CN112207481A - Low-temperature pressureless sintering micron silver soldering paste and preparation method and application thereof - Google Patents
Low-temperature pressureless sintering micron silver soldering paste and preparation method and application thereof Download PDFInfo
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- CN112207481A CN112207481A CN202010942292.6A CN202010942292A CN112207481A CN 112207481 A CN112207481 A CN 112207481A CN 202010942292 A CN202010942292 A CN 202010942292A CN 112207481 A CN112207481 A CN 112207481A
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- micron silver
- low
- temperature
- sintering
- micron
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
- B23K35/3006—Ag as the principal constituent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/40—Making wire or rods for soldering or welding
Abstract
The invention discloses a low-temperature pressureless sintering micron silver soldering paste, a preparation method and application thereof, the low-temperature pressureless sintering micron silver soldering paste is prepared from micron silver sheets and a solvent in a certain proportion, the micron silver sheets with proper sizes are selected to be matched with a specific solvent, no extra additive is needed, the uniform dispersion of the micron silver sheets can be realized, the solvent can also promote the tight combination of the micron silver sheets, after low-temperature sintering, the welding joint obtained by using the low-temperature pressureless sintering micron silver soldering paste has higher shearing strength and improved combination strength, a large amount of harmful substances can not be generated during sintering, the required sintering temperature is lower, the energy consumption and the production cost can be reduced, and the low-temperature pressureless sintering micron silver soldering paste can be used as a good welding material for packaging modules.
Description
Technical Field
The invention relates to the technical field of welding materials, in particular to low-temperature pressureless sintering micron silver soldering paste and a preparation method and application thereof.
Background
The silver solder paste is usually used as an interconnection material of a power semiconductor chip, has good electric conduction, heat conduction and high temperature resistance, is mainly prepared from various additives such as silver particles, a dispersing agent, a diluting agent, an organic carrier and the like, for example, Chinese patent CN110508970A (application publication No. 2019.11.19) discloses a three-peak system mixed silver solder paste which is prepared from nano-scale, submicron-scale and micron-scale silver particles, a dispersing agent, a binding agent and a diluting agent in a certain proportion, the sintering temperature is 230-270 ℃, but the sintering temperature required by the silver solder paste is higher, and the additives can generate a large amount of harmful substances at high temperature.
Disclosure of Invention
The invention aims to solve the technical problems that the existing silver soldering paste has high sintering temperature and generates a large amount of harmful substances during sintering, and provides the low-temperature pressureless sintering micron silver soldering paste which has low required sintering temperature, does not contain additives, does not generate a large amount of harmful substances during sintering and has good shear strength of a sintered welding joint.
The invention also aims to provide a preparation method of the low-temperature pressureless sintering micron silver soldering paste.
Another object of the present invention is to provide a use of the low-temperature pressureless sintering micron silver solder paste.
The above purpose of the invention is realized by the following technical scheme:
a low-temperature pressureless sintering micron silver soldering paste is prepared from 6-10 parts by mass of micron silver sheets and 1-2 parts by mass of a solvent, wherein the diameter of the micron silver sheets is 1-50 mu m, the thickness of the micron silver sheets is 0.05-5 mu m, and the solvent is one or more of ethylene glycol, 1, 2 propylene glycol, acrylic acid, sodium citrate, diethylene glycol diethyl ether, n-amyl ether and isoamyl ether.
The invention provides a low-temperature pressureless sintering micron silver soldering paste, which selects a solvent capable of improving the surface activity of micron silver sheets to uniformly disperse the micron silver sheets, is more favorable for dispersing the micron silver sheets in a system by optimizing the micron silver sheets and the size of the micron silver sheets, can promote the close connection between the micron silver sheets by the interaction of the solvent and the micron silver sheets during sintering, does not need additional additives such as an adhesive and the like, and therefore, does not generate a large amount of harmful substances during sintering.
Preferably, the silver paste is prepared from 8-9 parts by mass of micron silver flakes and 1-1.5 parts by mass of a solvent.
Preferably, the diameter of the micron silver sheet is 1-20 μm, and the thickness of the micron silver sheet is 0.05-1 μm.
Preferably, the silver paste also comprises 1-3 parts of micron silver balls.
Preferably, the diameter of the micron silver ball is 1-50 μm.
Preferably, the diameter of the micron silver ball is 1-5 μm.
Preferably, the solvent is one or more of ethylene glycol, 1, 2 propylene glycol, diethylene glycol diethyl ether, n-amyl ether, isoamyl ether.
The invention protects the preparation method of the low-temperature pressureless sintering micron silver soldering paste, and the low-temperature pressureless sintering micron silver soldering paste is obtained after micron silver sheets and a solvent are uniformly mixed.
The invention also protects the application of the low-temperature pressureless sintering micron silver soldering paste in the welding of the packaging module.
