CN115194145A - Preparation method of micron particle interconnection material with Cu @ in core-shell structure - Google Patents
Preparation method of micron particle interconnection material with Cu @ in core-shell structure Download PDFInfo
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- 239000002245 particle Substances 0.000 title claims abstract description 34
- 239000000463 material Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000007747 plating Methods 0.000 claims abstract description 44
- 239000010949 copper Substances 0.000 claims abstract description 26
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- 238000000034 method Methods 0.000 claims abstract description 15
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- 229910052802 copper Inorganic materials 0.000 claims abstract description 13
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- 229910052751 metal Inorganic materials 0.000 claims abstract description 11
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- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims description 13
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N 1,4-Benzenediol Natural products OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 8
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims description 6
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims description 6
- 229910000337 indium(III) sulfate Inorganic materials 0.000 claims description 3
- XGCKLPDYTQRDTR-UHFFFAOYSA-H indium(iii) sulfate Chemical compound [In+3].[In+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O XGCKLPDYTQRDTR-UHFFFAOYSA-H 0.000 claims description 3
- AJAXZLXLXZWIIE-UHFFFAOYSA-N indium;hydrochloride Chemical compound Cl.[In] AJAXZLXLXZWIIE-UHFFFAOYSA-N 0.000 claims description 3
- 239000002243 precursor Substances 0.000 claims description 3
- XURCIPRUUASYLR-UHFFFAOYSA-N Omeprazole sulfide Chemical compound N=1C2=CC(OC)=CC=C2NC=1SCC1=NC=C(C)C(OC)=C1C XURCIPRUUASYLR-UHFFFAOYSA-N 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 125000000687 hydroquinonyl group Chemical group C1(O)=C(C=C(O)C=C1)* 0.000 claims description 2
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical group OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims 3
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- 238000007254 oxidation reaction Methods 0.000 abstract description 5
- 239000010410 layer Substances 0.000 description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
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- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
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- 238000007772 electroless plating Methods 0.000 description 1
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- 229910052738 indium Inorganic materials 0.000 description 1
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- 230000001052 transient effect Effects 0.000 description 1
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- 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
- 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
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/52—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating using reducing agents for coating with metallic material not provided for in a single one of groups C23C18/32 - C23C18/50
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
- H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
- H01L21/768—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics
- H01L21/76838—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the conductors
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a preparation method of a micron particle interconnection material with a Cu @ in core-shell structure, which comprises the following steps: step one, preparing an alkaline plating solution containing a complexing agent, indium salt and an antioxidant at room temperature, and reacting the complexing agent and the indium salt In the alkaline plating solution to generate complex In 3+ To prevent In 3+ Direct precipitation of (2); step two, complexing In by using sodium borohydride as a reducing agent 3+ Reducing the In into a simple substance, and chemically plating In on a micron Cu ball; and step three, pouring the waste liquid obtained in the step two, alternately ultrasonically cleaning the plating powder by using absolute ethyl alcohol and distilled water, finally cleaning the plating powder by using the absolute ethyl alcohol, and then air-cooling, drying and sieving to obtain the Cu @ in core-shell structure metal powder.The micron particle interconnection material with the Cu @ in core-shell structure prepared by the method improves the oxidation resistance and stability of micron copper, and greatly reduces interconnection temperature and interconnection conditions on the premise of ensuring the conductivity of the interconnection material.
Description
Technical Field
The invention belongs to the technical field of electronic packaging micro-interconnection, and relates to a preparation method of a core-shell structure micron particle connecting material for low-temperature connection and high-temperature service.
Background
In recent years, microelectronic systems are developing towards high power, high density integration, miniaturization, multi-functionalization and the like, and higher requirements are put forward on electronic packaging interconnection materials in the aspects of performance, thermal management and the like, for example, when high temperature interconnection resistance (more than 200 ℃) is realized or multi-level packaging requires that front-level interconnection has low temperature connection, high temperature resistance and the like, and high interconnection temperature has great negative influence on the reliability of microelectronic products.
