CN116652447A - Preparation method of copper-based solder paste for one-step bonding and bonding method thereof - Google Patents
Preparation method of copper-based solder paste for one-step bonding and bonding method thereof Download PDFInfo
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- CN116652447A CN116652447A CN202210147647.1A CN202210147647A CN116652447A CN 116652447 A CN116652447 A CN 116652447A CN 202210147647 A CN202210147647 A CN 202210147647A CN 116652447 A CN116652447 A CN 116652447A
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- copper
- bonding
- soldering paste
- sintering
- solder paste
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 49
- 239000010949 copper Substances 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 229910000679 solder Inorganic materials 0.000 title claims description 23
- 239000000758 substrate Substances 0.000 claims abstract description 33
- 238000005476 soldering Methods 0.000 claims abstract description 30
- 239000003960 organic solvent Substances 0.000 claims abstract description 11
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 238000005245 sintering Methods 0.000 claims description 24
- 239000011248 coating agent Substances 0.000 claims description 10
- 238000000576 coating method Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 9
- 229910052709 silver Inorganic materials 0.000 claims description 9
- 239000004332 silver Substances 0.000 claims description 9
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 8
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 6
- 229910052737 gold Inorganic materials 0.000 claims description 6
- 239000010931 gold Substances 0.000 claims description 6
- 239000000919 ceramic Substances 0.000 claims description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 claims description 4
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims description 4
- KBPLFHHGFOOTCA-UHFFFAOYSA-N caprylic alcohol Natural products CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 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
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 claims description 4
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 claims description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 4
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Natural products OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 3
- OVKDFILSBMEKLT-UHFFFAOYSA-N alpha-Terpineol Natural products CC(=C)C1(O)CCC(C)=CC1 OVKDFILSBMEKLT-UHFFFAOYSA-N 0.000 claims description 3
- 229940088601 alpha-terpineol Drugs 0.000 claims description 3
- 229960005070 ascorbic acid Drugs 0.000 claims description 3
- 235000010323 ascorbic acid Nutrition 0.000 claims description 3
- 239000011668 ascorbic acid Substances 0.000 claims description 3
- TYQCGQRIZGCHNB-JLAZNSOCSA-N l-ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(O)=C(O)C1=O TYQCGQRIZGCHNB-JLAZNSOCSA-N 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- JLGLQAWTXXGVEM-UHFFFAOYSA-N triethylene glycol monomethyl ether Chemical compound COCCOCCOCCO JLGLQAWTXXGVEM-UHFFFAOYSA-N 0.000 claims description 3
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 2
- RUJPNZNXGCHGID-UHFFFAOYSA-N (Z)-beta-Terpineol Natural products CC(=C)C1CCC(C)(O)CC1 RUJPNZNXGCHGID-UHFFFAOYSA-N 0.000 claims description 2
- COBPKKZHLDDMTB-UHFFFAOYSA-N 2-[2-(2-butoxyethoxy)ethoxy]ethanol Chemical compound CCCCOCCOCCOCCO COBPKKZHLDDMTB-UHFFFAOYSA-N 0.000 claims description 2
- SGQLKNKVOZVAAY-UHFFFAOYSA-N 2-[2-(2-butoxyethoxy)ethoxy]ethyl acetate Chemical compound CCCCOCCOCCOCCOC(C)=O SGQLKNKVOZVAAY-UHFFFAOYSA-N 0.000 claims description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 2
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 2
- 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 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- -1 alcohol ethers Chemical class 0.000 claims description 2
- 150000001298 alcohols Chemical class 0.000 claims description 2
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 claims description 2
- 150000001408 amides Chemical class 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- 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 2
- 150000002148 esters Chemical class 0.000 claims description 2
- 235000019253 formic acid Nutrition 0.000 claims description 2