Preferably, the method comprises the following steps:
and (3) placing the low-temperature pressureless sintered micron silver soldering paste on a material to be welded, and sintering at 150-225 ℃ for 1-30 min at the heating rate of 5-10 ℃/min.
Preferably, the sintering temperature is 200-225 ℃.
Compared with the prior art, the invention has the beneficial effects that:
the low-temperature pressureless sintering micron silver soldering paste is prepared from micron silver sheets and a solvent according to a certain proportion, the micron silver sheets are selected and optimized in size, and then are matched with the solvent capable of improving the surface activity of the micron silver sheets, no additional additive is needed, the micron silver sheets can be uniformly dispersed, after pressureless low-temperature sintering, the shearing strength of a welding joint is high, a large amount of harmful substances cannot be generated during sintering, the required sintering temperature is low, and the energy consumption and the production cost are reduced.
Drawings
Fig. 1 is a schematic view of a low-temperature sintering process flow of the low-temperature pressureless sintering micron silver solder paste.
FIG. 2 is a cross-sectional micro-topography of a sintered solder joint of the low temperature pressureless sintered micro silver paste prepared in example 1.
Detailed Description
The present invention will be further described with reference to specific embodiments, but the present invention is not limited to the examples in any way. The starting reagents employed in the examples of the present invention are, unless otherwise specified, those that are conventionally purchased.
Example 1
A low-temperature pressureless sintering micron silver soldering paste comprises 8 parts of micron silver sheets with the diameter of 10 mu m and the thickness of 0.2 mu m calculated according to the mass parts and 2 parts of ethylene glycol.
The preparation method of the low-temperature pressureless sintering micron silver soldering paste comprises the following steps:
and (3) placing the micron silver sheets and ethylene glycol in a planetary stirrer, stirring for 6min in a vacuum mode, and uniformly stirring to obtain the low-temperature pressureless sintering micron silver soldering paste.
Example 2
A low-temperature pressureless sintering micron silver soldering paste is prepared from 7 parts of micron silver sheets, 1 part of micron silver balls and 2 parts of 1, 2-propylene glycol in parts by mass; wherein the diameter of the micron silver sheet is 5 μm, and the thickness is 0.3 μm; the diameter of the micron silver ball is 5 μm.
The preparation method of the low-temperature pressureless sintering micron silver solder paste is the same as that of the embodiment 1.
Example 3
A low-temperature pressureless sintering micron silver soldering paste comprises, by mass, 15 microns in diameter, 0.2 microns in thickness, 8 microns of silver flakes and 1.5 portions of n-amyl ether.
The preparation method of the low-temperature pressureless sintering micron silver solder paste is the same as that of the embodiment 1.
Example 4
A low-temperature pressureless sintering micron silver soldering paste is prepared from 6 parts of micron silver sheets with the diameter of 10 microns and the thickness of 0.2 microns, 2 parts of micron silver sheets with the diameter of 5 microns and the thickness of 0.1 microns and 2 parts of isoamyl ether by mass.
The preparation method of the low-temperature pressureless sintering micron silver solder paste is the same as that of the embodiment 1.
Example 5
A low-temperature pressureless sintering micron silver soldering paste comprises 9 parts of micron silver sheets and 2 parts of acrylic acid, wherein the micron silver sheets are calculated according to the mass parts, the diameter of each micron silver sheet is 1 mu m, and the thickness of each micron silver sheet is 0.05 mu m.
The preparation method of the low-temperature pressureless sintering micron silver solder paste is the same as that of the embodiment 1.
Example 6
A low-temperature pressureless sintering micron silver soldering paste is prepared from 10 parts of micron silver sheets and 2 parts of diethylene glycol diethyl ether by mass, wherein the diameter of each micron silver sheet is 50 mu m, and the thickness of each micron silver sheet is 5 mu m.
The preparation method of the low-temperature pressureless sintering micron silver solder paste is the same as that of the embodiment 1.
Example 7
A low-temperature pressureless sintering micron silver soldering paste comprises 9 parts of micron silver sheets and 2 parts of sodium citrate by mass, wherein the diameter of the micron silver sheets is 20 microns, and the thickness of the micron silver sheets is 0.4 microns.
The preparation method of the low-temperature pressureless sintering micron silver solder paste is the same as that of the embodiment 1.
Comparative example 1
A micro silver solder paste was prepared in the same manner as in example 1, except that the solvent was replaced with glycerin. The preparation method of the micron silver solder paste is the same as that of the embodiment 1.
Comparative example 2
A micro silver paste was prepared in the same manner as in example 1 except that the diameter of the micro silver flakes was replaced with micro silver balls having a diameter of 30 μm. The preparation method of the micron silver solder paste is the same as that of the embodiment 1.