Currently, the interconnect materials used in the field of microelectronic packaging are mainly alloy solder paste and conductive paste. However, the solder paste has many problems, such as short circuit caused by tin whisker phenomenon, fracture failure of the bonding pad caused by generation of intermetallic compounds, poor shock and impact resistance, and the like. In addition, the reflow temperature of the solder paste is high, and the solder paste cannot be used in some high-temperature sensitive products. The curing temperature of the conductive heat-conducting adhesive is generally lower (less than 150 ℃), which can effectively avoid the influence of high temperature on the chip in the interconnection process, but the resin matrix of the conductive heat-conducting adhesive is not high-temperature resistant, which easily causes the problems of narrower working temperature range, lower conductive heat-conducting performance, cracking and falling off of the chip caused by the thermal fatigue effect generated by devices, and the like. Therefore, it is urgent for the electronic industry to find an interconnection material with low cost and reliable quality.
Today, nano-metal materials are the hot research point because of their good electrical and thermal conductivity and ability to be sintered at lower temperatures, wherein nano-copper is a very potential microelectronic package interconnection material. The nano copper has high electric and thermal conductivity, lower interconnection welding temperature and lower cost, but the nano copper has the defect of easy oxidation, particularly conductive copper paste which needs to be sintered at low temperature, and the oxidation of the copper can cause the increase of the melting point and the failure of sintering.
Disclosure of Invention
Aiming at the problems of the existing electronic packaging nano soldering paste interconnection material, the invention provides a preparation method of a micron particle interconnection material with a Cu @ in core-shell structure. The micron particle interconnection material with the Cu @ in core-shell structure prepared by the method improves the oxidation resistance and stability of micron copper, and greatly reduces interconnection temperature and interconnection conditions on the premise of ensuring the conductivity of the interconnection material.
The purpose of the invention is realized by the following technical scheme:
a preparation method of micron particle interconnection material with Cu @ in core-shell structure realizes the preparation of Cu @ in core-shell structure metal powder by a chemical plating method, and comprises the following steps:
step one, preparation of precursor solution
Preparing alkaline plating solution containing complexing agent, indium salt and antioxidant at room temperature, and reacting the complexing agent with the indium salt In the alkaline plating solution to generate complex In 3+ To prevent In 3+ Wherein:
the preparation of the precursor solution is subdivided into four steps of indium salt dissolution, complexing agent use, pH adjustment and antioxidant addition;
the indium salt is one of indium sulfate, indium hydrochloride and indium nitrate;
the complexing agent is disodium ethylene diamine tetraacetate and/or triethanolamine and In 3+ When the complexing agent is a compound complexing agent of disodium ethylene diamine tetraacetate (EDTA-2 Na) and Triethanolamine (TEA), the concentration of EDTA-2Na In the alkaline plating solution is In 3+ 2~3 times the concentration of TEA In 3+ The concentration of EDTA-2Na In the alkaline plating solution is 2.5 to 3.5 times of the concentration of the sodium EDTA-2Na In the alkaline plating solution 3+ 2.3 times the concentration and TEA In 3+ The plating effect is optimal when the concentration is 3 times; when the complexing agent is disodium ethylene diamine tetraacetate, the concentration of EDTA-2Na In the alkaline plating solution is In 3+ Of a concentration4~6 times; when the complexing agent is triethanolamine, TEA concentration In the alkaline plating solution is In 3+ 4~6 times the concentration;
the pH value of the alkaline plating solution is 8.0 to 11.0;
the antioxidant is hydroquinone, and the concentration of the antioxidant in the alkaline plating solution is 0.1 to 1mg/L;
step two, chemically plating In
Complexing In by using sodium borohydride as reducing agent 3+ Reducing the solution into an In simple substance, and performing chemical plating of In on a micron Cu ball, wherein:
the size of the micron Cu ball is 10 to 100 mu m;
the pH value of the electroless plating In is 8.0 to 11.0;
the temperature of chemical plating In is 60 to 90 ℃;
sodium borohydride In concentration 3+ The concentration is 3.5 to 4 times, the adding method is divided adding, and the adding times are 3~5;
step three, obtaining Cu @ In core-shell structure powder
And D, pouring the waste liquid in the step II, alternately ultrasonically cleaning the plating powder by using absolute ethyl alcohol and distilled water, finally cleaning by using the absolute ethyl alcohol, air-cooling, drying and sieving to obtain the Cu @ in core-shell structure metal powder, wherein:
in the Cu @ in core-shell structure metal powder, the size of a micron copper particle is 10 to 100 mu m, and the thickness of a metal shell layer is 1 to 20 mu m.
