CN106853537A - A kind of preparation method of copper nano particles interconnection material - Google Patents
A kind of preparation method of copper nano particles interconnection material Download PDFInfo
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- CN106853537A CN106853537A CN201611158551.6A CN201611158551A CN106853537A CN 106853537 A CN106853537 A CN 106853537A CN 201611158551 A CN201611158551 A CN 201611158551A CN 106853537 A CN106853537 A CN 106853537A
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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
- 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
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- 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
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/102—Metallic powder coated with organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The present invention relates to a kind of copper nano particles interconnection material and preparation method thereof, the method belongs to nano metal material field using the synthetic method of liquid-phase reduction.The present invention is to mix cupric salt, reducing agent sodium hypophosphite, macromolecule stabilizer polyvinyl alcohol and deionized water by different mass percents；Then the copper salt solution is heated to 70 DEG C 90 DEG C, is incubated 90 150 minutes and obtains the dispersion liquid that polyvinyl alcohol coats copper nano particles；The copper nano particles dispersion liquid is carried out into multiple centrifugation with deionized water and is washed, preserved and be mutually used in conjunction copper nano particles dispersion liquid into deionized water or ethanol；Finally copper nano particles dispersion liquid is concentrated, is coated between copper sheet, be placed in batch-type furnace and heat connection copper base.The features such as advantage of the method is low cost, preparation method environmental protection, raw material are cheap and easy to get, is adapted to large-scale industrial production, and the polyvinyl alcohol prepared coats copper nano particles between 200nm 500nm, can be used for preparation and is mutually used in conjunction nano material.
Description
Technical field
The present invention relates to a kind of preparation method of copper nano particles interconnection material, the method uses the synthesis side of liquid-phase reduction
Method, belongs to nano metal material field.The present invention is first to gather cupric salt, reducing agent sodium hypophosphite, macromolecule stabilizer
Vinyl alcohol and deionized water are mixed by different mass percents；Secondly the copper salt solution is heated to 70 DEG C -90 DEG C, insulation
Obtain the dispersion liquid that polyvinyl alcohol coats copper nano particles within 90-150 minutes；Then by the copper nano particles dispersion liquid deionization
Water carries out multiple centrifugation and washs, and preserves and is mutually used in conjunction copper nano particles dispersion liquid into deionized water or ethanol；Most
Copper nano particles dispersion liquid is concentrated afterwards, is coated between two pieces of copper sheets, be placed in batch-type furnace and heat connection copper base.The party
The features such as advantage of method is low cost, preparation method environmental protection, raw material are cheap and easy to get, is adapted to large-scale industrialization life
Produce, the polyvinyl alcohol prepared coats copper nano particles between 200nm-500nm, can be used for preparation and be mutually used in conjunction nano metal material
Material.
Background technology
In recent years, microelectronics system develops to directions such as high power, High Density Integration, miniaturization and multifunctions, right
Electronic package interconnections material proposes requirement higher at the aspect such as performance and heat management, such as disposably realizes that high temperature resistant is interconnected
(being more than 200 DEG C) or multi-level packaging need prime interconnection to have law temperature joining and high-temperature stability etc. concurrently.Meet these requirements
Interconnection material can apply in large power semiconductor LED, high temperature wide bandgap semiconductor (SiC, GaN etc.) and vapour
The fields such as car engine power electronic device.Noble silver and the alloy material (about 280 DEG C of fusing point) with 80Au-20Sn as representative
It is the more typical high temperature resistant interconnection material of two analogies.On the one hand, silver is conductive by force, thermal conductivity is big, fusing point is high and comprehensive
The advantages of excellent in mechanical performance, it is widely used to microelectronic；On the other hand, the alloy material such as 80Au-20Sn has and leads
Heat and conduct electricity very well, anticorrosive, creep resistant the advantages of, in the welding of high power semiconductor lasers chip and ceramics absolutely at present
The photoelectric fields such as edge Metal Packaging have been obtained for being widely applied.But the price of both materials is all costly, and
And deelectric transferred ability of the silver in wet environment is weaker, can cause to cause short circuit.With bismuthino, auri, lead base, zinc-base etc.