- 239000008103 glucose Substances 0.000 claims description 2
- 229940093915 gynecological organic acid Drugs 0.000 claims description 2
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 2
- 150000002576 ketones Chemical class 0.000 claims description 2
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 2
- 150000007524 organic acids Chemical class 0.000 claims description 2
- 235000005985 organic acids Nutrition 0.000 claims description 2
- MOOYVEVEDVVKGD-UHFFFAOYSA-N oxaldehydic acid;hydrate Chemical compound O.OC(=O)C=O MOOYVEVEDVVKGD-UHFFFAOYSA-N 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- 239000012279 sodium borohydride Substances 0.000 claims description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 2
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 2
- 239000002344 surface layer Substances 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
- YFNKIDBQEZZDLK-UHFFFAOYSA-N triglyme Chemical compound COCCOCCOCCOC YFNKIDBQEZZDLK-UHFFFAOYSA-N 0.000 claims description 2
- 238000007605 air drying Methods 0.000 claims 1
- ALKZAGKDWUSJED-UHFFFAOYSA-N dinuclear copper ion Chemical compound [Cu].[Cu] ALKZAGKDWUSJED-UHFFFAOYSA-N 0.000 abstract description 8
- 238000004806 packaging method and process Methods 0.000 abstract description 4
- 238000004100 electronic packaging Methods 0.000 abstract description 3
- 238000009835 boiling Methods 0.000 abstract description 2
- 238000004377 microelectronic Methods 0.000 abstract description 2
- 230000001681 protective effect Effects 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 14
- 238000012360 testing method Methods 0.000 description 7
- 238000001816 cooling Methods 0.000 description 6
- 239000002105 nanoparticle Substances 0.000 description 6
- 238000001878 scanning electron micrograph Methods 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 239000011247 coating layer Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000007731 hot pressing Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- WUOACPNHFRMFPN-SECBINFHSA-N (S)-(-)-alpha-terpineol Chemical compound CC1=CC[C@@H](C(C)(C)O)CC1 WUOACPNHFRMFPN-SECBINFHSA-N 0.000 description 2
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 2
- 239000005751 Copper oxide Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229910000431 copper oxide Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 235000011187 glycerol Nutrition 0.000 description 2
- 238000009766 low-temperature sintering Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000013459 approach Methods 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229940116411 terpineol Drugs 0.000 description 1
- 230000000930 thermomechanical effect Effects 0.000 description 1
- 238000005406 washing Methods 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
- B23K35/40—Making wire or rods for soldering or welding
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Electric Connection Of Electric Components To Printed Circuits (AREA)
Abstract
The invention discloses a preparation method of copper-based soldering paste for one-step bonding and a bonding method thereof, belonging to the technical field of electronic packaging. The invention provides a preparation method of copper-based soldering paste for one-step bonding, which comprises the steps of stirring and mixing 60% -85% of copper powder, 5% -35% of organic solvent carrier and 0% -10% of reducing agent according to mass percentage, so as to obtain the copper-based soldering paste, wherein the copper-based soldering paste has excellent mechanical properties and is very suitable for interconnection of high-temperature power devices in microelectronic packaging. Based on the size of copper powder in the copper-based soldering paste and the boiling point of the organic solvent, the invention also provides a one-step bonding process, and reliable copper-copper joints can be formed between substrates through one-step bonding by external pressure without the processes of external protective gas, preheating and the like.
Description
Technical Field
The invention belongs to the technical field of electronic packaging, relates to a thermal sintering method of a copper material, and in particular relates to a preparation method of copper-based soldering paste for one-step bonding and a bonding method thereof.
