CN114799613B - Copper paste and preparation method and application thereof - Google Patents
Copper paste and preparation method and application thereof Download PDFInfo
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- CN114799613B CN114799613B CN202110120640.6A CN202110120640A CN114799613B CN 114799613 B CN114799613 B CN 114799613B CN 202110120640 A CN202110120640 A CN 202110120640A CN 114799613 B CN114799613 B CN 114799613B
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- copper
- paste
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- amine ligand
- complex
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 103
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 94
- 239000010949 copper Substances 0.000 title claims abstract description 94
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- 150000001412 amines Chemical class 0.000 claims abstract description 43
- 239000012691 Cu precursor Substances 0.000 claims abstract description 40
- 239000003446 ligand Substances 0.000 claims abstract description 40
- 238000005476 soldering Methods 0.000 claims abstract description 35
- 238000005245 sintering Methods 0.000 claims abstract description 33
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 13
- 239000003960 organic solvent Substances 0.000 claims abstract description 13
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 239000002245 particle Substances 0.000 claims description 32
- 238000000034 method Methods 0.000 claims description 28
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 24
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 15
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 12
- HFDWIMBEIXDNQS-UHFFFAOYSA-L copper;diformate Chemical compound [Cu+2].[O-]C=O.[O-]C=O HFDWIMBEIXDNQS-UHFFFAOYSA-L 0.000 claims description 9
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- TYFQFVWCELRYAO-UHFFFAOYSA-N suberic acid Chemical compound OC(=O)CCCCCCC(O)=O TYFQFVWCELRYAO-UHFFFAOYSA-N 0.000 claims description 8
- MFEIKQPHQINPRI-UHFFFAOYSA-N 3-Ethylpyridine Chemical compound CCC1=CC=CN=C1 MFEIKQPHQINPRI-UHFFFAOYSA-N 0.000 claims description 6
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 6
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 6
- 239000008103 glucose Substances 0.000 claims description 6
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 238000011946 reduction process Methods 0.000 claims description 6
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 5
- WUOACPNHFRMFPN-SECBINFHSA-N (S)-(-)-alpha-terpineol Chemical compound CC1=CC[C@@H](C(C)(C)O)CC1 WUOACPNHFRMFPN-SECBINFHSA-N 0.000 claims description 4
- RTBFRGCFXZNCOE-UHFFFAOYSA-N 1-methylsulfonylpiperidin-4-one Chemical compound CS(=O)(=O)N1CCC(=O)CC1 RTBFRGCFXZNCOE-UHFFFAOYSA-N 0.000 claims description 4
- 229940058020 2-amino-2-methyl-1-propanol Drugs 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- 239000002211 L-ascorbic acid Substances 0.000 claims description 4
- 235000000069 L-ascorbic acid Nutrition 0.000 claims description 4
- OVKDFILSBMEKLT-UHFFFAOYSA-N alpha-Terpineol Natural products CC(=C)C1(O)CCC(C)=CC1 OVKDFILSBMEKLT-UHFFFAOYSA-N 0.000 claims description 4
- 229940088601 alpha-terpineol Drugs 0.000 claims description 4
- CBTVGIZVANVGBH-UHFFFAOYSA-N aminomethyl propanol Chemical compound CC(C)(N)CO CBTVGIZVANVGBH-UHFFFAOYSA-N 0.000 claims description 4
- JFCQEDHGNNZCLN-UHFFFAOYSA-N anhydrous glutaric acid Natural products OC(=O)CCCC(O)=O JFCQEDHGNNZCLN-UHFFFAOYSA-N 0.000 claims description 4
- 229960005070 ascorbic acid Drugs 0.000 claims description 4
- NNRLDGQZIVUQTE-UHFFFAOYSA-N gamma-Terpineol Chemical compound CC(C)=C1CCC(C)(O)CC1 NNRLDGQZIVUQTE-UHFFFAOYSA-N 0.000 claims description 4
- IOQPZZOEVPZRBK-UHFFFAOYSA-N octan-1-amine Chemical compound CCCCCCCCN IOQPZZOEVPZRBK-UHFFFAOYSA-N 0.000 claims description 4
- BMVXCPBXGZKUPN-UHFFFAOYSA-N 1-hexanamine Chemical compound CCCCCCN BMVXCPBXGZKUPN-UHFFFAOYSA-N 0.000 claims description 3
- 241000208818 Helianthus Species 0.000 claims description 3
- 235000003222 Helianthus annuus Nutrition 0.000 claims description 3
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 3
- AOHJOMMDDJHIJH-UHFFFAOYSA-N propylenediamine Chemical compound CC(N)CN AOHJOMMDDJHIJH-UHFFFAOYSA-N 0.000 claims description 3
- RUJPNZNXGCHGID-UHFFFAOYSA-N (Z)-beta-Terpineol Natural products CC(=C)C1CCC(C)(O)CC1 RUJPNZNXGCHGID-UHFFFAOYSA-N 0.000 claims description 2
- QSNMFWFDOFQASV-UHFFFAOYSA-N 3-Butylpyridine Chemical compound CCCCC1=CC=CN=C1 QSNMFWFDOFQASV-UHFFFAOYSA-N 0.000 claims description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 2
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 2
- 125000003277 amino group Chemical group 0.000 claims description 2
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 claims description 2
- SVOAENZIOKPANY-CVBJKYQLSA-L copper;(z)-octadec-9-enoate Chemical compound [Cu+2].CCCCCCCC\C=C/CCCCCCCC([O-])=O.CCCCCCCC\C=C/CCCCCCCC([O-])=O SVOAENZIOKPANY-CVBJKYQLSA-L 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- QJVXKWHHAMZTBY-GCPOEHJPSA-N syringin Chemical compound COC1=CC(\C=C\CO)=CC(OC)=C1O[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 QJVXKWHHAMZTBY-GCPOEHJPSA-N 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 abstract description 5
