CN116140859A - High-precision nano soldering paste and preparation method thereof - Google Patents
High-precision nano soldering paste and preparation method thereof Download PDFInfo
- Publication number
- CN116140859A CN116140859A CN202310342519.7A CN202310342519A CN116140859A CN 116140859 A CN116140859 A CN 116140859A CN 202310342519 A CN202310342519 A CN 202310342519A CN 116140859 A CN116140859 A CN 116140859A
- Authority
- CN
- China
- Prior art keywords
- nano
- copper
- antimony alloy
- precision
- parts
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000005476 soldering Methods 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- KGHMFMDJVUVBRY-UHFFFAOYSA-N antimony copper Chemical compound [Cu].[Sb] KGHMFMDJVUVBRY-UHFFFAOYSA-N 0.000 claims abstract description 94
- 229910001245 Sb alloy Inorganic materials 0.000 claims abstract description 88
- 239000002140 antimony alloy Substances 0.000 claims abstract description 88
- 229910000679 solder Inorganic materials 0.000 claims abstract description 56
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000007788 liquid Substances 0.000 claims abstract description 24
- HJOVHMDZYOCNQW-UHFFFAOYSA-N isophorone Chemical compound CC1=CC(=O)CC(C)(C)C1 HJOVHMDZYOCNQW-UHFFFAOYSA-N 0.000 claims abstract description 22
- 230000004907 flux Effects 0.000 claims abstract description 21
- 239000004925 Acrylic resin Substances 0.000 claims abstract description 17
- 229920000178 Acrylic resin Polymers 0.000 claims abstract description 17
- 229910052709 silver Inorganic materials 0.000 claims abstract description 17
- 239000004332 silver Substances 0.000 claims abstract description 17
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002904 solvent Substances 0.000 claims abstract description 15
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 14
- 239000003085 diluting agent Substances 0.000 claims abstract description 11
- 239000011135 tin Substances 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 33
- 238000003756 stirring Methods 0.000 claims description 30
- 239000003795 chemical substances by application Substances 0.000 claims description 27
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 26
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 19
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 18
- 239000001257 hydrogen Substances 0.000 claims description 15
- 229910052739 hydrogen Inorganic materials 0.000 claims description 15
- 229910052786 argon Inorganic materials 0.000 claims description 13
- 239000001307 helium Substances 0.000 claims description 13
- 229910052734 helium Inorganic materials 0.000 claims description 13
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 13
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims description 10
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 claims description 10
- 238000000498 ball milling Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 239000013008 thixotropic agent Substances 0.000 claims description 10
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 claims description 10
- 230000003213 activating effect Effects 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 9
- 238000005530 etching Methods 0.000 claims description 8
- 235000006408 oxalic acid Nutrition 0.000 claims description 8
- 239000000080 wetting agent Substances 0.000 claims description 8
- 239000002202 Polyethylene glycol Substances 0.000 claims description 7
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical group C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 claims description 7
- 238000001704 evaporation Methods 0.000 claims description 7
- 230000004048 modification Effects 0.000 claims description 7
- 238000012986 modification Methods 0.000 claims description 7
- 229920001223 polyethylene glycol Polymers 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 5
- 239000003607 modifier Substances 0.000 claims description 4
- 238000002161 passivation Methods 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 2
- 238000003466 welding Methods 0.000 abstract description 22
- 239000002245 particle Substances 0.000 abstract description 15
- 230000003064 anti-oxidating effect Effects 0.000 abstract description 3
- 230000008569 process Effects 0.000 description 16
- 150000002431 hydrogen Chemical class 0.000 description 12
- 239000000203 mixture Substances 0.000 description 9
- 235000019441 ethanol Nutrition 0.000 description 8
- 238000000227 grinding Methods 0.000 description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 229910044991 metal oxide Inorganic materials 0.000 description 4
- 150000004706 metal oxides Chemical class 0.000 description 4
- 239000002923 metal particle Substances 0.000 description 4
- LYRFLYHAGKPMFH-UHFFFAOYSA-N octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(N)=O LYRFLYHAGKPMFH-UHFFFAOYSA-N 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 239000004952 Polyamide Substances 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 229910052787 antimony Inorganic materials 0.000 description 2