The micron-sized Cu @ in core-shell structure bimetallic powder prepared by the invention has the following characteristics: the In plating layer on the surface can be melted and connected with adjacent Cu nuclei when reflowing at low temperature, and the sufficient Cu atom source and the higher surface activity of the particles ensure that the In layer reflows for a short time to generate a Cu-In intermetallic compound with higher melting point. The invention realizes the purpose that the welding spot obtained after low-temperature short-time reflow has higher melting point by means of Cu-In phase change.
Compared with the prior art, the invention has the following advantages:
1. the melting point of In the Cu @ In core-shell structure high-temperature solder is only 156.6 ℃, so that connection can be carried out at a lower reflow temperature. When the In layer is completely exhausted and intermetallic compounds are generated, the service temperature of the In layer is increased. Therefore, low-temperature connection and high-temperature service can be realized.
The contact area of In and Cu In the Cu @ In core-shell material is large, so that the material is compared with the traditional material
Transient Liquid Phase (TLP) ligation allows for faster reaction rates.
2. The In can react with Cu to generate intermetallic compounds, so that the porosity can be reduced, the cost of raw materials can be greatly reduced, and great advantages are brought into play In industrialized mass production.
3. Since the inner Cu nuclei remain after the reaction is completed. Compared with a traditional full Intermetallic Compound (IMC) welding seam, the Cu core can better absorb external stress, so that local stress concentration is relieved, and the shearing resistance of the welding seam is improved. Moreover, as Cu has good electric and heat conductivity, the electric and heat conductivity of the finally formed welding line is greatly improved compared with that of the traditional full IMC welding line.
4. The shell prepared by the invention has compact metal form and uniform and controllable size, is easy to generate atomic diffusion at a lower temperature, is connected with the micron copper particles to form a three-dimensional interconnection system, not only improves the oxidation resistance and stability of the micron copper particles of the core layer, but also greatly reduces the interconnection temperature and interconnection conditions.
5. The micron particle interconnection material with the Cu @ in core-shell structure, prepared by the invention, can interconnect the chip and the substrate under the condition of low temperature and no pressure to complete the connection and packaging of the semiconductor device, and can be better applied to the fields of manufacturing of the semiconductor device, microelectronic packaging, power electronic packaging and the like.
Drawings
FIG. 1 is a schematic view of a micron metal structure of a Cu @ in core-shell structure of the present invention;
FIG. 2 is a Cu @ in core-shell structure solder paste integral interconnection device fabrication process.