- 238000007254 oxidation reaction Methods 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 239000002923 metal particle Substances 0.000 abstract description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 2
- 239000001257 hydrogen Substances 0.000 abstract description 2
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 2
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 239000000758 substrate Substances 0.000 description 72
- 238000012360 testing method Methods 0.000 description 42
- 239000010410 layer Substances 0.000 description 28
- 239000011248 coating agent Substances 0.000 description 22
- 238000000576 coating method Methods 0.000 description 22
- 229910000679 solder Inorganic materials 0.000 description 18
- 238000004806 packaging method and process Methods 0.000 description 17
- 238000001816 cooling Methods 0.000 description 13
- 238000001878 scanning electron micrograph Methods 0.000 description 12
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 10
- 229910052709 silver Inorganic materials 0.000 description 10
- 239000004332 silver Substances 0.000 description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 7
- 239000008367 deionised water Substances 0.000 description 7
- 229910021641 deionized water Inorganic materials 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 239000000919 ceramic Substances 0.000 description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004100 electronic packaging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
Classifications
-
- 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
- B23K35/302—Cu 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
- B23K35/02—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape
- B23K35/0222—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in soldering, brazing
- B23K35/0244—Powders, particles or spheres; Preforms made therefrom
- B23K35/025—Pastes, creams, slurries
-
- 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
- B23K35/36—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
- B23K35/3612—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest with organic compounds as principal constituents
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L24/00—Arrangements for connecting or disconnecting semiconductor or solid-state bodies; Methods or apparatus related thereto
- H01L24/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L24/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
- H01L24/27—Manufacturing methods
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L24/00—Arrangements for connecting or disconnecting semiconductor or solid-state bodies; Methods or apparatus related thereto
- H01L24/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L24/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
- H01L24/28—Structure, shape, material or disposition of the layer connectors prior to the connecting process
- H01L24/29—Structure, shape, material or disposition of the layer connectors prior to the connecting process of an individual layer connector
-
- 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
- H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L2224/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
- H01L2224/27—Manufacturing methods
- H01L2224/271—Manufacture and pre-treatment of the layer connector preform
- H01L2224/2711—Shaping
-
- 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
- H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L2224/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
- H01L2224/28—Structure, shape, material or disposition of the layer connectors prior to the connecting process
- H01L2224/29—Structure, shape, material or disposition of the layer connectors prior to the connecting process of an individual layer connector
- H01L2224/29001—Core members of the layer connector
- H01L2224/29099—Material
- H01L2224/291—Material with a principal constituent of the material being a metal or a metalloid, e.g. boron [B], silicon [Si], germanium [Ge], arsenic [As], antimony [Sb], tellurium [Te] and polonium [Po], and alloys thereof
- H01L2224/29138—Material with a principal constituent of the material being a metal or a metalloid, e.g. boron [B], silicon [Si], germanium [Ge], arsenic [As], antimony [Sb], tellurium [Te] and polonium [Po], and alloys thereof the principal constituent melting at a temperature of greater than or equal to 950°C and less than 1550°C
- H01L2224/29147—Copper [Cu] as principal constituent
Abstract
The invention discloses a copper paste, a preparation method and application thereof, wherein the copper paste comprises the following raw material components: copper powder, a complex of a copper precursor and an amine ligand, an organic solvent carrier and a reducing agent. The complex of the copper precursor and the amine ligand is added into the soldering paste, so that on one hand, hydrogen generated by the decomposition of the complex of the copper precursor and the amine ligand can inhibit oxidation in air to a certain extent, and on the other hand, metal particles generated by the in-situ decomposition of the complex of the copper precursor and the amine ligand are beneficial to sintering and promote interconnection. The copper soldering paste provided by the invention can completely realize the aim of bonding in air, and lower porosity and higher shear strength are obtained.
