CN105921737B - The preparation method and conducting resinl of a kind of cuprum argentum composite powder - Google Patents
The preparation method and conducting resinl of a kind of cuprum argentum composite powder Download PDFInfo
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- B22—CASTING; POWDER METALLURGY
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
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- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
- C09J9/02—Electrically-conducting adhesives
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Abstract
The invention discloses a kind of preparation method of highly conductive anti-oxidant cuprum argentum composite powder, comprise the following steps：(1) cu-ag alloy powderses are prepared using gas atomization, silver-colored mass percent is 3%~14% in the cu-ag alloy powderses；(2) cu-ag alloy powderses prepared by step (1) are subjected to Ageing Treatment in vacuum or inert atmosphere and obtain cuprum argentum composite powder.The cu-ag alloy powderses that the present invention is prepared first with aerosolization are spherical, particle size range selectivity is big (1~120 μm), silver content is low, rich silver mutually preferentially separates out at the defects of crystal boundary and forms continuous space network structure after Ageing Treatment, be advantageous to the formation of silver-colored conductive network, enhance electric conductivity to a certain extent.Simultaneously as the silver-colored phase that defect (crystal boundary, hole, hole) etc. is precipitated in matrix is covered, effectively inhibit copper silver powder at relatively high temperatures in the crystal boundary the defects of position preferential oxidation, the initial oxidation temperature of matrix can be significantly improved.
Description
Technical field
The invention belongs to powder metallurgical technology, more particularly to a kind of system of highly conductive, oxidation resistant cuprum argentum composite powder
Preparation Method and conducting resinl.
Background technology
It is well known that silver, copper are two kinds of best metals of electric conductivity, it is the indispensable material of electronics industry.Due to
Silver has high electrical and thermal conductivity performance and chemical stability (antioxygenic property is good under high temperature), and silver powder exists as conductive filler
It is considered as the preferred material of used in electronic industry slurry in a very long time.However, silver is asked in the presence of what some were difficult to avoid that itself
Topic, easy the shortcomings of silver ion migration and high cost occurs such as under direct current electro ultrafiltration.Especially the transport phenomena of silver ion and lead
The short circuit problem of cause is marched toward miniaturization, highly integrated a great problem as electronic product.Relative to silver, copper has price
Cheaply, excellent electric conductivity, ability of resisting to migration are significantly larger than the series of advantages such as silver, are the preferred alternative materials of conductive silver powder.
But the problems such as being oxidized easily due to copper powder during preparation and military service, its electric conductivity are suppressed.How copper is being kept
Its antioxygenic property is improved on the basis of powder is highly conductive, be related to its can as conductive, shielding filler key technology it
One.China Patent Publication No. CN101294281A, disclose " a kind of preparation method of silver-plated copper powder for low-temperature slurry ", the product
Ag contents be generally higher than 30%, but have obvious oxidation at 200 DEG C or so, influence the military service stability of the copper-silver metal powder.
China Patent Publication No. CN101664803A discloses " preparation method of coated copper-silver metal powder ", and this method is based on public affairs
On the basis of the number of opening is CN101294281A Chinese patent, by adjusting the pH value of solution, ion sequestering agent can be optimal
In the range of play its masking activity, promote silver copper surface deposit.These prepare the method for cuprum argentum composite powder mainly with chemistry side
Based on method, it is relatively low copper argentum reagent utilization rate to be present in them, and process is various and the common problem such as a large amount of discharging of waste liquid.In addition, this
The coating powder for interspersing structure prepared by a little conventional methods, surface silver content is low, does not possess antioxidation in normal temperature, causes the nothing of silver
Effect wastes, while there also have that deposition velocity is high, the adhesion of reunite between particle more serious, silvering and copper powder is not strong etc. to be prominent
Problem.
The content of the invention
The technical problem to be solved in the present invention is overcome the deficiencies in the prior art, there is provided a kind of preparation side of cuprum argentum composite powder
Method, cuprum argentum composite powder made from this method is while high conduction performance is kept, good in oxidation resistance, particularly suitable for environment
Temperature is higher, conductivity requirements are high, in terms of the electronic device of military service stable performance and its packaging, as electrode, electromagnetic screen coating,
Surface-assembled conducting resinl, it is conductively connected dispensing.
