CN109926577B - Copper paste capable of being sintered at low temperature and high density - Google Patents
Copper paste capable of being sintered at low temperature and high density Download PDFInfo
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- CN109926577B CN109926577B CN201910366417.2A CN201910366417A CN109926577B CN 109926577 B CN109926577 B CN 109926577B CN 201910366417 A CN201910366417 A CN 201910366417A CN 109926577 B CN109926577 B CN 109926577B
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- copper
- particles
- copper paste
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- 239000010949 copper Substances 0.000 title claims abstract description 101
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 100
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 100
- 239000002245 particle Substances 0.000 claims abstract description 64
- 238000005245 sintering Methods 0.000 claims abstract description 37
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229910052738 indium Inorganic materials 0.000 claims abstract description 33
- 239000011347 resin Substances 0.000 claims abstract description 19
- 229920005989 resin Polymers 0.000 claims abstract description 19
- 229910000765 intermetallic Inorganic materials 0.000 claims description 8
- 230000003647 oxidation Effects 0.000 claims description 8
- 238000007254 oxidation reaction Methods 0.000 claims description 8
- 238000002844 melting Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
- 239000004593 Epoxy Substances 0.000 claims 1
- 238000009766 low-temperature sintering Methods 0.000 abstract description 3
- 239000002905 metal composite material Substances 0.000 abstract description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 19
- 239000002184 metal Substances 0.000 description 13
- 229910052751 metal Inorganic materials 0.000 description 13
- 229910052709 silver Inorganic materials 0.000 description 8
- 239000004332 silver Substances 0.000 description 8
- 230000009467 reduction Effects 0.000 description 7
- 238000000034 method Methods 0.000 description 5
- 239000011148 porous material Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000002923 metal particle Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000005034 decoration Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001879 copper Chemical class 0.000 description 1
- HVMJUDPAXRRVQO-UHFFFAOYSA-N copper indium Chemical compound [Cu].[In] HVMJUDPAXRRVQO-UHFFFAOYSA-N 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
Images
Classifications
-
- 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
-
- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
Landscapes
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Powder Metallurgy (AREA)
- Conductive Materials (AREA)
Abstract
The invention relates to the field of metal composite materials, in particular to copper paste which can be used for low-temperature sintering and can obtain low porosity. The copper paste comprises: spherical copper particles, flake indium particles and high-linking resin; the proportion of the two copper particles is more than 80 percent, the proportion of the indium particles is between 10 and 20 percent, and the proportion of the high-linking resin is between 0 and 10 percent. Under the non-pressure condition, the sintering temperature of the copper paste can be as low as about 180 ℃ and 250 ℃, and the density of the sintered copper paste can reach more than 95%.
Description
Technical Field
The application relates to the field of metal composite materials, in particular to preparation of copper paste for low-temperature low-pressure sintering.
Background
New generation power modules for trolley, aviation, and other industries require high power and high service temperatures. Wide bandgap semiconductors have proven over the last 10 years to be able to withstand high operating temperatures above 300 ℃. However, conventional packaging materials, such as tin-based solder and conductive paste, are limited to operating below 200 ℃. Researchers have been looking for various ways to achieve high reliability at high temperatures and high power. In the past exploration, sintering of highly conductive and electrically conductive silver or copper in metals has been found to be a promising approach. For cost reasons, sintering copper is a technology that has been tried in recent years instead of sintering silver. The relatively high sintering temperature of sintered copper is still plagued the semiconductor packaging industry. Copper has a higher surface energy than silver, but is more easily oxidized, and thus generates an oxide having a lower surface energy, which is less soluble, on the surface. At present, most of nano copper particles are mainly spherical, and some nano copper particles are difficult to achieve mutual melting and sintering even below 30 nanometers, the main problem is that the problem of oxidation of the copper surface exists all the time, and with the further reduction of the size of the copper particles, the copper surface energy is increased, the mutual diffusion opportunity of metal atoms is increased, but the oxidation tendency is more aggravated, so that the reduction of the copper sintering temperature faces a great challenge. Also, sintering porosity is a concern because porosity reduces thermal conductivity and reliability of the sintered joint.