Description
Technical Field
The invention belongs to the technical field of device packaging, and relates to a copper paste and a preparation method and application thereof.
Background
With the rapid development of technologies such as electric automobiles, aerospace, 5G, high-speed rail, deep well oil and gas exploitation, etc., semiconductor devices with higher power are required, and these devices are required to be capable of operating in more severe environments, and the operating temperature is often greater than 200 ℃. Third generation semiconductor materials typified by SiC and GaN have excellent properties such as a wide band gap, high breakdown, and high thermal conductivity, and can operate at a temperature higher than 500 ℃, and are therefore favored in the field of electronic packaging. The traditional high Pb solder has great harm to human body and environment, the tin-based lead-free solder is not allowed to be redissolved, and the high-melting-point solder such as gold, bismuth and the like has respective defects. There is therefore an urgent need for lead-free interconnect materials in high temperature service to meet these needs. Interconnect materials based on metal particles, such as silver particles and copper particles, are considered to be promising alternatives due to their lower processing temperatures and higher operating temperatures. Silver interconnect structures formed from silver-based sintered materials have very high electrical and thermal conductivities and exhibit good shear strength even in high temperature and thermal shock experiments. But the use of silver is limited due to its high cost and high electromigration. Copper paste is expected to become a substitute for silver paste, copper has conductivity not inferior to silver, lower electron mobility than silver, but copper costs only 1% of the cost of silver, and copper reserves are abundant, and thus is receiving a great deal of attention. However, copper nanoparticles are susceptible to oxidation, greatly reducing their conductivity and shear strength of the interconnect structure. The usual method of suppressing oxidation is sintering under inert gas protection, but this increases the cost greatly. Therefore, it is necessary to develop a copper paste that can be sintered in air to solve the problem that general copper paste is easily oxidized in air and is difficult to sinter.
Disclosure of Invention
In order to solve the above-mentioned problems, the present invention is directed to a copper paste, a preparation method and an application thereof. The copper soldering paste and the bonding process under the air based on the soldering paste can completely realize the purpose of bonding in the air, and obtain lower porosity and higher shear strength.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: in one aspect, the invention provides a copper paste, which comprises the following raw material components: copper powder, a complex of a copper precursor and an amine ligand, an organic solvent carrier and a reducing agent.
Further, the material is prepared from the following raw material components in percentage by mass: 60-85% of copper powder, 5-25% of complex of copper precursor and amine ligand, 5-25% of organic solvent carrier and 1-10% of reducing agent.
Further, the copper powder is one or more of nano copper particles, micron copper particles and micron copper sheets.
Further, the complex of the copper precursor and the amine ligand is prepared by stirring the copper precursor and the amine ligand at room temperature;
preferably, the molar ratio of copper precursor to amine groups in amine ligand is 1:2-1: 4.
further, the copper precursor comprises one or more of copper acetate, copper formate and copper oleate, preferably copper formate;
preferably, the amine ligand comprises one or more of ethylenediamine, propylenediamine, 2-amino-2-methyl-1-propanol, hexylamine, octylamine, sunflower amine, 3-ethylpyridine, 3-butylpyridine.
Further, the organic solvent carrier comprises one or more of ethylene glycol, glycerol, propylene glycol, isopropanol, alpha-terpineol, beta-terpineol and gamma-terpineol.
Further, the reducing agent comprises one or more of L-ascorbic acid, glucose, citric acid, glutaric acid, suberic acid, succinic acid, caproic acid and formaldehyde.
In another aspect, the present invention provides a method for preparing the copper solder paste described in any one of the above, comprising the steps of: copper powder, a complex of a copper precursor and an amine ligand, an organic solvent carrier and a reducing agent are stirred and mixed to prepare the copper soldering paste.
In still another aspect, the present invention provides an application of any one of the copper paste described above in an electronic device package interconnection structure, where the electronic device package interconnection structure includes a first mother sheet, a second mother sheet, and a connection layer for connecting the first mother sheet and the second mother sheet, where the connection layer is formed by sintering the copper paste described above through a sintering process.