In order to solve the above technical problems, technical scheme proposed by the present invention is：
A kind of preparation method of cuprum argentum composite powder, comprises the following steps：
(1) cu-ag alloy powderses are prepared using gas atomization, in the cu-ag alloy powderses silver-colored mass percent for 3%~
14%；
(2) cu-ag alloy powderses prepared by step (1) are subjected to Ageing Treatment in vacuum or inert atmosphere and obtain copper silver again
Close powder.
Above-mentioned preparation method, it is preferred that in the step (2), in ageing process, aging temp is 150~350
DEG C, aging time is 10~600min, and less than 50 DEG C samplings are naturally cooled to after completion of prescription.
Above-mentioned preparation method, it is preferred that in the step (2), the vacuum pressure in ageing process is less than
0.1MPa。
Above-mentioned preparation method, it is preferred that in the step (2), the inert gas is argon gas or nitrogen.
Above-mentioned preparation method, it is preferred that the gas atomization is nitrogen or Powder In Argon Atomization.
Above-mentioned preparation method, it is preferred that in the step (1), the particle diameter for the cu-ag alloy powderses being prepared is micro- for 120
Rice is following.
Above-mentioned preparation method, it is preferred that cu-ag alloy powderses prepared by step (1) are sieved, filter out particle diameter point
Cloth is that 10~25 microns of powder carries out the Ageing Treatment of step (2) again.
Above-mentioned preparation method, it is preferred that silver is brilliant in copper particle interior edge copper in the cuprum argentum composite powder obtained after Ageing Treatment
Boundary is distributed in sequential like.
The present invention also provides a kind of conducting resinl, and its raw material includes the cuprum argentum composite powder obtained by above-mentioned preparation method.
Above-mentioned conducting resinl, it is preferred that its raw material is (3~6) including mass ratio:1 cuprum argentum composite powder and organic mixed
Compound, the organic mixture are (20~90) including mass ratio:(5~50):(10~50):The E-51 type ring oxygen of (1~10)
Resin, dicyandiamide, diluent 501,2-ethyl-4-methylimidazole.
Compared with prior art, the advantage of the invention is that：
(1) cu-ag alloy powderses that the present invention is prepared first with aerosolization are spherical big (1~120 μ of particle size range selectivity
M), silver content is low, and rich silver mutually preferentially separates out at the defects of crystal boundary and forms continuous space network structure after Ageing Treatment, has
Beneficial to the formation of silver-colored conductive network, electric conductivity is enhanced to a certain extent.Simultaneously as defect (crystal boundary, hole in matrix
Gap, hole) etc. the silver-colored phase that is precipitated covered, effectively inhibit the copper silver powder position in the crystal boundary the defects of at relatively high temperatures
Preferential oxidation, the initial oxidation temperature of matrix can be significantly improved.In consideration of it, cuprum argentum composite powder end made from the technique of the present invention is simultaneous
Have excellent electric conductivity and inoxidizability, be used in electronic industry slurry, preferable conductive filler, particularly suitable for environment temperature compared with
In terms of high, conductivity requirements height, the electronic device of military service stable performance and its packaging, such as electrode, electromagnetic screen coating, surface group
Dress conducting resinl, it is conductively connected dispensing.
(2) silver is uniformly solid-solubilized in Copper substrate in the intermediate products cu-ag alloy powderses of preparation method of the invention, timeliness heat
After processing, silver separates out from Copper substrate, and is preferentially separated out at crystal boundary position, and forms continuous silver-colored network.At timeliness heat of the present invention
Reason causes silver to be segregated in the grain boundaries that energy is higher, unstable, and crystal boundary is exactly the position that powder preferential oxidation occurs, these edges
The silver of crystal boundary distribution effectively prevent the generation that powder aoxidizes in lower temperature.
(3) conducting resinl made from cuprum argentum composite powder end of the invention is not only with conductance is high, moisture-proof is good, inoxidizability
The advantages that high, resistance to silver ion migration are hundred times of pure sliver-powder conducting glue.Cuprum argentum composite powder in a big way it is interior may replace it is existing
Silver powder, copper powder, have be widely applied very much value.
