CN105414556A - Water-base nano-silver paste thinning method and application of water-base nano-silver paste - Google Patents
Water-base nano-silver paste thinning method and application of water-base nano-silver paste Download PDFInfo
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- CN105414556A CN105414556A CN201510839979.6A CN201510839979A CN105414556A CN 105414556 A CN105414556 A CN 105414556A CN 201510839979 A CN201510839979 A CN 201510839979A CN 105414556 A CN105414556 A CN 105414556A
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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
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
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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
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0545—Dispersions or suspensions of nanosized particles
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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
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- B82Y40/00—Manufacture or treatment of nanostructures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
- H01L2224/80—Methods for connecting semiconductor or other solid state bodies using means for bonding being attached to, or being formed on, the surface to be connected
- H01L2224/83—Methods for connecting semiconductor or other solid state bodies using means for bonding being attached to, or being formed on, the surface to be connected using a layer connector
- H01L2224/838—Bonding techniques
- H01L2224/8384—Sintering
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Abstract
The invention discloses a water-base nano-silver paste thinning method and application of water-base nano-silver paste. The method includes the steps that firstly, deionized water is added into the water-base nano-silver paste for attenuation and cleaning; secondly, stirring and sufficient mixing are conducted; thirdly, a nitrate electrolyte solution is added to the mixed solution for flocculation; fourthly, high-speed centrifugal separation is conducted, an upper-layer solution is removed, and the nano-silver paste at the bottom is reserved; and fifthly, the first step, the second step, the third step and the fourth step are repeated multiple times, and the water-base nano-silver paste is obtained after thinning of organic wrapping layers. According to the water-base nano-silver paste thinning method and the application of the water-base nano-silver paste, the organic wrapping layers on the surfaces of nano-silver particles are thinned and attenuated, the effects of lowering the sintering temperature of the nano-silver paste and shortening the sintering time are achieved, and non-pressure auxiliary sintering interconnecting is achieved. The prepared nano-silver paste is used for the chip level sintering interconnecting technology, the mechanical performance and heat conductivity of a nano-silver paste interconnecting head obtained before the thinning treatment is conducted are obviously improved, and great significance is achieved on radiating of chip level interconnecting in large-power density electronic packaging.
Description
Technical field
The invention belongs to Electronic Packaging field, be applicable to electronic package interconnections range of application, be specifically related to the technique of chip-scale or other micro devices attachment water base nano silver slurry thining method and the quick interconnection with no pressure of low temperature thereof.
Background technology
Nanometer silver paste, as a kind of New-core chip level interconnection material, has three advantages compared to traditional solder solder: without interconnection welding spot remelting phenomenon, high heat-conductivity conducting performance, high reliability.
But the shortcoming of nanometer silver paste limits its range of application, namely interconnecting, temperature is high, required time is long, for heat-sensitive device and substrate, has exceeded its ability of being heated.In addition, nanometer silver paste needs to apply pressure and assists in chip level interconnect process, is unfavorable for the realization of automation.
The reason of nanometer silver paste the problems referred to above is caused to be coated on nano-Ag particles surface in nanometer silver paste to play protection nano-Ag particles that the organic coating layer thickness of agglomeration in advance does not occur is excessive.In interconnection process, organic coating layer needs first to carry out decomposing just to make nano-Ag particles come in contact, thus realizes sintering interconnection.And the sintering process of blocked up organic coating layer nano-Ag particles when seriously hindering chip level interconnect, cause required sintering interconnection temperature too high, overlong time, manufacturability is poor, the interconnection shearing strength of joint of formation and heat-conductivity conducting low.
Chinese patent " a kind of low temperature-sintered nano silver paste and preparation method thereof ", application number CN201110104399, disclose a kind of preparation method of nanometer silver paste, but preparation system is oil base nanometer silver paste, cannot carry out the thinning of organic coating layer according to this patent method.
Chinese patent " a kind of chip attachment nanometer silver paste and preparation method thereof ", application number CN201210426581.6, disclose a kind of preparation method of nanometer silver paste, use electronation to send out and prepare water base nano silver slurry, but owing to not carrying out reduction processing to organic coating layer, its nanometer silver paste be used for chip level interconnect obtain shearing strength of joint and thermal conductivity lower.
Other patent about nanometer silver paste, due to the technical field difference (biological medicine, printed electronic slurry) of application, does not explain.