Further, the sintering process is an air bonding process, and the air bonding process sequentially comprises a self-reduction process and a bonding process;
preferably, the self-reduction process is to sequentially perform three preheating steps at 60-180 ℃ on a first master sheet coated with any one of the copper soldering paste and a second master sheet coated with any one of the copper soldering paste; more preferably, the self-reduction process comprises a first preheating step set according to the decomposition temperature of the complex of the copper precursor and the amine ligand, a second preheating step set according to the boiling point of the organic solvent carrier and a third preheating step set according to the boiling point of the reducing agent, and preheating for 1-10 min at 60-180 ℃ in sequence;
preferably, the bonding temperature in the bonding process is 150-350 ℃, and the pressing pressure is 0.1-30 MPa.
Further, the first master slice or the second master slice comprises copper, gold and silver slices, or ceramic slices, silicon slices, functional devices and the like coated with copper, gold and silver on the surface layers.
The beneficial effects of the invention are as follows: the copper paste provided by the invention comprises copper powder, a complex of a copper precursor and an amine ligand, a reducing agent and an organic solvent carrier, wherein the complex of the copper precursor and the amine ligand is added into the copper paste, so that on one hand, hydrogen generated by decomposing the complex of the copper precursor and the amine ligand can inhibit oxidation in air to a certain extent, and on the other hand, metal particles generated by in-situ decomposition of the complex of the copper precursor and the amine ligand are beneficial to sintering and promote interconnection. The invention provides an air bonding process based on the soldering paste, which is designed based on the decomposition temperature of a complex of a copper precursor and an amine ligand in copper soldering paste, the boiling point of an organic solvent carrier and the boiling point of a reducing agent, and can realize the self-reduction of copper at low temperature through three preheating steps. The process can be well matched with the prepared copper soldering paste, realizes complete self-reduction of copper at low temperature through multiple steps of preheating, presses the microstructure to densify in the bonding process, reduces high porosity caused by rapid volatilization of the solvent, and inhibits oxidation in the bonding process so as to achieve the aim of bonding under air. The air bonding process provided by the invention has the advantages of simple flow, easiness in realization and contribution to large-scale industrial application. The sintering effect can be well achieved in the air at 150-350 ℃, the interconnection structure with higher shear strength can be obtained after the sintering is completed, the method can be well applied to the field of high-power and high-temperature electronic device packaging, and is particularly applicable to the packaging of third-generation semiconductor devices. According to the method, the pores are filled with copper generated by the decomposition of the complex of the copper precursor and the amine ligand, and the gas release speed is slowed down and the porosity is reduced through a preheating step.
Drawings
FIG. 1 is a schematic view of a copper-clad ceramic substrate in an embodiment of the invention;
FIG. 2 is a schematic diagram of a package interconnect structure in an embodiment of the invention;
FIG. 3 is an SEM image of nano-copper particles used in the present invention;
FIG. 4 is an SEM image of the shear fracture surface of a tie layer of example 1 of the present invention;
FIG. 5 is an SEM image of the shear fracture surface of a tie layer of example 2 of the present invention;
the ceramic substrate 1, the metal coating 2, the first master slice 3, the connecting layer 4 and the second master slice 5.
Detailed Description
For a better understanding of the present invention, the following description will further explain the present invention in conjunction with specific embodiments, but the present invention is not limited to the following examples.
Example 1
Copper formate, 2-amino-2-methyl-1-propanol and octylamine are mixed according to the molar ratio of 1:1:1 is stirred electromagnetically for 20min at room temperature to obtain a complex of the copper precursor and the amine ligand.
The nano copper particles with the particle size of 100nm (the SEM image of the nano copper particles is shown in figure 3), the complex of the copper precursor and the amine ligand, glutaric acid and ethylene glycol are stirred and mixed for 10min in a high-speed mixer, and copper soldering paste is prepared (the glutaric acid and the ethylene glycol are stirred and dissolved for 30min at 60 ℃ in advance), wherein the mass percentages are 75%, 13.5%, 1.5% and 10%, respectively.
The copper paste prepared by the method is applied to a packaging interconnection structure of an electronic device. The schematic structure of the package interconnection structure is shown in fig. 2, and the first master and the second master in the package interconnection structure are selected as DBC substrates, and the schematic structure of the DBC substrates is shown in fig. 1.
First, a master is processed: the DBC substrates (first master and second master) were ultrasonically washed in 5% dilute hydrochloric acid for 30s, rinsed with deionized water and absolute ethanol for 30s, respectively, and finally air dried.
Next, the copper paste prepared in this example was uniformly coated on the connection surface of the DBC substrate.
Next, two DBC substrates (first master and second master) coated with the copper paste were sequentially preheated in air at 110 ℃ for 5min, at 130 ℃ for 5min, and at 160 ℃ for 5min.