(4) preparation method processing step of the invention is simple, is not related to the use of any chemical solvent, so as to avoid producing
Environmental problem caused by a large amount of discharging of waste liquid, while the copper argentum reagent utilization rate in the preparation method is high.
Brief description of the drawings
Fig. 1 is the pattern micrograph of Kufil powder prepared by atomization in embodiment 1.
Fig. 2 be the embodiment of the present invention 1 after aging strengthening model silver in distribution schematic diagram of the particle along crystal boundary.
The mode that Fig. 3 instills deionized water between the electrode in the embodiment of the present invention 2 on a glass simulates condensation state
Figure.
Fig. 4 is the cuprum argentum composite powder particle that the silver-colored mass content obtained in the embodiment of the present invention 3 after timeliness 30min is 6%
Cross-section photographs.
Fig. 5 is the cuprum argentum composite powder particle that the silver-colored mass content obtained in the embodiment of the present invention 3 after timeliness 30min is 6%
The silver element distribution map of section.
Fig. 6 be the silver-colored mass content obtained in the embodiment of the present invention 3 after timeliness 30min be 6% cuprum argentum composite powder with it is pure
The aerial thermogravimetric analysis figure of copper powder.
Embodiment
For the ease of understanding the present invention, the present invention is made below in conjunction with Figure of description and preferred embodiment more complete
Face, meticulously describe, but protection scope of the present invention is not limited to embodiment in detail below.
Except there is a special instruction, the various reagents used in the present invention, raw material be can be commercially commodity or
Person can pass through product made from known method.
Embodiment 1：
A kind of preparation method of cuprum argentum composite powder of the invention, comprises the following steps：
(1) graphite crucible for being loaded with one 400g silver ingots and 3600g copper plates is put into the manufacture of PSI companies of Britain
In Hermiga gas atomization devices, 1150 DEG C are heated to 50 DEG C/min speed from room temperature, fusing obtains homogeneous hybrid alloys
Liquation, by hybrid alloys liquation being atomized to obtain Kufil powder that silver content is 10% using high pressure nitrogen atomization, (particle diameter is
Less than 120 microns).
(2) cu-ag alloy powderses that step (1) obtains first are screened out into -100 mesh powders, then using 600 mesh and 800 mesh
Standard screen to obtain particle size distribution range be 10~25 μm of Kufil powder, be as shown in Figure 1 subsphaeroidal powder.
(3) cu-ag alloy powderses that 20g steps (2) are sieving through are weighed to be put into the preferable stove of sealing, are reused electronic
Oil pump is pumped to vacuum in stove and reaches -0.05MPa, then starts to warm up to 350 DEG C and is incubated 180min, then naturally cools to
50 DEG C, cuprum argentum composite powder is taken out, silver crystal boundary in copper particle interior edge copper particle is in the signal of sequential like distribution in cuprum argentum composite powder
Figure is as shown in Figure 2.
It is 80 according to mass ratio:8:20:2:0.5 amount is by E-51 types epoxy resin, dicyandiamide, diluent 501,2- second
Base -4-methylimidazole, KH550 additions grind 50min to being uniformly mixed to get organic mixture in mortar.Again by the present embodiment
The cuprum argentum composite powder being prepared is 4 in mass ratio with the organic mixture:1 ratio mixing, 30min is ground to glue with pestle
Body is uniform, and then obtains the conducting resinl that cuprum argentum composite powder is filler.By well mixed conductive glue on stainless steel substrates, shape
Into 70 × 6 × 0.05mm film, intermediate temperature setting processing (200 DEG C of solidification temperature, solidifying duration 1h) is carried out afterwards.Reuse number
Word resistance meter surveys the resistance at its lines both ends, according to " ρ=R × (W × H)/L calculates resistivity, and (ρ is the body electricity of conducting resinl
Resistance rate；R is the resistance of conducting resinl；W, H, L are followed successively by the width, thickness and length of conductive adhesive layer) ", measure five times and try to achieve averagely
It is worth for 85 μ Ω cm, this shows conducting resinl made of the cuprum argentum composite powder end of the present embodiment and sliver-powder conducting glue electric conductivity phase
As (≤100 μ Ω cm).