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 229920002647 polyamide Polymers 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 229940037312 stearamide Drugs 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229940114069 12-hydroxystearate Drugs 0.000 description 1
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 238000001994 activation Methods 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012964 benzotriazole Substances 0.000 description 1
- 125000003354 benzotriazolyl group Chemical group N1N=NC2=C1C=CC=C2* 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 125000003976 glyceryl group Chemical group [H]C([*])([H])C(O[H])([H])C(O[H])([H])[H] 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 239000003381 stabilizer 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
-
- 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
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Electric Connection Of Electric Components To Printed Circuits (AREA)
Abstract
The application provides a high-precision nano soldering paste and a preparation method thereof, the high-precision nano soldering paste consists of liquid solder, soldering flux, an auxiliary agent and a solvent, wherein the liquid solder consists of nano copper-antimony alloy, nano tin, silver, acrylic resin and isophorone diluent, and the nano copper-antimony alloy and the nano tin are used as main components of the liquid solder, so that the size and the specification of a welding spot are further reduced after the soldering paste is welded, the requirement of the high-precision welding of the existing electronic equipment is met, and the high-precision nano soldering paste has the advantages of small solder particle size, high antioxidation degree, longer shelf life and convenience in popularization and implementation.
Description
Technical Field
The invention belongs to the technical field of soldering materials, and particularly relates to high-precision nano soldering paste and a preparation method thereof.
Background
The solder paste is a novel welding material which is generated along with SMT, is a paste mixture formed by solder powder, soldering flux and the like, is mainly used for welding electronic components such as PCB surface resistance, capacitance, IC and the like in the SMT industry, the existing solder paste can be divided into 3-8-level solder paste according to the particle size of the solder powder, wherein 8-level solder paste refers to solder paste prepared by using the solder powder with the particle size of 2-8 mu m, the precision degree of electronic equipment such as a mobile phone is obviously improved along with the limitation of equipment assembly specification, the particle size grade of the existing solder paste cannot meet the welding requirement of the precision electronic components, the existing nano metal powder is larger than a surface machine, the welding process is easier to oxidize, the defective product rate is high, the welding of the electronic components is inconvenient, the high precision is now needed, the oxidation resistance performance is high, and the high precision nano solder paste meeting the iterative welding requirement of the electronic components is urgently needed.
Disclosure of Invention
The invention provides high-precision nano soldering paste for solving the technical problem that the existing soldering paste cannot meet the welding requirement of high-precision electronic components;
the second object of the invention is to provide a method for preparing high-precision nano soldering paste.
In order to achieve the first object, the present application adopts the following scheme:
the high-precision nano soldering paste consists of, by weight, 75-82 parts of liquid solder, 10-17 parts of soldering flux, 6-8 parts of solvent and 1-2 parts of auxiliary agent;
the liquid solder consists of, by weight, 3-5 parts of nano copper-antimony alloy, 28-35 parts of nano tin, 1-3 parts of silver, 12-18 parts of acrylic resin and 28-33 parts of isophorone diluent;
the soldering flux consists of, by weight, 5-7 parts of a film forming agent, 2-3 parts of an activating agent, 1-2 parts of a thixotropic agent, 0.5-1 part of a slow etching agent and 0.5-1 part of a wetting agent.
Preferably, the solvent is one or more of ethanol, ethyl acetate, butyl acetate and acetone; more preferably, the solvent is ethanol, ethyl acetate and acetone with the mass ratio of 1:3: 0.5.
Preferably, the auxiliary agent comprises the following components in parts by weight, 0.5-1 part of stabilizer and 0.5-1 part of dispersing agent.
Preferably, the thixotropic agent is one or more of glyceryl tri-12-hydroxy stearate, polyamide and stearamide, the slow etching agent is benzotriazole, the wetting agent is OP-10, and more preferably, the thixotropic agent is 1 of polyamide and stearamide: 1, the expansibility of the solder paste can be obviously improved after the film forming agent, the activating agent and the thixotropic agent are compounded, so that the spreading area of the solder paste and the bonding pad is obviously improved.