Next, the DBC substrates (first master and second master) are stacked on top of each other to obtain a "sandwich" structure of DBC substrate/solder paste coating/DBC substrate.
Then, sintering the stacked structure of the DBC substrate/the soldering paste coating/the DBC substrate in air at the connection temperature of 250 ℃ under the pressure of 10MPa for 15min, sintering the soldering paste coating into a connection layer, and cooling to obtain the packaging interconnection structure shown in fig. 2.
Through testing, the shear force obtained after cooling the connection layer formed by sintering the solder paste of this example was 15.04MPa (wherein 5 test samples were prepared according to this example, and the test data taken as an average of 5 test samples). The SEM image of the shear fracture surface of the connection layer in this embodiment is shown in fig. 4, and it can be seen from the image that the copper particles are well sintered and connected, showing obvious particle growth and sintering neck, having better fracture morphology and better mechanical properties of the interconnection structure.
The shear fracture test for the connection layer is specifically as follows: the sample is fixed on a fixed clamp of a shear force tester, the push head of the tester is pushed and compressed at the speed of 100 mu m/s to carry out a shear fracture test, and the corresponding shear force is obtained through reading in the shear force tester when the sample breaks.
Example 2
Copper formate and propylenediamine were mixed in a molar ratio of 1:2, electromagnetic stirring for 20min at room temperature to obtain the complex of the copper precursor and the amine ligand.
The nano copper particles with the particle size of 100nm (the SEM image of the nano copper particles is shown in figure 3), a complex of a copper precursor and an amine ligand, citric acid and alpha-terpineol are stirred and mixed in a high-speed mixer for 10min, and copper soldering paste is prepared (the citric acid and the alpha-terpineol are stirred and dissolved for 30min at 60 ℃ in advance), wherein the mass percentages are 80%, 12%, 1% and 7%, respectively.
The copper paste prepared by the method is applied to a packaging interconnection structure of an electronic device. The schematic structure of the package interconnection structure is shown in fig. 2, and the first master and the second master in the package interconnection structure are selected as DBC substrates, and the schematic structure of the DBC substrates is shown in fig. 1.
First, a master is processed: the DBC substrates (first master and second master) were ultrasonically washed in 5% dilute hydrochloric acid for 30s, rinsed with deionized water and absolute ethanol for 30s, respectively, and finally air dried.
Next, the copper paste prepared in this example was uniformly coated on the connection surface of the DBC substrate.
Next, two DBC substrates (first master and second master) coated with the copper paste were sequentially preheated at 90 ℃ for 5min, at 110 ℃ for 5min, and at 140 ℃ for 5min under air.
Next, the DBC substrates (first master and second master) are stacked on top of each other to obtain a "sandwich" structure of DBC substrate/solder paste coating/DBC substrate.
Then, sintering the stacked structure of the DBC substrate/the soldering paste coating/the DBC substrate in air at the connection temperature of 250 ℃ under the pressure of 10MPa for 15min, sintering the soldering paste coating into a connection layer, and cooling to obtain the packaging interconnection structure shown in fig. 2.
Through testing, the shear force obtained after the solder paste of this example was sintered to form a connection layer was cooled was 9.66MPa (wherein 5 test samples were prepared according to this example, and the test data taken as an average of 5 test samples). The SEM image of the shear fracture surface of the connection layer in this embodiment is shown in fig. 5, and it can be seen from the image that the copper particles are well sintered and connected, showing obvious particle growth and sintering neck, having better fracture morphology and better mechanical properties of the interconnection structure.
The shear fracture test for the connection layer is specifically as follows: the sample is fixed on a fixed clamp of a shear force tester, the push head of the tester is pushed and compressed at the speed of 100 mu m/s to carry out a shear fracture test, and the corresponding shear force is obtained through reading in the shear force tester when the sample breaks.
Example 3
Copper formate and 3-ethylpyridine were mixed in a molar ratio of 1:2, electromagnetic stirring for 20min at room temperature to obtain the complex of the copper precursor and the amine ligand.
The nano copper particles with the particle size of 100nm (the SEM image of the nano copper particles is shown in figure 3), the complex of the copper precursor and the amine ligand, the caproic acid and the glycerol are stirred and mixed in a high-speed mixer for 10min, and the copper soldering paste is prepared and obtained, wherein the mass percentages of the nano copper particles are respectively 85%, 10%, 1% and 9%.
The copper paste prepared by the method is applied to a packaging interconnection structure of an electronic device. The schematic structure of the package interconnection structure is shown in fig. 2, and the first master and the second master in the package interconnection structure are selected as DBC substrates, and the schematic structure of the DBC substrates is shown in fig. 1.