Background
With the rapid development of electronic products in the directions of miniaturization, high power density and high thermo-mechanical reliability, third-generation semiconductor devices such as SiC, gaN and the like are receiving more and more attention due to the advantages of wide band gap and high breakdown electric field, and can be used in high-temperature and high-frequency working environments. In general, the operating temperature of some equipment may exceed 250 ℃, and conventional high temperature lead-free solders are greatly limited in their application due to their relatively high processing temperatures potentially damaging nearby electronic components. Nanoparticle sintering technology provides a new approach to develop alternative die attach and interconnect materials due to its excellent low temperature sintering and high temperature properties. Compared with the bulk material, the nanoscale metal material has a size effect, can realize low-temperature sintering high-temperature service, and provides a new material for replacing chip connection and interconnection. The high cost and poor electromigration resistance of silver nanomaterials make them impractical for mass production. In contrast, copper nanoparticles, which are lower cost, have excellent electromigration resistance, and electrical and thermal conductivity comparable to silver, are promising candidates. Copper-based solder paste prepared from copper powder as a raw material has low cost and can be used as a substitute for silver paste, but copper has high chemical reactivity, particularly oxidation affinity when stored in air, so that the surface is oxidized, and sintering can be inhibited. The prior nano copper paste formula is generally formed by adding copper nano particles and a reducing agent into MOD, the bonding process needs to be preheated, the preparation process is complicated, and in addition, protective gas or reducing gas needs to be connected to inhibit oxidation of nano copper during bonding, so that the cost is greatly increased, and the large-scale application of the nano copper paste in industry is limited.
Therefore, development of a low cost, oxidation resistant, simple process copper-based solder paste would greatly promote the development of the electronic packaging industry.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide a preparation method of copper-based soldering paste for one-step bonding and a bonding method thereof, and adopts the following technical scheme:
the first aspect of the present invention provides a method for preparing a copper-based solder paste for one-step bonding, comprising the specific steps of: and (3) stirring and mixing 60-85% of copper powder, 5-35% of organic solvent carrier and 0-10% of reducing agent by mass percent to obtain the copper-based soldering paste.
Further, the particle size of the copper powder is 10nm-5 μm. The morphology of the copper powder is particles, flakes and the like, and can be prepared by a physical and chemical method.
Further, the organic solvent carrier is one or more of alcohols, alcohol ethers, amides, esters, ketones, organic amines and organic acids.
Further, the organic solvent carrier is selected from one or more of methanol, ethanol, ethylene glycol, n-propanol, isopropanol, glycerol, n-butanol, isobutanol, n-butanol, t-butanol, n-pentanol, n-hexanol, n-octanol, terpineol, alpha-terpineol, beta-terpineol, gamma-terpineol, triethylene glycol monomethyl ether, triethylene glycol dimethyl ether, triethylene glycol butyl ether, and triethylene glycol butyl ether acetate.
Further, the reducing agent is selected from one or more of ascorbic acid, citric acid, glyoxylic acid monohydrate, hydrazine hydrate, glucose, sodium hypophosphite, sodium borohydride, potassium borohydride, and formic acid.
The second aspect of the invention provides the copper-based solder paste for one-step bonding prepared by the preparation method.
The third aspect of the invention provides a method for one-step bonding by using the copper-based solder paste, which comprises the following specific steps: and coating the copper-based soldering paste on a substrate, and sintering to finish bonding.
Further, the external pressure of the sintering is 1-20MPa;
the sintering temperature is 150-350 ℃;
the sintering time is 5-30min.
Further, the substrate is a copper, gold or silver sheet or a ceramic sheet, a silicon wafer or a power device with the surface layer coated with copper, gold or silver.
Further, the method also comprises the pretreatment of washing and airing the substrate by absolute ethyl alcohol.
By adopting the technical scheme, the beneficial effects are that:
(1) The invention provides a preparation method of copper-based soldering paste for one-step bonding, which is characterized in that copper powder and an organic solvent carrier are directly stirred and mixed to obtain stable copper-based soldering paste, and a reducing agent is properly introduced to effectively promote sintering of the copper powder. The copper-based solder paste has excellent mechanical properties and is very suitable for interconnection of high-temperature power devices in microelectronic packaging.
The proper organic solvent can promote the sintering of copper powder to a certain extent, and the reducing agent can reduce copper oxide generated in the sintering process, so that the copper powder can keep a lower oxidation degree in the sintering process, and the sintering of the copper powder is facilitated. In the soldering paste system, when in bonding, the solvent in the soldering paste volatilizes, the rest copper powder is sintered among the copper powder under the external pressure and high temperature, and meanwhile, the reducing agent reduces copper oxide into elemental copper; because no inert atmosphere protection is added, a small amount of oxygen can be permeated between copper-copper particles, and the sintering of copper powder is facilitated by the proper oxygen content. This process continues until bonding is completed, eventually forming a secure copper-copper joint.