Embodiment 2：
A kind of preparation method of cuprum argentum composite powder of the invention, comprises the following steps：
(1) graphite crucible for being loaded with one 35g silver ingots and 380g copper plates is put into the manufacture of PSI companies of Britain
In Hermiga gas atomization devices, 1200 DEG C are heated to 50 DEG C/min speed from room temperature, fusing obtains homogeneous alloy and melted
Liquid, it is atomized to be formed to obtain the Kufil powder that silver content is 8.43% using high pressure nitrogen (particle diameter is less than 120 microns).
(2) cu-ag alloy powderses that step (1) obtains first are screened out into -100 mesh powders, then using 600 mesh and 800 mesh
Standard screen to obtain particle size distribution range be 10~25 μm of Kufil powder.
(3) cu-ag alloy powderses that 10g steps (2) obtain are weighed to be put into the preferable stove of sealing, reuse electronic oil
Pump is pumped to vacuum in stove and reaches -0.05MPa, then starts to warm up to 300 DEG C and is incubated 260min, then naturally cools to 50
Below DEG C, cuprum argentum composite powder is taken out.
It is 90 according to mass ratio:9:18:1:0.5 amount is by E-51 types epoxy resin, dicyandiamide, diluent 501,2- second
Base -4-methylimidazole, KH550 additions grind 60min to being uniformly mixed to get organic mixture in mortar.Again by the present embodiment
The cuprum argentum composite powder being prepared is 5 in mass ratio with the organic mixture:1 ratio mixing, 35min is ground to glue with pestle
Body is uniform, and then obtains the conducting resinl that cuprum argentum composite powder is filler.By well mixed conductive glue on stainless steel substrates, shape
Into 70 × 6 × 0.05mm film, intermediate temperature setting processing (220 DEG C of solidification temperature, solidifying duration 50min) is carried out afterwards.
Cuprum argentum composite powder end conductive rubber made of the present embodiment is placed on 100 DEG C, 90%RH (relative humidity) environment
Determine its resistivity after middle 1200h, and by " resistance change rate=(constant temperature and humidity place after resistance-initial stage resistance)/initial stage electricity
Resistance × 100% " calculates resistance change rate, and the actually measured conducting resinl resistance change rate is 3%, the practical mesh less than 10%
Mark.
Conductive rubber printing in cuprum argentum composite powder end made of the present embodiment on a glass, is formed into a length of 10mm, a width of
2mm and apart 2mm two parallel poles, heat preservation solidification 50min in 180 DEG C of isoperibol is placed on by this parallel pole,
The electrode after solidification is accessed into loop again, condensation state is simulated by way of instilling deionized water between electrode, such as Fig. 3 institutes
Show, the electromigration situation of the different time under electric field action is finally taken with camera.After energization 60min the interpolar of conducting resinl two,
Obvious dendroid precipitate is had no from negative pole to positive pole, illustrates that the silver ion migration rate of cuprum argentum composite powder colloid is extremely low.Therefore should
Colloid military service stability is high, securely and reliably.
Cuprum argentum composite powder end conducting resinl made of the present embodiment is put on into stainless steel test piece, and (test piece is by 180 mesh water mills
What sand paper was polished and cleaned with acetone) side, it is sent into temperature after the unilateral overlap joint of the same test piece of two panels is clamped and has stablized 200
DEG C drying box in start curing process, taken out after 1h, be put on cupping machine and survey its shear strength.Sample prepares and test
Performed in strict accordance with GB/T7124-1986 standards, the shear strength of the electrocondution slurry measured is 22MPa, meets that LED encapsulation is used
The strong requirement more than 15MPa of shearing of electrocondution slurry.
Embodiment 3：
The preparation method of the cuprum argentum composite powder of the present invention, comprises the following steps：
(1) it is respectively 0.1g and 9.9g, 0.4g and 9.6g, 0.6g and 9.4g, 0.8g equipped with silver ingot and copper plate by seven
The Hermiga of PSI companies of Britain manufacture is put into 9.2g, 1.0g and 9.0g, 1.2g and 8.8g, 1.4g and 8.6g graphite crucible
In gas atomization device, 1200 DEG C are heated to 50 DEG C/min speed from room temperature, fusing obtains homogeneous alloy molten solution, uses high pressure
Nitrogen atomization forms the Kufil powder for obtaining 1%, 4%, 6%, 8%, 10%, 12% and 14% silver medal mass content successively.