The document "Development of Die Attachment Technology for Power IC Module Integrated inside Integrated Nano-Silver Joint", 2017 IEEE 67th Electronic Component and Technology Conference describes: the indium foil added In the silver sintering material can reduce the oxidation of a copper matrix In use and service, and the reliability of the device is greatly improved, possibly because of the barrier of a Cu-In intermetallic compound. Meanwhile, the indium with low melting point melts at 156 ℃, and is filled between the pores to help improve the compactness of the sintered body. The low-melting-point indium can further promote the reduction of bonding forming temperature, and the all Cu-In intermetallic compound formed by the micro-particle copper and the indium has high melting point, can meet the requirement of high service temperature of a sintering body bonding point, and has good reliability.
In fact, the conductive silver paste in the industry uses plate-like silver powder as a filler, because the silver powders are in surface contact with each other when conducting electricity, and therefore, the plate-like silver powder has much lower electrical resistance than the spherical silver powder due to point contact. Therefore, the silver flake powder is used, so that the using amount of the silver powder can be saved, the thickness of a coating can be reduced, and the miniaturization of electronic components is facilitated; in addition, when the plate-like silver powder and the spherical silver powder are mixed, the spherical silver powder is overlapped between the plate-like silver powders, and the silver content per unit area can be increased, thereby further reducing the resistivity and improving the conductivity. In US9875983B2, granted in 2018, the indai company proposed a collocation of two sizes, size-limited N-type (1-100nm) and M-type (0.1-1000 μ M), for theoretical calculations of pressureless sintered nanocrystals. They have experimentally demonstrated that particles of three shapes, sphere, tablet, and rod: the plate-like particles can provide maximum packing rate, thermal and electrical conductivity and shear force.
The preparation method of the flake copper powder mainly comprises a mechanical ball milling method, a solution reduction method, an ultrasonic auxiliary method and the like. The solution reduction method is one of the most potential preparation methods commonly used at present due to simple operation, low equipment requirement, high purity of the flake silver powder and good performance. Patent CN107405691A provides a solution reduction method with easy control of the shape and size of copper particles.
At present, the copper paste is mostly prepared from single spherical particles. The following patents relate to the formulation of more than one (copper) metal particle: CN106457383A of the american alpha corporation, defines a situation where two types of metal particles are collocated as a low pressure sintered powder, which limits the size and specific gravity of the two types of particles to a certain range, and is also collocated with a plurality of capping agents. However, the large particles are a minority. Another Intrinsiqu patent application US2014/0287158A directed only to copper particles proposes: the mixture with copper flakes has an average diameter between 1.0-8.0 microns and the nano-copper particles have an average diameter from 10 nanometers to 100 nanometers, wherein the ratio of copper flakes to nano-particles is between 2:1 and 5:1 weight percent.
Disclosure of Invention
In order to solve the above problems, the present invention proposes a copper paste doped with metallic indium particles and resin having a particular particle shape for the purpose of low temperature sintering with low porosity.
The invention provides a copper paste with low sintering temperature and low porosity, which comprises the following components in part by weight: spherical copper particles, flake indium particles and high-linking resin; in the metal particles, two copper particles account for more than 80 percent of the total weight, indium particles account for 1 to 20 percent of the total weight, and the high-linking resin with the curing temperature of 170 to 200 ℃ accounts for 0 to 10 percent of the total weight.
Preferably, the proportion of the indium particles is adjusted according to the requirements on the heat conducting property and the sintering temperature. The high indium content is advantageous for lowering the sintering temperature, but at the same time there is a risk of lowering the thermal conductivity of the sintered body.
Preferably, the sintering temperature of the copper paste is about 200 ℃, and the compactness is more than 98%.