Detailed Description
The technical solutions of the present invention are further described below with reference to the embodiments, but the present invention is not limited thereto, and any modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Example 1:
this example provides a method for preparing a core-shell structure of a microparticle interconnect material, in which EDTA-2Na and TEA are used as a complex complexing agent and In is In an alkaline plating solution 3+ Reaction to form complexed In 3+ Prevention of In 3+ Direct precipitation of (2). Then performing chemical plating of In on micron-sized Cu spheres, and complexing the In by using sodium borohydride as a reducing agent 3+ Reducing the In into a simple substance, depositing on a micron Cu ball, and finally obtaining Cu @ In double-layer core-shell structure powder. The specific implementation steps are as follows:
the method comprises the following steps: sequentially soaking Cu powder with the diameter of 10 mu m in acetone, 15% diluted hydrochloric acid and deionized water to remove organic matters and oxide layers on the surfaces of particles;
step two: weighing 1.51 g indium sulfate powder, placing the powder in a 100ml beaker, adding concentrated sulfuric acid to 4.5 g, adding distilled water to 20 ml, preparing a solution A, and placing the solution in an ultrasonic cleaner to vibrate until the solution is clear;
step three: weighing 2.0 g disodium ethylene diamine tetraacetate powder, placing the powder in a 100ml beaker, adding distilled water to 20 ml to prepare solution B, and placing the solution B in an ultrasonic cleaning machine to shake until the solution is clear;
step four: weighing 2.17 g triethanolamine and placing the triethanolamine in a 100ml beaker, adding distilled water to 10 ml, shaking and shaking the beaker to dissolve and clarify the triethanolamine;
step five: weighing 4.0 g sodium hydroxide particles, placing the sodium hydroxide particles in a 100ml beaker, adding distilled water to 20 ml, and placing the beaker in an ultrasonic cleaning machine to vibrate until the solution is clear;
step six: weighing 0.04 g hydroquinone particles, placing the particles in a 100ml beaker, adding distilled water to 10 ml, shaking and vibrating the beaker to dissolve and clarify the hydroquinone particles;
step seven: pouring the solution B into the solution A, adding a triethanolamine solution after uniformly stirring by using a glass rod, then dropwise adding a sodium hydroxide solution to the solution A by times and carefully till the pH value is about 9.0 (35.0 ℃), and uniformly stirring by using the glass rod after dropwise adding each time;
step eight: weighing 2.0 g sodium borohydride, placing the sodium borohydride in a 100ml beaker, adding distilled water to 20 ml, and standing by after all particles are dissolved;
step nine: pouring the solution obtained in the seventh step into a beaker filled with cleaned copper powder, pouring hydroquinone solution into the beaker, dripping about 6 ml sodium borohydride solution into a disposable dropper, putting the beaker into a magnetic stirrer for magnetic stirring, and putting the whole beaker into a heat collection type constant-temperature heating magnetic stirrer at 80 ℃ until the stirring speed is maximum;
step ten: dripping about 6 ml sodium borohydride solution into the solution every 10 min until the solution is used up, taking out the beaker after 10 min of dripping for the last time, standing for 1 min, and closing the heat-collecting constant-temperature heating magnetic stirrer;
step eleven: and pouring the waste liquid, alternately ultrasonically cleaning with absolute ethyl alcohol and distilled water to obtain plating powder, finally cleaning with absolute ethyl alcohol, air-cooling and drying after the cleaning, and removing agglomerated large particles by using a 250-mesh sieve to obtain the Cu @ In core-shell structure metal powder, wherein the thickness of the In plating layer is 18 microns.
The use method I comprises the following steps:
(1) Covering a chip on the surface of the micron particle interconnection material to obtain an integral device;
(2) And sintering the integral device to obtain the interconnection device, wherein the preparation process is as shown in figure 1.
The use method II comprises the following steps:
(1) Mixing the obtained Cu @ in particles and soldering flux according to a specific proportion and uniformly stirring to obtain Cu @ in solder paste;
(2) Fixing the components on the printed circuit board in a surface mounting mode by using solder paste;
(3) The welding of the components on the circuit board is realized through heating devices such as hot air backflow and the like.
Example 2:
this example differs from example 1 in that: in the first step, the size of the micron copper powder is changed to 30 μm, and the purpose of increasing the size of the copper powder is to obtain a thicker In plating layer, reduce the reflow temperature, and ensure that the thickness of the In plating layer is 20 μm.