Preferably, the activator is oxalic acid, citric acid and triethanolamine with the mass ratio of 1:1:2, the mixture has excellent activity and moderate corrosiveness, can efficiently take out the oxide on the surface of the bonding pad, and can not corrode the bonding pad in the welding process.
Preferably, the preparation method of the nano copper-antimony alloy comprises the following steps:
s101, placing the copper-antimony alloy block in a crucible at 40-60 ℃ for preheating and drying for 5-20min;
s102, placing the dried copper-antimony alloy into an arc plasma evaporator, vacuumizing to the vacuum degree of 0.03-0.056MPa by using a vacuum pump, and standing for 10-20min;
s103, introducing mixed gas of hydrogen, argon and helium into an arc plasma evaporator under the condition of 0.05-0.08MPa, evaporating copper-antimony alloy under the condition of 580-650A cathode current, and cooling to obtain crude nano copper-antimony alloy with the particle size of 190-410 nm;
s104, performing passivation modification on the crude nano copper-antimony alloy obtained in the step S103 to obtain the nano copper-antimony alloy.
Preferably, the preparation method of the copper-antimony alloy comprises the following steps: copper with the mass fraction of 93wt% and antimony with the mass fraction of 7wt% are simultaneously added into a crucible for high-temperature smelting to obtain liquid copper-antimony alloy, and the liquid copper-antimony alloy is poured into a die and cooled to room temperature to obtain the copper-antimony alloy.
Preferably, in the step S103, the volume ratio of the hydrogen, the argon and the helium is 1-3:5-8:1.
in the actual use process, the copper-antimony alloy is placed in an arc plasma evaporator, the copper-antimony alloy is evaporated into copper-antimony steam, hydrogen, argon and helium mixed gas are introduced, the copper-antimony steam is activated by the hydrogen, and is nucleated after colliding with the helium and the argon, and is settled to form coarse nano copper-antimony alloy, the hydrogen, the argon and the helium mixed gas are continuously introduced under the condition of 0.05-0.08MPa, however, the copper-antimony steam is fully activated and is fully impacted and nucleated with inert gas, incomplete reaction of the copper-antimony alloy is avoided, the nano copper-antimony alloy is continuously protected from oxidation after the complete reaction, compared with the traditional nano metal particle preparation method, the purity of metal can be obviously improved by using the arc plasma evaporation valve, the contact of nano metal particles and oxygen is reduced, and the content of metal oxides is reduced, so that the particle size of the nano copper-antimony alloy is 100-568nm.
Preferably, the passivation modification in the step S104 includes the following steps: and (3) putting the crude nano copper-antimony alloy obtained in the step (S103) into a magnetic stirrer containing a modifier, and stirring for 10-20min at 40-55 ℃ and 1200-1800 rpm.
Preferably, the modifier is BTA, oxalic acid, absolute ethyl alcohol and polyethylene glycol with the mass ratio of 1-3:1:2-3: 1.
In the actual use process, on the one hand, BTA, oxalic acid, absolute ethyl alcohol and polyethylene glycol mixture are used for modification, and on the other hand, a medium with reducibility is used for coating the nano copper-antimony alloy, so that the oxidation resistance in an aerobic environment is improved, and the storage time of the soldering paste is prolonged; on the other hand, after the coating of the reducing medium, the compatibility of the nano copper-antimony alloy and other components in the soldering flux is improved, the dispersion degree is improved, the nano copper-antimony alloy is placed for sedimentation and aggregation, and the nano particle size distribution is destroyed.
Preferably, the nano tin preparation method comprises the following steps: sequentially adding tin powder, citric acid and ethanol into an ultrasonic ball mill, ball-milling for 20-48 hours under the conditions of 200-350rpm,25-35 ℃ and ultrasonic vibration, and then filtering and drying to obtain the finished product.
Preferably, the ball-to-material ratio of the ultrasonic ball mill is 100-150:1, the ultrasonic vibration frequency is 15-30kHz, the power is 200-400W, and more preferably, the ultrasonic ball mill grinding ball is a stainless steel grinding ball with the diameter of 1.5-2 mm.