The copper paste provided by the invention has the advantages that the surface area is increased through the special design of the flake size of the copper particles, so that the purpose of low-temperature sintering is achieved, meanwhile, the flake and spherical copper particles are mixed to play a role in synthesizing surface energy and reducing the problem of deposition, and the spherical copper particles also play a role in filling pores, so that the density of a sintered body is further increased. The gaps are filled by the low-melting-point (156 ℃) indium particles, the heat conduction and the reliability are improved, most of fused indium metal can form high-melting-point copper and indium intermetallic compounds (Cu7In3 and the like) after contacting with copper, the fused indium metal and the sintered copper share high service temperature, meanwhile, the indium metal with low ionization energy can reduce the oxidation risk of the copper and further reduce the sintering temperature, and the flaky copper particles and the flaky indium particles are well fused, so that the protection of the copper by the indium is enhanced. In addition, the copper paste of the present invention incorporates a high-linking resin which shrinks after curing to achieve pressurization and further lower the sintering temperature. The copper paste can be sintered at low temperature under no pressure, has a density of over 95 percent, and can be compared favorably with sintered silver paste.
Drawings
FIG. 1 is a schematic view showing the structure of a copper paste according to the present invention;
FIG. 2 is a schematic view showing the internal structure of the copper paste according to the present invention during use;
FIG. 3 is a schematic view showing the internal structure of the copper paste of the present invention after sintering.
1-flaky copper particles; 2-spherical copper particles; 3-flaky indium particles; 4-high chain linking resin; 5-Cu-In intermetallic compound.
Detailed Description
In order that the objects, features and advantages of the invention will be more clearly understood, a more particular description of the invention will be rendered by reference to the appended drawings, in which numerous specific details are set forth in order to provide a thorough understanding of the invention, but the invention can be practiced in many ways other than as described. Accordingly, the invention is not limited by the specific implementations disclosed below.
In order to reduce the temperature of copper sintering, while reducing the sintering porosity, the present invention prepares copper pastes with two objectives in particular: 1) realizing pressureless and low-temperature copper sintering; 2) a low porosity sintered body is obtained. To achieve the first objective, the present invention primarily focuses on increasing copper surface area and reducing copper surface oxidation. The surface areas of different shapes are different, spherical and flake are two extreme examples of the surface area of an object with the same volume, flake has very large surface area and thus very large surface energy, and sphere is the reverse; therefore, in order to increase the surface area and increase the surface energy to lower the sintering temperature, the flaky copper particles serve as the main body of the copper paste and the spherical copper particles serve as auxiliary filling gaps and reduce particle deposition; the oxidation tendency of the copper is increased due to the increase of the surface area of the copper, and the invention adds another metal element, namely indium, with low melting point and low ionization energy, and also adds the metal element in the form of flaky particles to enhance the surface energy and improve the activity of the metal element, thereby effectively reducing the oxidation of the copper. In addition, in order to further improve the sintering efficiency and the compactness, a small amount of high-chain polymer is properly added into the copper paste, and the optimized effect is achieved by means of the pressure applied to the whole composite material during sintering caused by the curing shrinkage of the polymer. Specifically, as shown in fig. 1, the paste of the copper paste with low sintering temperature and low porosity of the present invention comprises: the main component of the paste is copper particles, and the paste comprises flaky copper particles 1 and spherical copper particles 2, wherein the diameter of the spherical copper particles 2 is less than 500 nm; also included are flake indium particles 3, and a high-link resin 4 (such as an epoxy resin or the like). The flake-like copper particles 1 and flake-like indium particles 3 have a size length of between 1 μm and 10 μm and a thickness of < 0.5. mu.m. The content of the high-chain resin 4 is between 0 and 10 percent. The metal content in the paste is more than 90%, wherein the copper content is more than 80%, and the indium content is 10-20%, the filling amount of the flaky indium particles can be adjusted according to the requirement on the heat-conducting performance temperature, when the copper content is increased and the indium content is reduced, the overall heat-conducting performance is improved, but the sintering temperature can also be increased.