First, a master is processed: the DBC substrates (first master and second master) were ultrasonically washed in 5% dilute hydrochloric acid for 30s, rinsed with deionized water and absolute ethanol for 30s, respectively, and finally air dried.
Next, the copper paste prepared in this example was uniformly coated on the connection surface of the DBC substrate.
Next, two DBC substrates (first master and second master) coated with the copper paste were sequentially preheated at 85 ℃ for 5min, at 140 ℃ for 5min, and at 160 ℃ for 5min under air.
Next, the DBC substrates (first master and second master) are stacked on top of each other to obtain a "sandwich" structure of DBC substrate/solder paste coating/DBC substrate.
Then, sintering the stacked structure of the DBC substrate/the soldering paste coating/the DBC substrate in air at the connection temperature of 250 ℃ under the pressure of 10MPa for 15min, sintering the soldering paste coating into a connection layer, and cooling to obtain the packaging interconnection structure shown in fig. 2.
Through testing, the shear force obtained after cooling the connection layer formed by sintering the solder paste of this example was 9.78MPa (wherein 5 test samples were prepared according to this example, and the test data taken as an average of 5 test samples).
The shear fracture test for the connection layer is specifically as follows: the sample is fixed on a fixed clamp of a shear force tester, the push head of the tester is pushed and compressed at the speed of 100 mu m/s to carry out a shear fracture test, and the corresponding shear force is obtained through reading in the shear force tester when the sample breaks.
Example 4
Copper acetate and sunflower amine are mixed according to a mole ratio of 1:2, electromagnetic stirring for 20min at room temperature to obtain the complex of the copper precursor and the amine ligand.
The nano copper particles with the particle size of 100nm (the SEM image of the nano copper particles is shown in figure 3), the complex of the copper precursor and the amine ligand, suberic acid and ethylene glycol are stirred and mixed in a high-speed mixer for 10min, and copper soldering paste is prepared (suberic acid and ethylene glycol are stirred and dissolved at 60 ℃ for 30min in advance), wherein the mass percentages are 75%, 14%, 1% and 10%, respectively.
The copper paste prepared by the method is applied to a packaging interconnection structure of an electronic device. The schematic structure of the package interconnection structure is shown in fig. 2, and the first master and the second master in the package interconnection structure are selected as DBC substrates, and the schematic structure of the DBC substrates is shown in fig. 1.
First, a master is processed: the DBC substrates (first master and second master) were ultrasonically washed in 5% dilute hydrochloric acid for 30s, rinsed with deionized water and absolute ethanol for 30s, respectively, and finally air dried.
Next, the copper paste prepared in this example was uniformly coated on the connection surface of the DBC substrate.
Next, two DBC substrates (first master and second master) coated with the copper paste were sequentially preheated for 5min at 110 ℃ under air, 5min at 130 ℃ and 5min at 140 ℃.
Next, the DBC substrates (first master and second master) are stacked on top of each other to obtain a "sandwich" structure of DBC substrate/solder paste coating/DBC substrate.
Then, sintering the stacked structure of the DBC substrate/the soldering paste coating/the DBC substrate in air at the connection temperature of 250 ℃ under the pressure of 10MPa for 15min, sintering the soldering paste coating into a connection layer, and cooling to obtain the packaging interconnection structure shown in fig. 2.
Through testing, the shear force obtained after cooling the connection layer formed by sintering the solder paste of this example was 10.79MPa (wherein 5 test samples were prepared according to this example, and the test data taken as an average of 5 test samples).
The shear fracture test for the connection layer is specifically as follows: the sample is fixed on a fixed clamp of a shear force tester, the push head of the tester is pushed and compressed at the speed of 100 mu m/s to carry out a shear fracture test, and the corresponding shear force is obtained through reading in the shear force tester when the sample breaks.
Example 5
Copper formate and hexylamine are mixed according to a mole ratio of 1:2, electromagnetic stirring for 20min at room temperature to obtain the complex of the copper precursor and the amine ligand.
The nano copper particles with the particle size of 100nm (the SEM image of the nano copper particles is shown in figure 3), the complex of the copper precursor and the amine ligand, glucose and propylene glycol are stirred and mixed in a high-speed mixer for 10min, and copper soldering paste is prepared (the glucose and the propylene glycol are stirred and dissolved at 60 ℃ for 30min in advance), wherein the mass percentages are respectively 70%, 18%, 2.5% and 9.5%.