Summary of the invention
The object of the invention is by the thinning organic layer thickness being coated on nanometer silver paste surface, realize the quick interconnection process with no pressure of low temperature, solve in prior art, nanometer silver paste is high for chip level interconnect technological temperature, required time long, need the defect of aux. pressure.
For achieving the above object, the invention provides a kind of water base nano silver slurry thining method, method comprises following steps:
Step 1, adds deionized water in water base nano silver slurry, carries out dilution cleaning;
Step 2, stirs, fully mixes;
Step 3, adds nitrate electrolyte solution, flocculates, stir in mixed solution;
Step 4, carries out high speed centrifugation separation, removes upper solution, retains bottom nanometer silver paste;
Step 5, repeats step 1-step 4 several times, obtain organic coating layer thinning after water base nano silver slurry.
Above-mentioned water base nano silver slurry thining method, wherein, in step 1, water base nano silver slurry concentration is in deionized water 0.1-1g/mL.
Above-mentioned water base nano silver slurry thining method, wherein, in step 2, also comprises applying ultrasonication.
Above-mentioned water base nano silver slurry thining method, wherein, in step 3, described nitrate concentration of electrolyte solutions is 1-5mol/L.Described nitrate electrolyte is preferably potassium nitrate or sodium nitrate or the mixture of the two.
Above-mentioned water base nano silver slurry thining method, wherein, in step 4, described high speed centrifugation is separated, and rotating speed is 2000-5000r/min.
Above-mentioned water base nano silver slurry thining method, wherein, in step 5, repeats 2-4 step 1-step 4.
Present invention also offers the purposes of a kind of water base nano silver slurry adopting above-mentioned water base nano silver slurry thining method to prepare for chip-scale sintering interconnection process.
Described chip-scale sintering interconnection process parameter is: after 80-120 DEG C of low-temperature space insulation 5-20min, and raised temperature is to 150-300 DEG C, and insulation 30-120s, with stove cooling or Air flow, forms interconnection joint.
This chip-scale sintering interconnection process, does not need to apply pressure and assists.
Beneficial effect of the present invention:
1, the inventive method can the organic coating layer on nano-Ag particles surface in the water base nanometer silver paste of thinning dilution simply and effectively, its thickness and coated density are declined, thus reach the effect reducing nanometer silver paste sintering temperature, shorten sintering time, and realize, without the interconnection of pressure assisted sintering, being easy to automation.
2, the nanometer silver paste prepared of the inventive method, for chip-scale sintering interconnection process, the interconnection shearing strength of joint of acquisition is up to 60MPa, and thermal conductivity reaches 229W/mK; Significantly improve the mechanical property not making nanometer silver paste interconnection joint before reduction processing, and significantly promoting the heat radiation of high power density Electronic Packaging SMIS chip level interconnection of thermal conductivity is significant.
3, the chip level interconnect technique of nanometer silver paste has also been carried out effective optimization by the present invention, reduces sintering interconnection temperature, shortens interconnection time, without the need to pressure assisted sintering.Nanometer silver paste is made to be applicable to the interconnection of the not high device of heat resistance and substrate.This technique can be mutually compatible with now widely used solder interconnection process, expands the range of application of nanometer silver paste.
Detailed description of the invention
Water base nano silver slurry thining method provided by the invention comprises following steps:
Step 1: the deionized water adding 10mL-100mL in every 10g water base nano silver slurry, carries out dilution cleaning;
Step 2: apply ultrasonication, carry out mechanical agitation simultaneously, fully mix;
Step 3: the nitrate electrolyte solution adding 1mol/L-5mol/L, 10mL-100mL in mixed solution, flocculates, stirs; This nitrate electrolyte is preferably potassium nitrate or sodium nitrate or the mixture of the two.
Step 4: carry out high speed centrifugation separation, rotating speed is 2000-5000r/min, removes upper solution, retains bottom nanometer silver paste;
Step 5: by nanometer silver paste according to above-mentioned four steps, repeatedly carry out 2-4 time, obtain organic coating layer thinning after water base nano silver slurry.
Nanometer silver paste point step 5 obtained is applied to substrate pads surface, chip placement on pad, the interconnection of chip and substrate is realized by hot blast workbench or heating furnace, this interconnection process parameter is, after 80-120 DEG C of low-temperature space insulation 5-20min, raised temperature is to 150-300 DEG C, insulation 30-120s, with stove cooling or Air flow, forms interconnection joint.This technical process does not need to apply pressure and assists, and is easy to automation.