When the internal condition of the copper paste body is used is shown in fig. 2, copper indium particles are fused with each other, and the suspension durability of the particles is improved due to the existence of the resin, so that the copper paste body can stay for a long time between the application step and the sintering step. In addition, a certain overall pressure is applied due to the shrinkage force after the resin is cured, the density is enhanced, the sintering efficiency is improved, the sintering temperature of the paste can be as low as 180 ℃ and 250 ℃ under the condition of no pressure, and the density can reach more than 95%. The sintered dot body thus formed is a crosslinked body In which copper atoms are interdiffused and fused, and the gap thereof is filled with a Cu — In intermetallic compound having a high melting point (as shown In fig. 3).
The invention adopts several measures to reduce the copper sintering temperature and porosity: 1) spherical copper particles are still maintained, and flaky copper particles are introduced, because the flaky particles are in the form with the highest surface area in all shapes, the intersolubility among metals is increased, the sintering temperature is reduced, and meanwhile, the filling rate of the copper particles is increased; 2) flaky metal indium particles with low ionization energy are introduced, and the flaky particles are guaranteed to be well contacted and wrapped with copper particles, so that the oxidation of the copper surface in use and service is reduced, and the interaction of metal at high temperature is enhanced; 3) the reduction of the sintering porosity is also achieved by the filling of low-melting-point metal indium, because most of the indium flows into pores after being fused at 156 ℃ to form high-melting-point intermetallic compounds with copper, and the high-melting-point intermetallic compounds and the sintered copper share the task of high service temperature; 4) introducing a small amount of high-chain resin, curing at 170-200 ℃, wherein the high-chain reaction of the resin can cause the whole body to shrink, so as to provide a certain internal pressure effect; it is known that under the condition of pressure, the sintering temperature can be reduced and the density can be improved; in addition, the resin will promote particle suspension dispersion; 5) the pores can block heat conduction, and meanwhile, the copper paste is also a place with concentrated stress, and the copper paste can be sintered at low temperature to form a high-density sintering point, so that high reliability and high heat conductivity are achieved; in addition, the paste has a long shelf life and a long working residence time due to the addition of indium and resin.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (5)
1. A copper paste comprising: copper particles and indium particles, wherein the copper particles account for more than 80 percent of the total weight percentage, the indium particles account for 10-20 percent of the total weight percentage, and the copper particles comprise spherical copper particles and flaky copper particles; the copper paste comprises high-chain resin accounting for 0-10%; the length of the flaky copper particles and the flaky indium particles is 1-10 mu m, and the thickness of the flaky copper particles and the flaky indium particles is less than 0.5 um; the sintering temperature of the copper paste is 200-250 ℃, and the density of the copper paste after sintering is more than 95%; the sintered body after the copper paste is sintered forms a Cu-In intermetallic compound with a high melting point so as to improve the service temperature and reduce the oxidation In service.
2. The copper paste according to claim 1, wherein the high-chain resin is an epoxy-based resin.
3. The copper paste according to claim 1, wherein the curing temperature of the high-chain resin is 170 to 200 ℃.
4. The copper paste of claim 1, wherein the proportion of indium particles is adjustable according to the requirements of thermal conductivity and sintering temperature.