Although the alloy material and ag material to represent can meet the resistant to elevated temperatures performance of electronic device, due to alloy material
Fusion temperature is too high, suitable for application in the occasion for needing law temperature joining electronic device.In addition, unleaded is also Electronic Packaging
Inexorable trend.In order to overcome above mentioned problem, proposition prepares silver nano material, is driven by the sintering of the nanosizing reduction silver of silver
Power, thus reduces the sintering temperature of silver.In view of the cost factor that silver nano material makes, silver nanoparticle interconnection material is limited
Development.Therefore, it is badly in need of finding the substitute of silver nano material.There is good ductility due to copper nano material, excellent lead
Electrical conductivity, and the performance such as deelectric transferred ability is stronger than silver nano material.Therefore, in order to reduce the cost of interconnection material, carry
Go out and replace silver nanoparticle interconnection material using the copper nano particles of inexpensive and high conductivity.
At present, synthesis copper nano material method mainly have Radiation Synthesis Method, mechanical milling method, plasma sputtering,
Template, microemulsion method, hydro-thermal method and solution phase chemical reduction etc..The physical method in these preparation methods, such as plasma
Body is sputtered, and required equipment is general all costly, and obtained copper nano particles particle diameter is larger and distributing inhomogeneity, and surface lacks bag
Cover material, therefore easily oxidation.Liquid phase reduction in chemical preparation process due to do not need special container, it is easy to operate,
The features such as process is easy to control and can realize batch production, thus it is of greatest concern.It is that one kind uses reducing agent, by solution
The bivalent cupric ion method that is restored to zeroth order.The reaction system reported at present mainly has：Boron hydrogen is used in water solution system
Change the reducing metal salt presomas (copper nitrate, copper sulphate, copper chloride etc.), mating surface such as sodium, potassium borohydride or L-AA
Stabilizer prevents copper nano particles from aoxidizing, such as water-copper sulphate-sodium borohydride-lauryl sodium sulfate, water-copper chloride-hydrazine hydrate
(N2H4·H2O)-cetyl trimethylammonium bromide, water-copper nitrate-L-AA-polyvinylpyrrolidone, water-nitric acid
Copper-sodium borohydride-polyvinyl alcohol etc.；With 1,2- dihydroxy hexadecane, L-AA or hypophosphorous acid in organic solvent system
The reducing metal salt such as sodium presoma (copper sulphate, copper acetate, copper chloride, Kocide SD etc.), mating surface stabilizer prevents copper from receiving
Rice grain is aoxidized, such as ethylene glycol-copper sulphate-L-AA-polyvinylpyrrolidone, diethylene glycol-copper sulphate-hypophosphorous acid
Sodium-polyvinylpyrrolidone, octyl ether-copper sulphate -1,2- dihydroxy hexadecane-polyvinylpyrrolidone, ethylene glycol-hydroxide
Copper-L-AA-polyethylene glycol etc..Copper nano material based on above method acquisition is mainly for the preparation of Nanometer Copper conductive paste
In material and inkjet printing nano-copper conductive ink, and the copper nano particles system in low-temperature sintering interconnection applications only includes
Copper sulphate, copper acetate, copper chloride etc. are reduced with sodium hypophosphite in organic multicomponent alcohol solvent system, and uses polyvinylpyrrolidone bag
Covering prevents copper nano particles surface oxidation；With hydrazine hydrate reduction copper chloride, copper nitrate, copper acetate etc. in water solution system, it is used in combination
Cetyl trimethylammonium bromide cladding prevents copper nano particles surface oxidation.But, due to the organic solvent in synthetic system
It is general with reducing agent all poisonous, influence environment and human health, and also the use of organic solvent can increase the life of copper nano particles
Produce cost.Therefore the use of these reaction systems receives certain limitation.
The content of the invention
The new side that polyvinyl alcohol (PVA) coats copper nano particles interconnection material is prepared it is an object of the invention to provide one kind
Method, obtains a kind of polyvinyl alcohol cladding copper nano particles for being suitably applied in interconnection field.Polyvinyl alcohol coats copper nano particles
Preparation using liquid-phase reduction method.First by cupric salt, reducing agent, macromolecule stabilizer and deionized water by different
Mass percent mixes；Secondly the cupric salt deionized water solution is heated to 70 DEG C -90 DEG C, is incubated 90-150 minutes and obtains
The dispersion liquid of polymeric PTC materials copper nano particles；Then the copper nano particles dispersion liquid is carried out into repeatedly centrifugation point with deionized water
From and wash, remove unnecessary macromolecule stabilizer, be stored in certain density deionized water or ethanol solution, interconnected
Use copper nano particles dispersion liquid；The copper nano particles ultrasonic mixing in ethanol or deionized water is finally placed on, vacuum baking is placed in
Case is concentrated, and is evenly coated between the copper sheet by polishing, and heating and thermal insulation can connection copper base in batch-type furnace.In liquid phase
It is, in order to realize the environmental protection of copper nano particles preparation method, to realize honest and clean for the purpose of deionized water that solvent is used in reducing process
The large-scale industrial production method of valency.