In the actual use process, the tin powder pigment is subjected to ultrasonic ball milling until the particle size is 200-500nm, nano tin is the main component of the solder, the cost of the solder can be effectively reduced by using a ball milling process, the tin activity is higher, the activation process is severe with hydrogen, the danger coefficient is high, the tin hardness is low, the ball milling process is convenient to implement, and the safety coefficient is high.
Preferably, the preparation method of the liquid solder comprises the following steps: sequentially adding the nano copper-antimony alloy, nano tin, silver, acrylic resin and isophorone diluent into a magnetic stirrer, and stirring at 500-1400rpm and 25-30 ℃ for 1-2 hours to obtain the nano copper-antimony alloy.
In the practical use process, the nanometer copper-antimony alloy, nanometer tin and silver are further coated by acrylic resin, the contact of the nanometer copper-antimony alloy, nanometer tin and silver with oxygen is further isolated, after the acrylic resin is coated, the content of metal oxide is further reduced, the wettability and the libido expansion rate of the soldering paste are obviously improved, the welding effect is obviously improved, furthermore, after the nanometer copper-antimony alloy, nanometer tin and silver are coated by the acrylic resin, auxiliary agents and solvents are matched, after the welding is finished, the hydrophilicity of residual substances on a welding plate is strong, and after the soldering residues are soaked in 78-90% ethanol solution for 3-5min, the soldering residues can be removed.
Preferably, the film forming agent is one or a combination of more than two of hydrogenated rosin, disproportionated rosin, maleic rosin and polymerized rosin, and more preferably, the film forming agent is the mass ratio of hydrogenated rosin to polymerized rosin is 1: 1.
In order to achieve the second object, the present application adopts the following technical scheme:
the preparation method of the high-precision nano soldering paste comprises the following steps:
s201, sequentially adding a film forming agent, an activating agent, a thixotropic agent, a slow etching agent and a wetting agent into a stirring kettle, and stirring for 20-30min at the temperature of 40-50 ℃ and the speed of 300-420rpm to obtain a soldering flux;
s202, sequentially adding the solder, the soldering flux, the auxiliary agent and the solvent into a vacuum stirring kettle, and stirring for 3-7h under the conditions of 25-35 ℃ and 400-620rpm to obtain the high-precision nano soldering paste.
Compared with the prior art, the application has the following beneficial effects:
1. the application provides a high-precision nano soldering paste and a preparation method thereof, the high-precision nano soldering paste consists of liquid solder, soldering flux, an auxiliary agent and a solvent, wherein the liquid solder consists of nano copper-antimony alloy, nano tin, silver, acrylic resin and isophorone diluent, and the nano copper-antimony alloy and the nano tin are used as main components of the liquid solder, so that the size and the specification of a welding spot are further reduced after the soldering paste is welded, the requirement of the high-precision welding of the existing electronic equipment is met, and the high-precision nano soldering paste has the advantages of small solder particle size, high antioxidation degree, longer shelf life and convenience in popularization and implementation.
2. The application provides a preparation method of high-precision nano soldering paste, which is characterized in that solder, soldering flux, auxiliary agent and solvent are stirred in a vacuum environment to prepare the environment-friendly low-residue easy-cleaning soldering paste, and the preparation method has the advantages of wide application field, small environmental pollution, simple and convenient operation, strong reproducibility and low implementation cost.
Detailed Description
The invention is further described in connection with tables 1-2 and specific examples 1-3 below:
(1) The preparation method of the copper-antimony alloy comprises the following steps:
and (3) adding 93wt% of copper and 7wt% of antimony into a crucible at the same time, smelting at high temperature to obtain liquid copper-antimony alloy, pouring the liquid copper-antimony alloy into a mould, and cooling to room temperature to obtain the copper-antimony alloy.