Comparative example 3
A micro silver paste was prepared in the same manner as in example 1 except that the size of the micro silver flakes was changed to 100 μm in diameter and 8 μm in thickness. The preparation method of the micron silver solder paste is the same as that of the embodiment 1.
Comparative example 4
A micron silver solder paste was prepared in the same manner as in example 1 except that the solvent was replaced with glycerin, and 0.1 part of ascorbic acid was added as an additive. The preparation method of the micron silver solder paste is the same as that of the embodiment 1.
Applications of
The micron silver solder paste prepared in each example and each comparative example is placed between a silver-plated silicon chip and a copper substrate, and then the silver-plated silicon chip and the copper substrate are placed on a heating table for pressureless sintering, wherein the specific sintering conditions are shown in the following table 1:
TABLE 1 use of micron silver solder paste prepared in each example and comparative example
| Sintering temperature (. degree. C.) | Rate of temperature rise | Sintering time (min) | |
| Example 1 | 210 | 5 | 15 |
| Example 2 | 225 | 6 | 20 |
| Example 3 | 220 | 7 | 20 |
| Example 4 | 225 | 5 | 25 |
| Example 5 | 210 | 5 | 10 |
| Example 6 | 150 | 5 | 30 |
| Example 7 | 190 | 5 | 15 |
| Comparative example 1 | 250 | 5 | 15 |
| Comparative example 2 | 210 | 5 | 15 |
| Comparative example 3 | 210 | 5 | 15 |
| Comparative example 4 | 210 | 5 | 15 |
Performance testing
1. Test method
Shear strength of the welded joint: the shear strength was measured at room temperature using an MFM1200 push-pull force tester from the company Try precision at a test speed of 10 μm/S.
2. Test results
TABLE 2 results of testing applicability of micro silver solder paste prepared in each example and comparative example
| Shear strength of welded joint (MPa) | |
| Example 1 | 20.6 |
| Example 2 | 35.5 |
| Example 3 | 33.2 |
| Example 4 | 43.2 |
| Example 5 | 22.2 |
| Example 6 | 19.7 |
| Example 7 | 28.8 |
| Comparative example 1 | 17.2 |
| Comparative example 2 | 5.2 |
| Comparative example 3 | 7.1 |
| Comparative example 4 | 12.2 |
As can be seen from table 2, the welded joint after sintering of the low-temperature pressureless sintered micron silver solder paste prepared by the invention has higher shear strength, namely better bonding strength of the sintering layer, wherein the embodiment 2 adopts the combination of the micron silver sheet and the micron silver ball, and because the micron silver ball with a certain size and the micron silver sheet can be uniformly mixed in a solvent, the compactness is improved, the shear strength is improved to a certain extent, and the embodiment 4 adopts two micron silver sheets with different sizes, the shear strength is optimal; in contrast, in comparative example 1, the solvent is replaced by glycerol, in comparative example 4, the solvent is replaced by glycerol, ascorbic acid is also added, but because the silver flakes cannot be well dispersed in the glycerol, the glycerol cannot promote tight connection between the silver flakes, and the shear strength of the welded joint is reduced at a lower sintering temperature; comparative example 2 since the micro silver flakes were replaced with micro silver balls, the weld joint shear strength decreased significantly at lower sintering temperatures; comparative example 3 the weld joint shear strength was significantly reduced due to the oversize of the micron silver flakes. The results show that the sintering temperature required by the low-temperature pressureless sintering micron silver soldering paste is lower, so that a better welding effect can be obtained, the energy consumption is reduced, no additional additive is needed, and no harmful substances are generated.
As can be seen from figure 1, the microstructure change of the low-temperature pressureless sintering micron silver soldering paste in the sintering process is that the solvent volatilizes when the temperature is raised to a certain temperature in the sintering process, and metal bonding is formed among silver particles along with the temperature rise, so that a compact and reliable welding joint is finally obtained.
The cross section of the joint obtained by welding two aluminum plates with silver solder paste is shown in fig. 2, the gray parts of the upper side and the lower side are aluminum substrates, the middle part is porous silver formed by welding with solder paste, and as can be seen from fig. 2, all parts are tightly combined during welding, which indicates that a reliable welded joint is obtained after welding.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (10)
1. The low-temperature pressureless sintering micron silver soldering paste is characterized by comprising 6-10 parts by mass of micron silver sheets and 1-2 parts by mass of solvent, wherein the diameter of the micron silver sheets is 1-50 mu m, the thickness of the micron silver sheets is 0.05-5 mu m, and the solvent is one or more of ethylene glycol, 1, 2 propylene glycol, acrylic acid, sodium citrate, diethylene glycol diethyl ether, n-amyl ether and isoamyl ether.