The cupric salt used in the method that polyvinyl alcohol cladding copper nano particles are prepared using liquid phase reduction is three
One kind in water copper nitrate, five water copper nitrates, cupric sulfate pentahydrate, copper chloride dihydrate, macromolecule stabilizer for it is water-soluble preferably and
Nontoxic 1788 types or 1799 type polyvinyl alcohol, reducing agent uses sodium hypophosphite.
Liquid phase reduction prepares the mutual specific preparation process for being used in conjunction polyvinyl alcohol cladding copper nano particles：
(1), a certain amount of deionized water is added in three-neck flask, 70 DEG C -90 DEG C (notes is then heated in oil bath
It is solution 1)；
(2) a certain amount of sodium hypophosphite and 1788 type polyvinyl alcohol are added in solution 1 respectively, stirring is to complete
Dissolving；
(3) certain density nitrate trihydrate copper, five water copper nitrates, five water sulfuric acid, are configured in another three-neck flask
The divalence copper solution such as copper, copper chloride dihydrate, solvent is deionized water, then in oil bath heating stirring to 70 DEG C of -90 DEG C of (solution
It is designated as solution 2)；
(4), solution 2 is poured into solution 1, is reacted about 90-150 minutes, solution colour becomes brown by blueness, from oil bath
In directly remove flask, be cooled to 25 DEG C；
(5), the solution centrifugal for reacting gained, 9000 turns of rotating speed, the time of centrifugation is 5-30 minutes；
(6) add deionized water to be cleaned by ultrasonic after, supernatant liquor is poured out 5-10 minutes, be repeated twice；
(7), be placed on copper nano particles ultrasonic mixing 30-90 minutes in ethanol or deionized water, be subsequently placed in 25 DEG C-
60 DEG C of vacuum drying oven is concentrated 30-90 minutes, obtains being applied to the copper nano particles dispersion liquid of electronic interconnection.
The present invention has an advantageous effect in that compared with background technology：
The present invention is by bivalent cupric ion precursor nitrate trihydrate copper, five water copper nitrates, cupric sulfate pentahydrate, copper chloride dihydrate
One kind, partial hydrolysis or all the non-toxic polyethylene alcohol of hydrolysis, deionized water and reducing agent sodium hypophosphite fill in the liquid phase
Divide uniform mixing, be heated to uniform temperature, and be incubated the regular hour, the copper that polyvinyl alcohol is coated is obtained after there is electronation
Nano particle.The solvent that the method is used is deionized water, it is possible to achieve the environmental protection of preparation method, realizes cheap big rule
The industrialized preparing process of mould.Have certain than the PVP commonly used using polyvinyl alcohol as macromolecule stabilizer
Advantage, polyvinyl alcohol can discharge acetic acid in being mainly reflected in heating connection procedure, can delay the oxidation of copper nano particles.Base
In above-mentioned analysis, the polyvinyl alcohol cladding copper nano particles that the method is obtained are dispersed in deionized water or ethanol solution, so
The copper sheet surface by polishing is coated in afterwards, directly in air ambient low temperature sintering can obtain the connection effect of better performances.
Brief description of the drawings
Fig. 1 is that the ESEM of the 1788 type polyvinyl alcohol cladding copper nano particles interconnection material of the embodiment of the present invention 1 is surveyed
Test result.
Fig. 2 is that the Fourier of the 1788 type polyvinyl alcohol cladding copper nano particles interconnection material according to the gained of embodiment 1 is red
Outer test result.
Fig. 3 is the tensile strength that copper nano particles interconnection material is coated according to 1788 type polyvinyl alcohol of the gained of embodiment 1
Test result.
Specific embodiment
The invention will be further described with reference to the accompanying drawings and examples.