(2) Based on the size of copper powder in the copper-based soldering paste and the boiling point of an organic solvent, the designed one-step bonding process can form a reliable copper-copper joint through one-step bonding between substrates by external pressure without the processes of external protection gas, preheating and the like. The process can be well matched with the prepared copper-based soldering paste, the sintering molding of copper at low temperature is realized through a one-step bonding process, the microstructure is densified by applying external pressure in the bonding process, the sintering effect can be well achieved in the air at 150-350 ℃, after the sintering is completed, the soldering paste coating is sintered into a connecting layer, the copper-copper interconnection structure with higher shear strength is obtained, and the combined shear test result shows that the copper-copper interconnection structure has excellent mechanical properties and can be well applied to the field of high-power and high-temperature device packaging. The bonding process can be performed in air, one-step bonding is realized, the process is simple, the realization is easy, and the large-scale industrial application is facilitated.
Drawings
FIG. 1 is a schematic view of a copper-clad ceramic substrate according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of a package interconnect structure in accordance with an embodiment of the present invention;
fig. 3 is a schematic representation of one of the copper powders used in the examples of the present invention;
FIG. 4 is an SEM image of the shear fracture surface of a tie layer of example 1;
FIG. 5 is an SEM image of the shear fracture surface of a tie layer according to example 2 of the present invention;
fig. 6 is an SEM image of the shear fracture surface of the connection layer in example 3 of the present invention.
Detailed Description
The copper-based soldering paste can be applied to a packaging interconnection structure of an electronic device, the copper-based soldering paste is coated on a substrate and sintered under preset conditions, and a stable copper-copper interconnection structure is formed through the copper-based soldering paste, so that bonding between the substrates is realized. The substrate can be copper, gold or silver sheet, or ceramic sheet coated with copper, gold or silver, silicon wafer, power device, etc. In the embodiment of the invention, the effect of the copper-based solder paste and the one-step bonding process of the invention is detected by adopting the ceramic substrate coated with the metal coating as shown in fig. 1, and the package interconnection structure is shown in fig. 2, wherein the first master and the second master used in the package interconnection are selected as the substrates. As a preferred scheme, the master is pre-treated before the solder paste is applied, and the substrates (the first master and the second master) are ultrasonically washed in absolute ethanol for 30s and dried.
The specific operation of the shear fracture test on the connection layer is 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 1
1.2g of copper nanoparticles with the particle size of 100-500nm and 0.4g of ethylene glycol are stirred and mixed for 4min at 2000rpm/min in a high-speed mixer to prepare the soldering paste.
The solder paste prepared in this example was uniformly coated on the connection surface of the pretreated substrate; stacking the two substrates to obtain a sandwich structure of the substrates, the soldering paste coating layers and the substrates; the above substrate/solder paste coating/substrate stack structure was sintered in air at a pressure of 10MPa and a hot pressing temperature of 225 c for a pressure holding time of 10min. The solder paste coating is sintered into a connection layer, and after cooling, a package interconnect structure as shown in fig. 2 is obtained, and an SEM image of the shear fracture surface of the connection layer is shown in fig. 4.
Through a shear fracture test, the shear strength of the connection layer formed by sintering the soldering paste in the embodiment after cooling is 20-30MPa.
Example 2
The solder paste was prepared by mixing 1.2g of copper nanoparticles having a particle size of 20-200nm, 0.36g of an equal mass mixture of glycerin and α -terpineol, and 0.04g of ascorbic acid in a high-speed mixer with stirring at 2000rpm/min for 4 min.
