A publication Critical patent/CN116079277A/en
Pending legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/24—Selection of soldering or welding materials proper
    • B23K35/26—Selection of soldering or welding materials proper with the principal constituent melting at less than 400 degrees C
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/17—Metallic particles coated with metal
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • B22F5/006—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of flat products, e.g. sheets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/02—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape
    • B23K35/0222—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in soldering, brazing
    • B23K35/0233—Sheets, foils

Abstract

The invention provides an In-Cu@Ag solder preform and a preparation method thereof, comprising the steps of preparing nano Cu particles by reducing soluble copper salt In a liquid phase; preparing nano Cu@Ag, namely adding a silver nitrate solution into a dispersion system of copper powder and trisodium citrate, and performing displacement reaction on the surfaces of copper particles to form Cu@Ag core shells; preparing an In-Cu@Ag solder preform, namely preparing In foil or micron In particles and a nano Cu@Ag core-shell material by a pressurizing or heating pressurizing mode to form the solder preform; the In-Cu@Ag solder prepared by the method can realize low-temperature connection and high-temperature service, so that the interconnection temperature and the interconnection condition are reduced, and the pores and holes In the formed joint can be effectively reduced; the chip and the substrate can be interconnected under the condition of low temperature and no pressure, and the method can be well applied to the fields of manufacturing of semiconductor devices, microelectronic packaging, power electronic packaging and the like.