Embodiment 1：
Deionized water 40ml is measured first, is added in three-neck flask, it is heated to 70 DEG C in oil bath, be separately added into
4 grams of sodium hypophosphites and 2.5 gram of 1788 type polyvinyl alcohol, stir 1 hour to whole dissolvings；Secondly in another three-neck flask
The nitrate trihydrate copper deionized water solution of 1M is configured, 70 DEG C are heated to；Then the nitrate trihydrate copper deionized water solution of 1M is added
Enter in sodium hypophosphite and 1788 type polyethylene deionized water solutions, stirring to well mixed, reaction 90 minutes at 70 DEG C, directly
Removal three-neck flask is connect, 25 DEG C are cooled to；Finally solution is cleaned with deionized water, centrifugal rotational speed is 9000 turns, centrifugation time
It is 8 minutes, the copper nano particles that will be obtained are placed in deionized water or ethanol and preserve, obtains being applied to the copper nanometer of electronic interconnection
Particle dispersion.Above-mentioned sodium hypophosphite, 1788 type polyvinyl alcohol and nitrate trihydrate copper are all from Aladdin Reagent Company, not
Through being further purified.
Connection copper sheet step is as follows：40 points of copper nano particles ultrasonic mixing in ethanol or deionized water is placed on first
Clock, the vacuum drying oven for being subsequently placed in 40 DEG C is concentrated 30 minutes, is evenly coated between the copper sheet by polishing；Finally by copper sheet
It is placed in batch-type furnace, 300 DEG C are incubated 1 hour, and programming rate is 10 DEG C per minute, are sintered under air ambient, naturally cool to 25
℃。
The ESEM of the polyvinyl alcohol cladding copper nano particles in embodiment 1 is as shown in Figure 1.Sample in embodiment 1
Fourier's infrared test result is as shown in Figure 2.Using in example 1 copper nano particles implement interconnection, its result as shown in figure 3,
Tensile strength can reach 0.8MPa.
Can be seen that polyvinyl alcohol coats the diameter about 200nm- of copper nano particles from the ESEM result in Fig. 1
Between 500nm, granular size is relatively uniform, and distribution more disperses, and the shape difference of each particle is smaller, mostly spherical.Fig. 2
In Fourier's infrared test result illustrate in position 3443cm-1Place is-OH group stretching vibrations, position 1630cm-1Place is C
=C stretching vibrations, position 1072cm-1Place is PVA skeleton C-O stretching vibrations, position 628cm-1Place is-OH group stretching vibrations,
It is possible thereby to judge that copper nano particles outside is coated with polyvinyl alcohol.
Embodiment 2：
Method according to embodiment 1 prepares polyvinyl alcohol cladding copper nano particles, and difference is：The time lengthening of reaction is extremely
150 minutes.The copper nano particles ultrasonic mixing 40 minutes in ethanol or deionized water is finally placed on, 40 DEG C true is subsequently placed in
Empty baking oven is concentrated 30 minutes, obtains being applied to the copper nano particles dispersion liquid of electronic interconnection.Tensile strength can reach 0.7MPa.
Embodiment 3：
Method according to embodiment 1 prepares polyvinyl alcohol cladding copper nano particles, and difference is：The stabilizing polymer for using
Agent is 1799 type polyvinyl alcohol, and the aqueous temperature for dissolving 1799 type polyvinyl alcohol is 90 DEG C, the deionized water of cupric sulfate pentahydrate
Solution is heated to 90 DEG C.The copper nano particles ultrasonic mixing 40 minutes in ethanol or deionized water is finally placed on, is subsequently placed in
40 DEG C of vacuum drying oven is concentrated 30 minutes, obtains being applied to the copper nano particles dispersion liquid of electronic interconnection.Tensile strength can reach
To 0.75MPa.
Embodiment 4：
Method according to embodiment 1 prepares polyvinyl alcohol cladding copper nano particles, and difference is：The mantoquita for using is five water
Copper sulphate.The copper nano particles ultrasonic mixing in ethanol or deionized water is finally placed on, 40 DEG C of vacuum drying oven is subsequently placed in
Concentration 30 minutes, obtains being applied to the copper nano particles dispersion liquid of electronic interconnection.Tensile strength can reach 0.78MPa.