Technical scheme of the present invention is described in detail below in conjunction with embodiment.
Embodiment 1
Take 10g water base nano silver slurry, 100mL deionized water is joined in nanometer silver paste, apply ultrasonication and mechanical agitation, nanometer silver paste is mixed.The potassium nitrate solution of 100mL, 3mol/L is added in the above-mentioned solution mixed, stir fully.Carry out high speed centrifugation separation, rotating speed is 3000r/min.Remove upper solution.The nanometer silver paste of bottom is proceeded washed with de-ionized water and potassium nitrate solution flocculation step, repeat four times.Finally obtain organic coating layer thinning after water base nano silver slurry.
By the nanometer silver paste spot printing after thinning and substrate position to be welded, chip placement, uses the heating of hot blast workbench, and after 120 DEG C of insulation 5min, raised temperature to 250 DEG C, temperature retention time is 120s, Air flow, forms sintering interconnection joint.Shearing strength of joint is 40MPa, and thermal conductivity is 190W/mK.
Embodiment 2
Take 10g water base nano silver slurry, 50mL deionized water is joined in nanometer silver paste, apply ultrasonication and mechanical agitation, nanometer silver paste is mixed.The sodium nitrate solution of 50mL, 1mol/L is added in the above-mentioned solution mixed, stir fully.Carry out high speed centrifugation separation, rotating speed is 2000r/min.Remove upper solution.The nanometer silver paste of bottom is proceeded washed with de-ionized water and sodium nitrate solution flocculation step, repeat four times.Finally obtain organic coating layer thinning after water base nano silver slurry.
By the nanometer silver paste spot printing after thinning and substrate position to be welded, chip placement, uses the heating of hot blast workbench, and after 80 DEG C of insulation 20min, raised temperature to 200 DEG C, temperature retention time is 60s, Air flow, forms sintering interconnection joint.Shearing strength of joint is 35MPa, and thermal conductivity is 173W/mK.
Embodiment 3
Take 10g water base nano silver slurry, 10mL deionized water is joined in nanometer silver paste, apply ultrasonication and mechanical agitation, nanometer silver paste is mixed.The potassium nitrate solution of 10mL, 5mol/L is added in the above-mentioned solution mixed, stir fully.Carry out high speed centrifugation separation, rotating speed is 5000r/min.Remove upper solution.The nanometer silver paste of bottom is proceeded washed with de-ionized water and sodium nitrate solution flocculation step, repeat secondary.Finally obtain organic coating layer thinning after water base nano silver slurry.
By the nanometer silver paste spot printing after thinning and substrate position to be welded, chip placement, uses the heating of hot blast workbench, and after 100 DEG C of insulation 10min, raised temperature to 300 DEG C, temperature retention time is 30s, Air flow, forms sintering interconnection joint.Shearing strength of joint is 60MPa, and thermal conductivity is 229W/mK.
In sum, the invention provides a kind of short-cut method organic coating layer on nano-Ag particles surface in the water base nanometer silver paste of thinning dilution effectively, its thickness and coated density are declined, this nanometer silver paste is used for chip level interconnect technique, not only reduce sintering interconnection temperature, shorten interconnection time, and without the need to pressure assisted sintering, make nanometer silver paste be applicable to the interconnection of the not high device of heat resistance and substrate, expand the range of application of nanometer silver paste.And, nanometer silver paste prepared by the inventive method, for chip-scale sintering interconnection process, the interconnection shearing strength of joint of acquisition is up to 60MPa, and thermal conductivity reaches 229W/mK; Significantly improve the mechanical property not making nanometer silver paste interconnection joint before reduction processing, and significantly promoting the heat radiation of high power density Electronic Packaging SMIS chip level interconnection of thermal conductivity is significant.
Although content of the present invention has done detailed introduction by above preferred embodiment, will be appreciated that above-mentioned description should not be considered to limitation of the present invention.After those skilled in the art have read foregoing, for multiple amendment of the present invention and substitute will be all apparent.Therefore, protection scope of the present invention should be limited to the appended claims.