Description

In-Cu@Ag solder pre-prepared sheet and preparation method thereof
Technical Field
The invention belongs to the technical field of electronic packaging micro-interconnection, and particularly relates to an In-Cu@Ag solder pre-manufactured sheet and a preparation method thereof.
Background
With the rapid development of third generation power semiconductor devices such as silicon carbide (SiC) and gallium nitride (GaN), the service temperature of the third generation power semiconductor devices can reach 250 ℃ to 300 ℃, and the conventional chip-mounting interconnection material is difficult to meet the high-temperature working condition, so that new alternative materials are urgently required to be searched. The melting point of the metal nano-particles is reduced along with the reduction of the size of the nano-particles due to the size effect of the metal nano-materials, so that the metal nano-materials can be sintered and molded at a temperature far lower than the melting point of the block. Meanwhile, the nano material can stably work for a long time at a higher temperature after being sintered, so that the requirements of low-temperature sintering and high Wen Fuyi are well met, and the nano material is an ideal chip interconnection material. The sintering temperature of the nano Ag is low, the service temperature is high, and the nano Ag has excellent electrical conductivity and thermal conductivity, strong corrosion resistance and oxidation resistance, but the electromigration and chemical migration phenomena are serious, short circuit failure is easy to occur in a circuit, and the reliability of a product is seriously affected. Nano Cu is extremely easy to oxidize, and the generated oxide can increase the sintering temperature and also can influence the electric conductivity and the thermal conductivity of welding spots.
In order to solve the problems, researchers prepare a nano Cu@Ag core-shell structure. The structural characteristics of the inner core Cu shell Ag can fully exert the advantages of the two materials, and can meet the requirements of improving the migration resistance of silver and enhancing the oxidation resistance of copper, but the nano core-shell material has the problems of larger porosity and holes.
Disclosure of Invention
In order to solve the problems, the invention discloses an In-Cu@Ag solder preform and a preparation method thereof.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
the invention provides a preparation method of an In-Cu@Ag solder preform, which comprises the following steps:
step (1) preparation of nano Cu particles: the nano Cu particles are prepared by using a chemical reduction method through oxidation-reduction reaction of soluble copper salt and a reducing agent in a liquid phase;
and (2) preparing a nano Cu@Ag core-shell material: adding the nano Cu particles obtained in the step (1) into ethylene glycol, and then adding trisodium citrate to prepare a dispersion system of the nano Cu particles and trisodium citrate; adding a silver nitrate solution into a dispersion system of nano Cu particles and trisodium citrate by adopting a displacement reaction method, washing powder for three times by using distilled water, and drying at 40 ℃ to obtain a nano Cu@Ag core-shell material;
and (3) preparing an In-Cu@Ag solder preform: and (3) preparing the In foil or the micron In particles and the nano Cu@Ag core-shell material obtained In the step (2) by a pressurizing or heating pressurizing mode to form an In-Cu@Ag solder preform.
Further, in the step (1), cu is oxidized and reduced in a liquid phase by a soluble copper salt and a reducing agent under the state of normal temperature and pressure (or a temperature slightly higher than 100 ℃ C.) or under hydrothermal conditions 2+ Reducing the copper into Cu atoms so as to grow into copper simple substances with different morphologies, and preparingPreparing nano Cu particles; wherein the soluble copper salt comprises any one of copper sulfate and copper nitrate, and the reducing agent comprises any one of hydrazine hydrate, ascorbic acid, sodium hypophosphite and formaldehyde.
Further, in the step (2), the addition amount of the ethylene glycol is 100ml, the addition amount of the nano Cu particles is 0.08mol, and the addition amount of the trisodium citrate is 0.016mol.
Further, the content and structure of the obtained copper-silver bimetallic component are different along with the different addition of silver nitrate; the molar ratio of the silver nitrate solution to the nano Cu particles to the trisodium citrate in the step (2) is 1: 5-8: 1.
further, the reaction temperature of the displacement reaction method in the step (2) is 25-90 ℃, and the reaction time is 20-60 min.
Further, in the step (3), the preparation of the In-Cu@Ag solder preform comprises the following steps: and (3) arranging the nano Cu@Ag core-shell particles and In foil prepared In the step (2) In a die according to the sequence of the In foil, the nano Cu@Ag core-shell particles and the In foil, wherein the thickness of the In foil is 25-50 mu m, the adding amount of the nano Cu@Ag core-shell particles is 0.08-0.16 mol, heating to 150 ℃ and simultaneously applying the pressure of 10-40 MPa for 5-10 min, so that the Ag shells are melted to form connecting necks serving as prefabricated piece frameworks, and melting and filling the pores of the prefabricated pieces by the In foil to obtain the In-Cu@Ag solder prefabricated pieces.