The solder paste prepared in this example was uniformly coated on the connection surface of the pretreated substrate; stacking the two substrates to obtain a sandwich structure of the substrates, the soldering paste coating layers and the substrates; the above substrate/solder paste coating/substrate stack structure was sintered in air at a pressure of 12MP a and a hot pressing temperature of 225 c for a pressure holding time of 10min. The solder paste coating is sintered into a connection layer, and after cooling, a package interconnect structure as shown in fig. 2 is obtained, and an SEM image of the shear fracture surface of the connection layer is shown in fig. 5.
Through a shear fracture test, the shear strength of the connection layer formed by sintering the soldering paste in the embodiment after cooling is 20-30MPa.
Example 3
1.7g of copper nano particles with the particle size of 100-300nm and 0.3g of triethylene glycol monomethyl ether are stirred and mixed for 4min at 2000rpm/min in a high-speed mixer, and the soldering paste is prepared.
The solder paste prepared in this example was uniformly coated on the connection surface of the pretreated substrate; stacking the two substrates to obtain a sandwich structure of the substrates, the soldering paste coating layers and the substrates; sintering the stacked structure of the substrate/the soldering paste coating/the substrate in the downloading air with the pressure of 10MPa and the hot pressing temperature of 300 ℃ for 20min. The solder paste coating is sintered into a connection layer, and after cooling, a package interconnect structure as shown in fig. 2 is obtained, and an SEM image of the shear fracture surface of the connection layer is shown in fig. 6.
Through a shear fracture test, the shear strength of the connection layer formed by sintering the soldering paste in the embodiment after cooling is 30-40MPa.
The copper-copper joints obtained in the above examples all showed higher interconnect strength after shear strength testing.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. While still being apparent from variations or modifications that may be made by those skilled in the art are within the scope of the invention.
Claims (10)
1. The preparation method of the copper-based solder paste for one-step bonding is characterized by comprising the following specific steps of: and (3) stirring and mixing 60-85% of copper powder, 5-35% of organic solvent carrier and 0-10% of reducing agent by mass percent to obtain the copper-based soldering paste.
2. The method of claim 1, wherein the copper powder has a particle size of 10nm to 5 μm.
3. The method of claim 1, wherein the organic solvent carrier is one or more of alcohols, alcohol ethers, amides, esters, ketones, organic amines, and organic acids.
4. The method of claim 3, wherein the organic solvent carrier is selected from one or more of methanol, ethanol, ethylene glycol, n-propanol, isopropanol, glycerol, n-butanol, isobutanol, n-butanol, t-butanol, n-pentanol, n-hexanol, n-octanol, terpineol, α -terpineol, β -terpineol, γ -terpineol, triethylene glycol monomethyl ether, triethylene glycol dimethyl ether, triethylene glycol butyl ether, and triethylene glycol butyl ether acetate.
5. The method of claim 1, wherein the reducing agent is selected from one or more of ascorbic acid, citric acid, glyoxylic acid monohydrate, hydrazine hydrate, glucose, sodium hypophosphite, sodium borohydride, potassium borohydride, and formic acid.
6. A copper-based solder paste for one-step bonding prepared by the preparation method of any one of claims 1 to 5.
7. A method of one-step bonding using the copper-based solder paste of claim 6, comprising the steps of: and coating the copper-based soldering paste on a substrate, and sintering to finish bonding.
8. The method of claim 7, wherein the sintering is performed at an applied pressure of 1 to 20MPa;
the sintering temperature is 150-350 ℃;
the sintering time is 5-30min.
9. The method of claim 7, wherein the substrate is copper, gold, silver sheet, or ceramic sheet coated with copper, gold, silver on a surface layer, silicon wafer, or power device.
10. The method of claim 7, further comprising pre-treating the substrate with an absolute ethanol wash, air drying.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN118123153A (en) * | 2024-04-28 | 2024-06-04 | 陕西众森电能科技有限公司 | Copper paste curing process and device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN118123153A (en) * | 2024-04-28 | 2024-06-04 | 陕西众森电能科技有限公司 | Copper paste curing process and device |
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