2. The low-temperature pressureless sintering micron silver solder paste according to claim 1, which is characterized by comprising 8-9 parts of micron silver sheets and 1-1.5 parts of solvent by mass.
3. The low-temperature pressureless sintering micron silver solder paste according to claim 1 or 2, wherein the micron silver sheet has a diameter of 1-20 μm and a thickness of 0.05-1 μm.
4. The low-temperature pressureless sintering micron silver solder paste as claimed in claim 1, further comprising 1-3 parts of micron silver balls.
5. The low-temperature pressureless sintering micron silver solder paste as claimed in claim 4, wherein the diameter of the micron silver ball is 1-50 μm.
6. The low temperature pressureless sintering micrometer silver solder paste of claim 1, wherein the solvent is one or more of ethylene glycol, 1, 2 propylene glycol, diethylene glycol diethyl ether, n-amyl ether, isoamyl ether.
7. The method for preparing the low-temperature pressureless sintering micron silver solder paste according to any one of claims 1 to 6, wherein the low-temperature pressureless sintering micron silver solder paste is obtained by uniformly mixing micron silver sheets and a solvent.
8. Use of the low-temperature pressureless-sintered micron silver solder paste as claimed in any one of claims 1 to 6 in package module soldering.
9. Use according to claim 8, characterized in that it comprises the following steps:
and (3) placing the low-temperature pressureless sintered micron silver soldering paste on a material to be welded, and sintering at 150-225 ℃ for 1-30 min at the heating rate of 5-10 ℃/min.
10. Use according to claim 9, wherein the sintering temperature is 200 to 225 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010942292.6A CN112207481A (en) | 2020-09-09 | 2020-09-09 | Low-temperature pressureless sintering micron silver soldering paste and preparation method and application thereof |
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| CN202010942292.6A CN112207481A (en) | 2020-09-09 | 2020-09-09 | Low-temperature pressureless sintering micron silver soldering paste and preparation method and application thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113492281A (en) * | 2021-05-27 | 2021-10-12 | 中山大学 | Micron silver soldering paste directly sintered on bare copper at low temperature and without pressure, and preparation method and application thereof |
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| JP2002192380A (en) * | 2000-12-27 | 2002-07-10 | Jsr Corp | Soldering paste composition |
| CN101038795A (en) * | 2001-10-18 | 2007-09-19 | 霍尼韦尔国际公司 | Conductive paste and heat diffusion material |
| CN101367158A (en) * | 2008-09-24 | 2009-02-18 | 上海大学 | Binary leadless soldering plaster |
| CN103639614A (en) * | 2013-12-04 | 2014-03-19 | 马鑫 | Nanoscale/micron size particle mixing type lead-free solder paste with size effect and manufacturing method thereof |
| US20170365576A1 (en) * | 2014-12-17 | 2017-12-21 | Nippon Steel & Sumikin Materials Co., Ltd. | Bonding wire for semiconductor device |
| CN108526751A (en) * | 2018-04-26 | 2018-09-14 | 深圳市先进连接科技有限公司 | A kind of micro-nano mixing soldering paste and preparation method thereof can be used for pressureless sintering |
| CN110508970A (en) * | 2019-07-15 | 2019-11-29 | 天津大学 | Three peak systems of one kind mixing silver paste and its application |
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2020
- 2020-09-09 CN CN202010942292.6A patent/CN112207481A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4859825A (en) * | 1986-11-26 | 1989-08-22 | Maria Polvara | Spot welding electrode and method for making it |
| JP2002192380A (en) * | 2000-12-27 | 2002-07-10 | Jsr Corp | Soldering paste composition |
| CN101038795A (en) * | 2001-10-18 | 2007-09-19 | 霍尼韦尔国际公司 | Conductive paste and heat diffusion material |
| CN101367158A (en) * | 2008-09-24 | 2009-02-18 | 上海大学 | Binary leadless soldering plaster |
| CN103639614A (en) * | 2013-12-04 | 2014-03-19 | 马鑫 | Nanoscale/micron size particle mixing type lead-free solder paste with size effect and manufacturing method thereof |
| US20170365576A1 (en) * | 2014-12-17 | 2017-12-21 | Nippon Steel & Sumikin Materials Co., Ltd. | Bonding wire for semiconductor device |
| CN108526751A (en) * | 2018-04-26 | 2018-09-14 | 深圳市先进连接科技有限公司 | A kind of micro-nano mixing soldering paste and preparation method thereof can be used for pressureless sintering |
| CN110508970A (en) * | 2019-07-15 | 2019-11-29 | 天津大学 | Three peak systems of one kind mixing silver paste and its application |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113492281A (en) * | 2021-05-27 | 2021-10-12 | 中山大学 | Micron silver soldering paste directly sintered on bare copper at low temperature and without pressure, and preparation method and application thereof |
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Application publication date: 20210112 |