5. The copper paste according to claim 1 or 2, wherein the copper paste is used for preparing a low-temperature sintered copper film.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910366417.2A CN109926577B (en) | 2019-05-05 | 2019-05-05 | Copper paste capable of being sintered at low temperature and high density |
| PCT/CN2019/123818 WO2020224257A1 (en) | 2019-05-05 | 2019-12-06 | Copper paste sinterable at low temperature and high density |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910366417.2A CN109926577B (en) | 2019-05-05 | 2019-05-05 | Copper paste capable of being sintered at low temperature and high density |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109926577A CN109926577A (en) | 2019-06-25 |
| CN109926577B true CN109926577B (en) | 2020-11-17 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201910366417.2A Expired - Fee Related CN109926577B (en) | 2019-05-05 | 2019-05-05 | Copper paste capable of being sintered at low temperature and high density |
Country Status (2)
| Country | Link |
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| CN (1) | CN109926577B (en) |
| WO (1) | WO2020224257A1 (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109926577B (en) * | 2019-05-05 | 2020-11-17 | 深圳第三代半导体研究院 | Copper paste capable of being sintered at low temperature and high density |
| CN110773908A (en) * | 2019-10-28 | 2020-02-11 | 深圳第三代半导体研究院 | Preparation method and sintering method of low-temperature sintered indium-doped nano-silver sintering paste |
| CN112926171B (en) * | 2019-12-05 | 2024-05-31 | 中国有研科技集团有限公司 | Implementation method for nano copper powder sintered compact density theoretical deduction |
| CN111942726B (en) * | 2020-06-29 | 2022-04-19 | 深圳第三代半导体研究院 | Sintering process |
| CN114199055B (en) * | 2020-08-28 | 2024-04-09 | 广州力及热管理科技有限公司 | Sheet metal element having a cured composite structure and method for producing the same |
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| CN1273423A (en) * | 1999-05-10 | 2000-11-15 | 松下电器产业株式会社 | Electgrode for PTC thermister and manufacture method thereof and PTC thermistor |
| CN101146644A (en) * | 2005-04-01 | 2008-03-19 | 旭化成电子材料元件株式会社 | Conductive filler and solder material |
| CN101295739A (en) * | 2007-04-26 | 2008-10-29 | 比亚迪股份有限公司 | Conductive slurry for solar battery front side electrode and production method thereof |
| CN103021512A (en) * | 2011-09-21 | 2013-04-03 | 三星电机株式会社 | Conductive paste composition for low temperature firing |
| JP5656380B2 (en) * | 2008-09-30 | 2015-01-21 | 三菱マテリアル株式会社 | Conductive ink composition, solar cell using the composition, and method for producing solar cell module |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4197110B2 (en) * | 2001-08-07 | 2008-12-17 | 三井金属鉱業株式会社 | Mixed copper powder, method for producing the mixed copper powder, copper paste using the mixed copper powder, and printed wiring board using the copper paste |
| JP4158713B2 (en) * | 2004-02-03 | 2008-10-01 | 住友金属鉱山株式会社 | Copper paste composition for external electrodes |
| JP5858201B1 (en) * | 2014-06-25 | 2016-02-10 | 住友金属鉱山株式会社 | Copper powder and copper paste, conductive paint, conductive sheet using the same |
| JP6473223B2 (en) * | 2015-03-05 | 2019-02-20 | 国立大学法人大阪大学 | Method for producing copper particles |
| CN109926577B (en) * | 2019-05-05 | 2020-11-17 | 深圳第三代半导体研究院 | Copper paste capable of being sintered at low temperature and high density |
-
2019
- 2019-05-05 CN CN201910366417.2A patent/CN109926577B/en not_active Expired - Fee Related
- 2019-12-06 WO PCT/CN2019/123818 patent/WO2020224257A1/en active Application Filing
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1273423A (en) * | 1999-05-10 | 2000-11-15 | 松下电器产业株式会社 | Electgrode for PTC thermister and manufacture method thereof and PTC thermistor |
| CN101146644A (en) * | 2005-04-01 | 2008-03-19 | 旭化成电子材料元件株式会社 | Conductive filler and solder material |
| CN101295739A (en) * | 2007-04-26 | 2008-10-29 | 比亚迪股份有限公司 | Conductive slurry for solar battery front side electrode and production method thereof |
| JP5656380B2 (en) * | 2008-09-30 | 2015-01-21 | 三菱マテリアル株式会社 | Conductive ink composition, solar cell using the composition, and method for producing solar cell module |
| CN103021512A (en) * | 2011-09-21 | 2013-04-03 | 三星电机株式会社 | Conductive paste composition for low temperature firing |
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| Publication number | Publication date |
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| CN109926577A (en) | 2019-06-25 |
| WO2020224257A1 (en) | 2020-11-12 |
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