(2) cu-ag alloy powderses that pure copper powder and step (1) obtain first are screened out into -100 mesh powders, then using 600
Mesh and 800 the polished standard screens obtain the Kufil powder that particle size distribution range is 10~25 μm.
(3) divide 3 batches to weigh 8 kinds of powder, each every kind of powder 2g that step (2) obtains and be put into the preferable stove of sealing
It is interior, reuse electric oil pump and be pumped to vacuum in stove and reach -0.08MPa, then start to warm up to 300 DEG C and be incubated respectively
10th, 30,60min, then 50 DEG C are naturally cooled to, take out cuprum argentum composite powder.The initial oxidation temperature measured using thermogravimetric analyzer
As shown in table 1, initial oxidation weightening temperature is defined as the temperature that gain in weight is 1%.As shown in Table 1, silver content increase and when
Effect heat treatment can significantly improve the oxidation resistance at cuprum argentum composite powder end.Pure copper powder and different silver content copper silver are multiple in the present embodiment
Powder electrical conductivity of powder after 200 DEG C of oxidations is closed to be shown in Table 2, as shown in Table 2, the increase of heat treatment time and silver content, by
In the raising of powder inoxidizability, be advantageous to improve the electrical conductivity of powder at high temperature.But silver content is too high may to cause silver
Ion transfer phenomenon is aggravated, therefore silver content is controlled in 3%-14% in the cuprum argentum composite powder of the present invention.
The pure copper powder and the oxidation resistance of cuprum argentum composite powder that the embodiment 3 of table 1 is prepared
The pure copper powder and the electrical conductivity of cuprum argentum composite powder that the embodiment 3 of table 2 is prepared
The silver-colored mass content that timeliness 30min is obtained in the present embodiment is 6% cuprum argentum composite powder particle cross-section photographs such as Fig. 4
Shown, the silver element analysis of section is as shown in figure 5, from Fig. 4 and Fig. 5, and after heat treatment, silver is prior to copper crystal boundary in particle
Separate out and be in continuously distributed state, form the conductive network based on silver.
The cuprum argentum composite powder and pure copper powder that the silver-colored mass content that timeliness 30min is obtained in the present embodiment is 6% are in atmosphere
Thermogravimetric analysis as shown in fig. 6, compared to fine copper powder, the oxidation resistance of the Kufil powder of nonageing is higher, through when
After effect processing, alloy powder now should because the precipitation of silver copper crystal boundary along particle, the antioxygenic property of powder further improve
Powder can be suitable for using as conducting resinl at relatively high temperatures in the case where keeping high conductivity.
Claims (3)
1. a kind of conducting resinl, it is characterised in that its raw material is (3~6) including mass ratio:1 cuprum argentum composite powder and organic mixed
Compound, the organic mixture are (20~90) including mass ratio:(5~50):(10~50):The E-51 type ring oxygen of (1~10)
Resin, dicyandiamide, diluent 501,2-ethyl-4-methylimidazole；Wherein, the preparation method of the cuprum argentum composite powder include with
Lower step：
(1) cu-ag alloy powderses are prepared using gas atomization, silver-colored mass percent is 3%~14% in the cu-ag alloy powderses；
(2) cu-ag alloy powderses prepared by step (1) are subjected to Ageing Treatment in vacuum or inert atmosphere and obtain cuprum argentum composite powder；
In ageing process, aging temp is 150~350 DEG C, and aging time is 10~600min, and vacuum pressure is less than 0.1MPa；
Silver is in continuously distributed in copper particle interior edge copper crystal boundary in the cuprum argentum composite powder obtained after Ageing Treatment；
Cu-ag alloy powderses prepared by step (1) are sieved, the powder that particle diameter distribution is 10~25 microns is filtered out and carries out again
The Ageing Treatment of step (2).
2. conducting resinl as claimed in claim 1, it is characterised in that in the step (2), inert atmosphere refers to argon gas or nitrogen
Gas.