Further, in the step (3), the preparation of the In-Cu@Ag solder preform comprises the following steps: firstly, placing the nano Cu@Ag core-shell material prepared In the step (2) into a die, heating to 150 ℃ for presintering to form a prefabricated sheet framework, reducing the porosity of the prefabricated sheet framework to 10% -20% by using a roll press, preparing In into soldering paste, printing on the prefabricated sheet framework by using screen printing single side, wherein the In content In the soldering paste is 75% -90% of the mass of the soldering paste, adopting In powder with the size of 200-300 meshes, heating to 160 ℃ for 5-10 min, and cooling to obtain the In-Cu@Ag solder prespecified sheet.
Further, in the step (3), the preparation of the In-Cu@Ag solder preform comprises the following steps: mixing the nano Cu@Ag core-shell material prepared In the step (2) with micron In particles, wherein the size of the micron In particles is 1-5 mu m, and the mass ratio of the prepared nano Cu@Ag core-shell material to the micron In particles is 20-25: and 1, placing the solder In a die, applying a pressure of 20-40 MPa, and maintaining the pressure for 5-10 min to obtain the In-Cu@Ag solder pre-manufactured sheet.
The invention also provides an In-Cu@Ag solder pre-manufactured sheet, which is prepared by the preparation method.
The beneficial effects of the invention are as follows:
in-cu@ag solder preform has a melting point of In of only 156.6 ℃, so that joining can be performed at a lower reflow temperature. When the In layer is completely depleted, the service temperature is increased after the intermetallic compound is generated. Thus, low temperature connection can be achieved, high Wen Fuyi;
the intermetallic compound generated when In is connected with Ag can improve the joint strength;
(3) Because the contact area between In and Ag In the In-Cu@Ag solder preform is large, compared with the traditional TLP (Transient Liquid Phase transient liquid phase) connection, the method has a higher reaction speed;
(4) In and nano Cu@Ag core-shell can be matched with each other, so that space is fully utilized, and porosity is reduced. The cost of raw materials can be greatly reduced, and the porosity can be reduced by playing a great advantage in industrialized mass production;
(5) In, ag and Cu can generate intermetallic compounds, and the joint strength is improved because the internal Cu nucleus still exists after the reaction is completed. Compared with the traditional full IMCs (Intermetallic Compound intermetallic compound) weld, the Cu core can better absorb external stress, so that local stress concentration is relieved, and the shearing resistance of the weld is improved. In addition, as Cu has good electric and heat conducting capacities, the electric and heat conducting capacities of the finally formed welding seam are greatly improved compared with those of the traditional full IMCs welding seam;
(6) Compared with the traditional soldering paste, the soldering paste pre-manufactured sheet can increase the alloy amount and avoid the adhesion of the soldering paste while not increasing the soldering flux.
Drawings
FIG. 1 is a schematic diagram of the structure of an In-Cu@Ag solder preform according to the present invention.
Description of the embodiments
The present invention is further illustrated in the following drawings and detailed description, which are to be understood as being merely illustrative of the invention and not limiting the scope of the invention.
Examples
The embodiment provides an In-Cu@Ag solder pre-manufactured sheet and a preparation method thereof, wherein nano Cu particles are prepared by a liquid phase reduction method, then nano Cu@Ag core-shell materials are prepared by a displacement method, and the In-Cu@Ag solder pre-manufactured sheet is prepared by a heating and pressurizing mode In a die, and the specific implementation steps are as follows:
(1) Preparation of nano Cu particles:
35.85 g sodium hypophosphite, 2.5 g PVP and 100ml ethylene glycol are poured into a three-neck flask 1, heated to 90 ℃ and stirred for dissolution;
7.9g of copper nitrate is poured into a three-neck flask 2, then 100ml glycol is poured into the three-neck flask, and the three-neck flask is heated to 90 ℃ and stirred for dissolution;
keeping the three-neck flask 1 continuously heated and stirred, pouring the solution in the three-neck flask 2 into the three-neck flask 1, and continuously heated and stirred for reaction for 20 min;
stopping heating and cooling to room temperature after the reaction is finished, adding deionized water for dilution, centrifuging for 15 min at 6000 r/min by using a centrifuge to enable nano copper particles to settle, pouring out supernatant, adding deionized water, performing ultrasonic dispersion to enable the nano copper particles to be sufficiently cleaned in the deionized water, centrifuging to pour out supernatant, repeatedly cleaning for 3 times, adding absolute ethyl alcohol, performing ultrasonic dispersion to enable the nano copper particles to be sufficiently cleaned in the absolute ethyl alcohol, centrifuging to pour out supernatant, repeatedly cleaning for 3 times, finally placing the collected nano copper particles in a vacuum drying box, and drying for 4 h at room temperature under the vacuum condition of-1 MPa to obtain nano Cu particles;