Example 3:
this example differs from example 1 in that: and In the second step, indium hydrochloride powder is selected and dissolved by using dilute hydrochloric acid, and the thickness of the In plating layer is 16 microns.
Example 4:
this example differs from example 1 in that: using a single complexing agent EDTA-2Na, in 3+ The concentration of EDTA-2Na In the plating solution is In by reference 3+ The thickness of the In plating layer was 15 μm, which is 5 times the concentration.
Example 5:
this example differs from example 1 in that: use of a single complexing agent TEA, in 3+ The concentration of TEA In the plating solution was In with reference to the concentration 3+ The thickness of the In plating layer was 12 μm, which is 5 times the concentration.
Claims (10)
1. A preparation method of micron particle interconnection material with Cu @ in core-shell structure is characterized by comprising the following steps:
step one, preparation of precursor solution
Preparing alkaline plating solution containing complexing agent, indium salt and antioxidant at room temperature, and reacting the complexing agent with the indium salt In the alkaline plating solution to generate complex In 3+ To prevent In 3+ Direct precipitation of (2);
step two, chemically plating In
Complexing In by using sodium borohydride as reducing agent 3+ Reducing the In into a simple substance, and chemically plating In on a micron Cu ball;
step three, obtaining Cu @ In core-shell structure powder
And D, pouring the waste liquid obtained in the step two, alternately ultrasonically cleaning the plating powder by using absolute ethyl alcohol and distilled water, finally cleaning by using the absolute ethyl alcohol, and then air-cooling, drying and sieving to obtain the Cu @ in core-shell structure metal powder.
2. The method for preparing a micron particle interconnection material with a Cu @ in core-shell structure according to claim 1, wherein the indium salt is one of indium sulfate, indium hydrochloride and indium nitrate.
3. The method for preparing micron particle interconnection material with Cu @ In core-shell structure as claimed In claim 1, wherein the complexing agent is disodium ethylenediamine tetraacetate and/or triethanolamine, in 3+ When the concentration is used as reference, and the complexing agent is a compound complexing agent of ethylene diamine tetraacetic acid and triethanolamine, the concentration of EDTA-2Na In the alkaline plating solution is In 3+ 2~3 times the concentration, TEA In 3+ The concentration is 2.5 to 3.5 times; when the complexing agent is disodium ethylene diamine tetraacetate, the concentration of EDTA-2Na In the alkaline plating solution is In 3+ 4~6 times the concentration; when the complexing agent is triethanolamine, the concentration of TEA In the alkaline plating solution is In 3+ 4~6 times the concentration.
4. The preparation method of the micron particle interconnection material with the Cu @ in core-shell structure as claimed in claim 1, wherein the pH value of the alkaline plating solution is 8.0 to 11.0.
5. The preparation method of the micron particle interconnection material with the Cu @ in core-shell structure as claimed in claim 1, wherein the antioxidant is hydroquinone, and the concentration of the antioxidant in an alkaline plating solution is 0.1 to 1mg/L.
6. The preparation method of the micron particle interconnection material with the Cu @ in core-shell structure according to claim 1, wherein the size of the micron Cu ball is 10 to 100 μm.
7. The method for preparing a micron particle interconnection material with a Cu @ In core-shell structure according to claim 1, wherein the pH of the electroless In plating is 8.0 to 11.0.
8. The preparation method of the micron particle interconnection material with the Cu @ In core-shell structure according to claim 1, wherein the electroless In plating temperature is 60-90 ℃.
9. The method for preparing micron particle interconnection material with Cu @ In core-shell structure according to claim 1, wherein the concentration of sodium borohydride is In 3+ The concentration is 3.5 to 4 times, the adding method is divided into adding times, and the adding times are 3~5 times.
10. The preparation method of the micron particle interconnection material with the Cu @ in core-shell structure according to claim 1, wherein in the Cu @ in core-shell structure metal powder, the size of micron copper particles is 10 to 100 μm, and the thickness of a metal shell layer is 1 to 20 μm.
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