Claims (7)
1. a kind of preparation method of copper nano particles interconnection material, it is characterised in that comprise the following steps：
(1) liquid-phase reduction method is used, reducing agent and macromolecule stabilizer is dissolved in a certain amount of solvent, be sufficiently mixed uniform
Afterwards, solution system is heated to certain temperature, is then added in the solution containing reducing agent and macromolecule stabilizer identical
The cupric salt solution of temperature, insulation reaction for a period of time after, by reacted solution centrifugal separate and repeatedly deionization washing
Wash；
(2) copper nano particles obtained in step (1) are preserved in a liquid, obtains the copper nano particles dispersion liquid being mutually used in conjunction；
(3) liquid in step (2) is carried out into ultrasonic mixing, be subsequently placed in vacuum drying oven concentration, then be evenly coated in by
Between the copper sheet of polishing, heating and thermal insulation is that can be used to connect copper base in batch-type furnace.
2. the preparation method of a kind of copper nano particles interconnection material according to claim 1, it is characterised in that：The step
(1) solvent in uses deionized water, and reducing agent is sodium hypophosphite, and macromolecule stabilizer is 1788 types, 1799 type polyvinyl alcohol
In one kind.
3. the preparation method of a kind of copper nano particles interconnection material according to claim 1, it is characterised in that：The step
(1) cupric salt in is the one kind in nitrate trihydrate copper, five water copper nitrates, cupric sulfate pentahydrate or copper chloride dihydrate.
4. the preparation method of a kind of copper nano particles interconnection material according to claim 1, it is characterised in that：The step
(1) reaction temperature of system is in 70 DEG C -90 DEG C, soaking time is 90-150 minutes in.
5. the preparation method of a kind of copper nano particles interconnection material according to claim 1, it is characterised in that：The step
(2) copper nano particles are placed in ethanol or deionized water after centrifuge washing and preserve.
6. the preparation method of a kind of copper nano particles interconnection material according to claim 1, it is characterised in that：The step
(3) vacuum drying oven thickening temperature is 25 DEG C -60 DEG C in, and concentration time is 30-90 minutes.
7. the preparation method of a kind of copper nano particles interconnection material according to claim 1, it is characterised in that：The step
(3) Technology for Heating Processing in batch-type furnace is 300 DEG C and is incubated 1 hour, and programming rate is 10 DEG C per minute, is burnt under air ambient
Knot, naturally cools to 25 DEG C.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108098191A (en) * | 2017-12-17 | 2018-06-01 | 华中科技大学 | A kind of preparation method of copper nano particles soldering paste and products thereof |
| CN109483092A (en) * | 2018-12-12 | 2019-03-19 | 中国矿业大学 | A kind of preparation method of the high switching performance welding material of high heat-conductivity conducting based on copper nano particles |
| CN110037058A (en) * | 2019-04-04 | 2019-07-23 | 金华市飞凌生物科技有限公司 | Cause the compound of insect muscle cramp |
| CN110369911A (en) * | 2019-06-27 | 2019-10-25 | 上海三一重机股份有限公司 | A kind of copper nano-weld material and preparation method thereof |
| CN112399896A (en) * | 2018-06-26 | 2021-02-23 | 阿尔法装配解决方案公司 | Nanocopper pastes and films for sintered die attach and similar applications |
| CN114516654A (en) * | 2022-02-09 | 2022-05-20 | 广州科城环保科技有限公司 | Preparation method of modified copper hydroxide and modified copper hydroxide prepared by same |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108098191A (en) * | 2017-12-17 | 2018-06-01 | 华中科技大学 | A kind of preparation method of copper nano particles soldering paste and products thereof |
| CN112399896A (en) * | 2018-06-26 | 2021-02-23 | 阿尔法装配解决方案公司 | Nanocopper pastes and films for sintered die attach and similar applications |
| CN109483092A (en) * | 2018-12-12 | 2019-03-19 | 中国矿业大学 | A kind of preparation method of the high switching performance welding material of high heat-conductivity conducting based on copper nano particles |
| CN110037058A (en) * | 2019-04-04 | 2019-07-23 | 金华市飞凌生物科技有限公司 | Cause the compound of insect muscle cramp |
| CN110369911A (en) * | 2019-06-27 | 2019-10-25 | 上海三一重机股份有限公司 | A kind of copper nano-weld material and preparation method thereof |
| CN114516654A (en) * | 2022-02-09 | 2022-05-20 | 广州科城环保科技有限公司 | Preparation method of modified copper hydroxide and modified copper hydroxide prepared by same |
| CN114516654B (en) * | 2022-02-09 | 2024-02-27 | 广州科城环保科技有限公司 | Preparation method of modified copper hydroxide and modified copper hydroxide prepared by preparation method |
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