(2) Preparing a nano Cu@Ag core-shell material:
after fully grinding and dispersing the obtained nano Cu particles, weighing 5.12g of nano Cu particles, pouring the nano Cu particles into a three-neck flask 3, adding 100ml of ethylene glycol, adding 4.13g of trisodium citrate, heating the three-neck flask 3 to 90 ℃, and stirring for dissolution;
into a three-necked flask 4, 100ml glycol solvent was poured. Then adding 2.72g of silver nitrate, heating to 90 ℃, stirring and dissolving, namely pouring the solution in the three-neck flask 4 into the three-neck flask 3, and reacting for 20 min to finish silver shell coating; after the reaction is completed, taking out the solution, centrifuging at 6000 r/min for 15 min by using a centrifuge to enable particles to settle, pouring out supernatant, adding deionized water, performing ultrasonic dispersion to enable nano copper particles to be fully cleaned in the deionized water, centrifuging to pour out supernatant, repeatedly cleaning for 4 times, adding absolute ethyl alcohol, performing ultrasonic dispersion to enable the nano copper particles to be fully cleaned in the absolute ethyl alcohol, centrifuging to pour out supernatant, placing the collected particles in a vacuum drying box, and drying at room temperature under-1 MPa vacuum for 1 h to obtain nano Cu@Ag nuclear shell particle materials;
(3) Preparation of In-Cu@Ag solder preform sheet:
arranging the prepared nano Cu@Ag core-shell particles and In foil In the order of In foil-nano Cu@Ag particles-In foil In a die, heating to 150 ℃ and applying a pressure of 40+/-5 MPa for 5-10 min while keeping the thickness of the In foil to 25+/-5 mu m, melting the Ag shells to form a prefabricated sheet skeleton, melting the In foil and filling the pores of the prefabricated sheet, and obtaining the In-Cu@Ag solder prefabricated sheet.
The using method comprises the following steps:
(1) After the surface of the component is coated with solder paste, adding a solder pre-sheet at the tail end of a solder paste pattern to obtain an integral device;
(2) Sintering the integral device to obtain an interconnection device;
examples
This embodiment differs from embodiment 1 in that: in the step (1), copper sulfate pentahydrate is used as a copper source; in the second step, citric acid was used instead of sodium citrate, and CTAB (cetyltrimethylammonium bromide) was added as a surfactant.
The using method comprises the following steps:
(1) After the surface of the component is coated with solder paste, adding a solder pre-sheet at the tail end of a solder paste pattern to obtain an integral device;
(2) Sintering the integral device to obtain an interconnection device;
examples
This embodiment differs from embodiment 1 in that: in the first step, copper sulfate is selected as a copper source; in the second step, hydrazine hydrate is used as a reducing agent. The method has the advantages of high reaction speed, high purity of the prepared metal powder and low cost of raw materials. Furthermore, the oxidation product of hydrazine hydrate is clean N 2 。
The using method comprises the following steps:
(1) After the surface of the component is coated with solder paste, adding a solder pre-sheet at the tail end of a solder paste pattern to obtain an integral device;
(2) Sintering the integral device to obtain an interconnection device;
examples
This embodiment differs from embodiment 1 in that: in the step (3), the prepared nano Cu@Ag core-shell material is firstly placed In a mould and heated to 150 ℃ for presintering to form a framework, a roll press is used for reducing the porosity of the prefabricated sheet framework to 20-30%, in is prepared into soldering paste, screen printing is used for single-sided printing on the prefabricated sheet framework, the In content of the used soldering paste is 75% of the mass of the soldering paste, the size of the adopted In powder is 200-300 meshes, the temperature is kept for 10min after heating to 160 ℃, and the In-Cu@Ag solder prefabricated sheet can be obtained after cooling.
The using method comprises the following steps:
(1) After the surface of the component is coated with solder paste, adding a solder pre-sheet at the tail end of a solder paste pattern to obtain an integral device;
(2) Sintering the integral device to obtain an interconnection device;
examples
This embodiment differs from embodiment 1 in that: in the step (3), the prepared nano Cu@Ag core-shell material is mixed with micron In particles, the size of the micron In particles is 5 mu m, and then the mixture is placed In a die, the pressure of 40+/-5 MPa is applied, and the pressure is maintained for 10 minutes, so that an In-Cu@Ag solder preform is obtained.
The using method comprises the following steps:
(1) After the surface of the component is coated with solder paste, adding a solder pre-sheet at the tail end of a solder paste pattern to obtain an integral device;
(2) Sintering the integral device to obtain an interconnection device;
it should be noted that the foregoing merely illustrates the technical idea of the present invention and is not intended to limit the scope of the present invention, and that a person skilled in the art may make several improvements and modifications without departing from the principles of the present invention, which fall within the scope of the claims of the present invention.