Claims (10)
1. a water base nano silver slurry thining method, it is characterized in that, method comprises following steps:
Step 1, adds deionized water in water base nano silver slurry, carries out dilution cleaning;
Step 2, stirs, fully mixes;
Step 3, adds nitrate electrolyte solution, flocculates, stir in mixed solution;
Step 4, carries out high speed centrifugation separation, removes upper solution, retains bottom nanometer silver paste;
Step 5, repeats step 1-step 4 several times, obtain organic coating layer thinning after water base nano silver slurry.
2. water base nano silver slurry thining method as claimed in claim 1, is characterized in that, in step 1, water base nano silver slurry concentration is in deionized water 0.1-1g/mL.
3. water base nano silver slurry thining method as claimed in claim 1, is characterized in that, in step 2, also comprise applying ultrasonication.
4. water base nano silver slurry thining method as claimed in claim 1, it is characterized in that, in step 3, described nitrate concentration of electrolyte solutions is 1-5mol/L.
5. water base nano silver slurry thining method as claimed in claim 1, is characterized in that, in step 3, described nitrate electrolyte is potassium nitrate or sodium nitrate or the mixture of the two.
6. water base nano silver slurry thining method as claimed in claim 1, it is characterized in that, in step 4, described high speed centrifugation is separated, and rotating speed is 2000-5000r/min.
7. water base nano silver slurry thining method as claimed in claim 1, is characterized in that, in step 5, repeat 2-4 step 1-step 4.
8. the water base nano silver adopting water base nano silver according to claim 1 slurry thining method to prepare starches the purposes sintering interconnection process for chip-scale.
9. purposes as claimed in claim 8, is characterized in that, this chip-scale sintering interconnection process parameter is: after 80-120 DEG C of low-temperature space insulation 5-20min, and raised temperature is to 150-300 DEG C, and insulation 30-120s, with stove cooling or Air flow, forms interconnection joint.
10. purposes as claimed in claim 9, is characterized in that, this chip-scale sintering interconnection process, does not need to apply pressure and assists.
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| CN201510839979.6A CN105414556A (en) | 2015-11-27 | 2015-11-27 | Water-base nano-silver paste thinning method and application of water-base nano-silver paste |
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| CN201510839979.6A CN105414556A (en) | 2015-11-27 | 2015-11-27 | Water-base nano-silver paste thinning method and application of water-base nano-silver paste |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108847395A (en) * | 2018-06-25 | 2018-11-20 | 深圳市先进连接科技有限公司 | A kind of preparation of pre-sintering nanometer network silverskin and packaging method quickly connected for low temperature |
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| US6660058B1 (en) * | 2000-08-22 | 2003-12-09 | Nanopros, Inc. | Preparation of silver and silver alloyed nanoparticles in surfactant solutions |
| CN1600477A (en) * | 2003-09-28 | 2005-03-30 | 中国印钞造币总公司 | Method for preparing nano silver powder |
| CN1876293A (en) * | 2006-04-03 | 2006-12-13 | 庄平 | Nano-class silver colloidal solution and preparation method thereof |
| CN102290117A (en) * | 2011-04-25 | 2011-12-21 | 深圳市唯特偶新材料股份有限公司 | Low temperature-sintered nano silver paste and preparation method thereof |
| CN102935518A (en) * | 2012-10-31 | 2013-02-20 | 哈尔滨工业大学深圳研究生院 | Nano silver paste for chip mounting and method for preparing nano silver paste |
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- 2015-11-27 CN CN201510839979.6A patent/CN105414556A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6660058B1 (en) * | 2000-08-22 | 2003-12-09 | Nanopros, Inc. | Preparation of silver and silver alloyed nanoparticles in surfactant solutions |
| CN1600477A (en) * | 2003-09-28 | 2005-03-30 | 中国印钞造币总公司 | Method for preparing nano silver powder |
| CN1876293A (en) * | 2006-04-03 | 2006-12-13 | 庄平 | Nano-class silver colloidal solution and preparation method thereof |
| CN102290117A (en) * | 2011-04-25 | 2011-12-21 | 深圳市唯特偶新材料股份有限公司 | Low temperature-sintered nano silver paste and preparation method thereof |
| CN102935518A (en) * | 2012-10-31 | 2013-02-20 | 哈尔滨工业大学深圳研究生院 | Nano silver paste for chip mounting and method for preparing nano silver paste |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108847395A (en) * | 2018-06-25 | 2018-11-20 | 深圳市先进连接科技有限公司 | A kind of preparation of pre-sintering nanometer network silverskin and packaging method quickly connected for low temperature |
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Application publication date: 20160323 |