The copper paste prepared by the method is applied to a packaging interconnection structure of an electronic device. The schematic structure of the package interconnection structure is shown in fig. 2, and the first master and the second master in the package interconnection structure are selected as DBC substrates, and the schematic structure of the DBC substrates is shown in fig. 1.
First, a master is processed: the DBC substrates (first master and second master) were ultrasonically washed in 5% dilute hydrochloric acid for 30s, rinsed with deionized water and absolute ethanol for 30s, respectively, and finally air dried.
Next, the copper paste prepared in this example was uniformly coated on the connection surface of the DBC substrate.
Next, two DBC substrates (first master and second master) coated with the copper paste were sequentially preheated at 100 ℃ for 5min,130 ℃ for 5min, and 160 ℃ for 5min under air.
Next, the DBC substrates (first master and second master) are stacked on top of each other to obtain a "sandwich" structure of DBC substrate/solder paste coating/DBC substrate.
Then, sintering the stacked structure of the DBC substrate/the soldering paste coating/the DBC substrate in air at the connection temperature of 250 ℃ under the pressure of 10MPa for 15min, sintering the soldering paste coating into a connection layer, and cooling to obtain the packaging interconnection structure shown in fig. 2.
Through testing, the shear force obtained after cooling the connection layer formed by sintering the solder paste of this example was 13.45MPa (wherein 5 test samples were prepared according to this example, and the test data taken as an average of 5 test samples).
The shear fracture test for the connection layer is specifically as follows: the sample is fixed on a fixed clamp of a shear force tester, the push head of the tester is pushed and compressed at the speed of 100 mu m/s to carry out a shear fracture test, and the corresponding shear force is obtained through reading in the shear force tester when the sample breaks.
Example 6
Copper formate and octylamine are mixed according to a mole ratio of 1:2, electromagnetic stirring for 20min at room temperature to obtain the complex of the copper precursor and the amine ligand.
The nano copper particles with the particle size of 100nm (the SEM image of the nano copper particles is shown in figure 3), the complex of the copper precursor and the amine ligand, the L-ascorbic acid and the ethylene glycol are stirred and mixed in a high-speed mixer for 10min, and copper soldering paste is prepared (the L-ascorbic acid and the ethylene glycol are stirred and dissolved at 60 ℃ for 30min in advance), wherein the mass percentages are 75%, 14%, 1% and 10%, respectively.
The copper paste prepared by the method is applied to a packaging interconnection structure of an electronic device. The schematic structure of the package interconnection structure is shown in fig. 2, and the first master and the second master in the package interconnection structure are selected as DBC substrates, and the schematic structure of the DBC substrates is shown in fig. 1.
First, a master is processed: the DBC substrates (first master and second master) were ultrasonically washed in 5% dilute hydrochloric acid for 30s, rinsed with deionized water and absolute ethanol for 30s, respectively, and finally air dried.
Next, the copper paste prepared in this example was uniformly coated on the connection surface of the DBC substrate.
Next, two DBC substrates (first master and second master) coated with the copper paste were sequentially preheated at 100 ℃ for 5min,130 ℃ for 5min, and 150 ℃ for 5min under air.
Next, the DBC substrates (first master and second master) are stacked on top of each other to obtain a "sandwich" structure of DBC substrate/solder paste coating/DBC substrate.
Then, sintering the stacked structure of the DBC substrate/the soldering paste coating/the DBC substrate in air at the connecting temperature of 275 ℃ under the pressure of 10MPa for 15min, sintering the soldering paste coating into a connecting layer, and cooling to obtain the packaging interconnection structure shown in fig. 2.
Through testing, the shear force obtained after cooling the connection layer formed by sintering the solder paste of this example was 14.53MPa (wherein 5 test samples were prepared according to this example, and the test data taken as an average of 5 test samples).
The shear fracture test for the connection layer is specifically as follows: the sample is fixed on a fixed clamp of a shear force tester, the push head of the tester is pushed and compressed at the speed of 100 mu m/s to carry out a shear fracture test, and the corresponding shear force is obtained through reading in the shear force tester when the sample breaks.
Example 7
Copper formate and 2-amino-2-methyl-1-propanol were mixed in a molar ratio of 1:2, electromagnetic stirring for 20min at room temperature to obtain the complex of the copper precursor and the amine ligand.
The nano copper particles with the particle size of 100nm (the SEM image of the nano copper particles is shown in figure 3), the complex of the copper precursor and the amine ligand, glucose and glycerol are stirred and mixed in a high-speed mixer for 10min, and copper soldering paste is prepared (glucose and glycerol are stirred and dissolved at 60 ℃ for 30min in advance), wherein the mass percentages are 75%, 15%, 1.5% and 8.5% respectively.