3. conducting resinl as claimed in claim 1, it is characterised in that in the step (1), the cu-ag alloy powderses that are prepared
Particle diameter is less than 120 microns.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610274044.2A CN105921737B (en) | 2016-04-28 | 2016-04-28 | The preparation method and conducting resinl of a kind of cuprum argentum composite powder |
| PCT/CN2017/089121 WO2017186192A1 (en) | 2016-04-28 | 2017-06-20 | Preparation method for copper-silver composite powder, and conductive adhesive |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610274044.2A CN105921737B (en) | 2016-04-28 | 2016-04-28 | The preparation method and conducting resinl of a kind of cuprum argentum composite powder |
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| CN105921737A CN105921737A (en) | 2016-09-07 |
| CN105921737B true CN105921737B (en) | 2018-01-19 |
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| CN105921737B (en) * | 2016-04-28 | 2018-01-19 | 中南大学 | The preparation method and conducting resinl of a kind of cuprum argentum composite powder |
| TWI668709B (en) | 2017-07-25 | 2019-08-11 | 日商千住金屬工業股份有限公司 | Method for synthesizing copper-silver alloy, forming method of conducting part, copper-silver alloy and conducting part |
| CN111101008B (en) * | 2019-12-26 | 2021-08-17 | 浙江杭机新型合金材料有限公司 | High-strength high-conductivity copper-silver alloy material and preparation method thereof |
| CN115260955B (en) * | 2022-07-26 | 2024-04-19 | 深圳市计量质量检测研究院 | Silver conductive adhesive containing conductive additive and preparation method and application thereof |
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| US4716081A (en) * | 1985-07-19 | 1987-12-29 | Ercon, Inc. | Conductive compositions and conductive powders for use therein |
| US6620344B2 (en) * | 1999-05-28 | 2003-09-16 | Dowa Mining Co., Ltd. | Copper particle clusters and powder containing the same suitable as conductive filler of conductive paste |
| CN1176234C (en) * | 2002-12-31 | 2004-11-17 | 西安理工大学 | High temperature resistant anti-oxidant base metal copper-silver alloy composition and its producing method |
| JP5080731B2 (en) * | 2005-10-03 | 2012-11-21 | 三井金属鉱業株式会社 | Fine silver particle-attached silver-copper composite powder and method for producing the fine silver particle-attached silver-copper composite powder |
| CN100464001C (en) * | 2006-04-11 | 2009-02-25 | 中国科学院金属研究所 | High-strength high-conductivity oxidation-resisting low-silver copper-base alloy and preparation thereof |
| CN101158018A (en) * | 2007-11-19 | 2008-04-09 | 北京矿冶研究总院 | AgCu coating material and preparation method of coating |
| CN101418393B (en) * | 2008-12-01 | 2010-06-02 | 昆明贵金属研究所 | Novel method for preparing AgCuV alloy material |
| CN102423805A (en) * | 2011-11-23 | 2012-04-25 | 西安理工大学 | Preparation method of CuCr alloy powder with low chromium content |
| CN102489710B (en) * | 2011-12-19 | 2013-10-02 | 中国兵器工业第五二研究所 | Method for increasing collection efficiency in preparing nanometer copper-silver alloy powder by using inductive plasmas |
| JP2014005531A (en) * | 2012-01-17 | 2014-01-16 | Dowa Electronics Materials Co Ltd | Silver-coated copper alloy powder and method for producing the same |
| CN103820664B (en) * | 2014-02-25 | 2016-04-06 | 西安理工大学 | A kind of short route prepares the method for precipitation strength chromiumcopper |
| CN105921737B (en) * | 2016-04-28 | 2018-01-19 | 中南大学 | The preparation method and conducting resinl of a kind of cuprum argentum composite powder |
-
2016
- 2016-04-28 CN CN201610274044.2A patent/CN105921737B/en not_active Expired - Fee Related
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2017
- 2017-06-20 WO PCT/CN2017/089121 patent/WO2017186192A1/en active Application Filing
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| Publication number | Publication date |
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| CN105921737A (en) | 2016-09-07 |
| WO2017186192A1 (en) | 2017-11-02 |
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