Claims (9)

1. The preparation method of the In-Cu@Ag solder preform is characterized by comprising the following steps of:
step (1) preparation of nano Cu particles: the nano Cu particles are prepared by using a chemical reduction method through oxidation-reduction reaction of soluble copper salt and a reducing agent in a liquid phase;
and (2) preparing a nano Cu@Ag core-shell material: adding the nano Cu particles obtained in the step (1) into ethylene glycol, and then adding trisodium citrate to prepare a dispersion system of the nano Cu particles and trisodium citrate; adding a silver nitrate solution into a dispersion system of nano Cu particles and trisodium citrate by adopting a displacement reaction method, washing powder for three times by using distilled water, and drying at 40 ℃ to obtain a nano Cu@Ag core-shell material;
and (3) preparing an In-Cu@Ag solder preform: and (3) preparing the In foil or the micron In particles and the nano Cu@Ag core-shell material obtained In the step (2) by a pressurizing or heating pressurizing mode to form an In-Cu@Ag solder preform.
2. The method for preparing the In-cu@ag solder preform according to claim 1, wherein In step (1), the soluble copper salt comprises any one of copper sulfate and copper acetate monohydrate, and the reducing agent comprises any one of hydrazine hydrate, ascorbic acid, sodium borohydride and formaldehyde.
3. The method for producing an In-cu@ag solder preform as In claim 1 wherein In step (2) said ethylene glycol is added In an amount of 100ml, said nano Cu particles are added In an amount of 0.08mol, and said trisodium citrate is added In an amount of 0.016mol.
4. The method for preparing an In-cu@ag solder preform as In claim 1 wherein the molar ratio of said silver nitrate solution to said nano Cu particles to said trisodium citrate In step (2) is 1: 5-8: 1.
5. the method for preparing an In-Cu@Ag solder preform according to claim 1, wherein the reaction temperature of the substitution reaction method In the step (2) is 25-90 ℃ and the reaction time is 20-60 min.
6. The method for producing an In-cu@ag solder preform according to claim 1, wherein In step (3), the production of the In-cu@ag solder preform comprises the steps of: arranging the nano Cu@Ag core-shell particles and In foil prepared In the step (2) In a die according to the sequence of In foil-nano Cu@Ag core-shell particles-In foil, wherein the thickness of the In foil is 25-50 mu m, the addition amount of the nano Cu@Ag core-shell particles is 0.08-0.16 mol, heating to 150 ℃, and applying a pressure of 10-40 MPa for 5-10 min to obtain an In-Cu@Ag solder preform.
7. The method for producing an In-cu@ag solder preform according to claim 1, wherein In step (3), the production of the In-cu@ag solder preform comprises the steps of: firstly, placing the nano Cu@Ag core-shell material prepared In the step (2) into a die, heating to 150 ℃ for presintering to form a prefabricated sheet framework, reducing the porosity of the prefabricated sheet framework to 10% -20% by using a roll press, preparing In into soldering paste, printing on the prefabricated sheet framework by using screen printing single face, wherein the In content In the soldering paste is 75% -90% of the mass of the soldering paste, adopting In powder with the size of 200-300 meshes, heating to 160 ℃ for 5-10 min, and cooling to obtain the In-Cu@Ag solder prefabricated sheet.
8. The method for producing an In-cu@ag solder preform according to claim 1, wherein the production of the In-cu@ag solder preform In step (3) comprises the steps of: mixing the nano Cu@Ag core-shell material prepared In the step (2) with micron In particles, wherein the size of the micron In particles is 1-5 mu m, and the mass ratio of the prepared nano Cu@Ag core-shell material to the micron In particles is 20-25: and 1, placing the solder In a die, applying a pressure of 20-40 MPa, and maintaining the pressure for 5-10 min to obtain the In-Cu@Ag solder pre-manufactured sheet.
9. An In-cu@ag solder preform, characterized by being prepared by the preparation method of any one of claims 1 to 8.
CN202310045341.XA 2023-01-30 2023-01-30 In-Cu@Ag solder pre-prepared sheet and preparation method thereof Pending CN116079277A (en)

Priority Applications (1)

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CN202310045341.XA CN116079277A (en) 2023-01-30 2023-01-30 In-Cu@Ag solder pre-prepared sheet and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202310045341.XA CN116079277A (en) 2023-01-30 2023-01-30 In-Cu@Ag solder pre-prepared sheet and preparation method thereof

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Publication Number Publication Date
CN116079277A true CN116079277A (en) 2023-05-09

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Country Status (1)

Country Link
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