The copper paste prepared by the method is applied to a packaging interconnection structure of an electronic device. The schematic structure of the package interconnection structure is shown in fig. 2, and the first master and the second master in the package interconnection structure are selected as DBC substrates, and the schematic structure of the DBC substrates is shown in fig. 1.
First, a master is processed: the DBC substrates (first master and second master) were ultrasonically washed in 5% dilute hydrochloric acid for 30s, rinsed with deionized water and absolute ethanol for 30s, respectively, and finally air dried.
Next, the copper paste prepared in this example was uniformly coated on the connection surface of the DBC substrate.
Next, two DBC substrates (first master and second master) coated with the copper paste were sequentially preheated at 110 ℃ for 5min,140 ℃ for 5min, and 160 ℃ for 5min under air.
Next, the DBC substrates (first master and second master) are stacked on top of each other to obtain a "sandwich" structure of DBC substrate/solder paste coating/DBC substrate.
Then, sintering the stacked structure of the DBC substrate/the soldering paste coating/the DBC substrate in air at the connection temperature of 250 ℃ under the pressure of 10MPa for 15min, sintering the soldering paste coating into a connection layer, and cooling to obtain the packaging interconnection structure shown in fig. 2.
Through testing, the shear force obtained after cooling the connection layer formed by sintering the solder paste of this example was 11.24MPa (wherein 5 test samples were prepared according to this example, and the test data taken as an average of 5 test samples).
The shear fracture test for the connection layer is specifically as follows: the sample is fixed on a fixed clamp of a shear force tester, the push head of the tester is pushed and compressed at the speed of 100 mu m/s to carry out a shear fracture test, and the corresponding shear force is obtained through reading in the shear force tester when the sample breaks.
The embodiments described above are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the embodiments described above, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principles of the present invention should be made in the equivalent manner, and are included in the scope of the present invention.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.
Claims (7)
1. The copper paste is characterized by comprising the following raw material components: copper powder, complex of copper precursor and amine ligand, organic solvent carrier and reducer;
the material is prepared from the following raw material components in percentage by mass: 60-85% of copper powder, 5-25% of complex of copper precursor and amine ligand, 5-25% of organic solvent carrier and 1-10% of reducing agent; the complex of the copper precursor and the amine ligand is prepared by stirring the copper precursor and the amine ligand at room temperature; the molar ratio of the copper precursor to amine groups in the amine ligand is 1:2-1:4, a step of; the preparation method of the copper soldering paste comprises the following steps: copper powder, a complex of a copper precursor and an amine ligand, an organic solvent carrier and a reducing agent are stirred and mixed to prepare the copper soldering paste.
2. The copper paste of claim 1, wherein the copper powder is one or more of nano copper particles, micro copper flakes.
3. The copper paste of claim 1, wherein the copper precursor comprises one or more of copper acetate, copper formate, copper oleate; the amine ligand comprises one or more of ethylenediamine, propylenediamine, 2-amino-2-methyl-1-propanol, hexylamine, octylamine, sunflower amine, 3-ethylpyridine and 3-butylpyridine.
4. The copper paste of claim 1, wherein the organic solvent carrier comprises one or more of ethylene glycol, glycerol, propylene glycol, isopropanol, α -terpineol, β -terpineol, γ -terpineol.
5. The copper paste according to claim 1, wherein the reducing agent comprises one or more of L-ascorbic acid, glucose, citric acid, glutaric acid, suberic acid, succinic acid, caproic acid, formaldehyde.
6. Use of the copper paste according to any one of claims 1 to 5 in an electronic device package interconnect structure comprising a first master, a second master and a connection layer for connecting the first master and the second master, the connection layer being formed by sintering using the copper paste by a sintering process.
7. The use according to claim 6, wherein the sintering process is an air bonding process comprising a self-reduction process followed by a bonding process; the self-reduction process comprises the steps of sequentially carrying out three preheating steps on a first master slice coated with the copper soldering paste and a second master slice coated with the copper soldering paste at 60-180 ℃; the self-reduction process comprises a first preheating step set according to the decomposition temperature of a complex of a copper precursor and an amine ligand, a second preheating step set according to the boiling point of an organic solvent carrier and a third preheating step set according to the boiling point of a reducing agent, and preheating for 1-10 min at 60-180 ℃ in sequence; the bonding temperature in the bonding process is 150-350 ℃, and the pressing pressure is 0.1-30 MPa.
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| CN116825742B (en) * | 2023-08-28 | 2023-11-03 | 合肥阿基米德电子科技有限公司 | Preformed soldering lug, and preparation method and application thereof |
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