Example 1
The preparation method of the nano copper-antimony alloy comprises the following steps:
s101, placing the copper-antimony alloy block in a crucible at 42.5 ℃ for preheating and drying for 18min;
s102, placing the dried copper-antimony alloy into an arc plasma evaporator, vacuumizing to the vacuum degree of 0.037MPa by using a vacuum pump, and standing for 17min;
s103, mixing hydrogen, argon and helium in a volume ratio of 1:5:1, introducing the mixed gas into an arc plasma evaporator under the condition of 0.07MPa, evaporating copper-antimony alloy under the condition of cathode current 625A, and cooling to obtain crude nano copper-antimony alloy with the average particle diameter of 217 nm;
s104, adding the crude nano copper-antimony alloy obtained in the step S103 into a material containing BTA, oxalic acid, absolute ethyl alcohol and polyethylene glycol in a mass ratio of 1:1:2:1, stirring for 15min at 47 ℃ and 1325rpm in a magnetic stirrer of the mixture to obtain the nano copper-antimony alloy.
The preparation method of the nano tin comprises the following steps:
sequentially adding tin powder, citric acid and ethanol into an ultrasonic ball mill according to the mass ratio of 1:0.5:2, and at 330rpm and 35 ℃, the ball-to-material ratio is 145:1, carrying out ball milling for 48 hours under the condition that ultrasonic vibration frequency is 27kHz, power is 380W, an ultrasonic ball mill grinding ball is a stainless steel grinding ball with the diameter of 2mm, and then filtering and drying to obtain nano tin with the average particle size of 227 nm;
the preparation method of the liquid solder comprises the following steps of:
sequentially adding the nano copper-antimony alloy, nano tin, silver, acrylic resin and isophorone diluent into a magnetic stirrer, and stirring at 662rpm and 27 ℃ for 1.2 hours to obtain the nano copper-antimony alloy.
The preparation method of the high-precision nano soldering paste comprises the following steps of:
s201, sequentially adding a film forming agent, an activating agent, a thixotropic agent, a slow etching agent and a wetting agent into a stirring kettle, and stirring at 41.5 ℃ and 381rpm for 25min to obtain a soldering flux;
s202, sequentially adding the solder, the soldering flux, the auxiliary agent and the solvent into a vacuum stirring kettle, and stirring for 6.2 hours under the conditions of 26 ℃,420rpm and 0.035MPa of vacuum degree, thus obtaining the high-precision nano soldering paste.
Example 2
The preparation method of the nano copper-antimony alloy comprises the following steps:
s101, placing the copper-antimony alloy block in a crucible at 51.5 ℃ for preheating and drying for 12min;
s102, placing the dried copper-antimony alloy into an arc plasma evaporator, vacuumizing to the vacuum degree of 0.045MPa by using a vacuum pump, and standing for 16min;
s103, mixing hydrogen, argon and helium according to the volume ratio of 2:7:1, introducing the mixed gas into an arc plasma evaporator under the condition of 0.06MPa, evaporating the copper-antimony alloy under the condition of cathode current 611A, and cooling to obtain a crude nano copper-antimony alloy with the particle size of 320 nm;
s104, adding the crude nano copper-antimony alloy obtained in the step S103 into a material containing BTA, oxalic acid, absolute ethyl alcohol and polyethylene glycol with the mass ratio of 2:1:2:1, stirring for 16min at 47.5 ℃ and 1477rpm in a magnetic stirrer of the mixture to obtain the nano copper-antimony alloy.
The preparation method of the nano tin comprises the following steps:
sequentially adding tin powder, citric acid and ethanol into an ultrasonic ball mill according to the mass ratio of 1:0.5:2, and at 311rpm and 30 ℃, the ball-to-material ratio is 127:1, carrying out ball milling for 37 hours under the condition that ultrasonic vibration frequency is 21kHz, power is 333W, an ultrasonic ball mill grinding ball is a stainless steel grinding ball with the diameter of 1.7mm, and then filtering and drying to obtain 485nm nano tin with the average particle diameter;
the preparation method of the liquid solder comprises the following steps of:
sequentially adding the nano copper-antimony alloy, nano tin, silver, acrylic resin and isophorone diluent into a magnetic stirrer, and stirring at the speed of 856rpm and the temperature of 27.2 ℃ for 1.5 hours to obtain the nano copper-antimony alloy.
The preparation method of the high-precision nano soldering paste comprises the following steps of:
s201, sequentially adding a film forming agent, an activating agent, a thixotropic agent, a slow etching agent and a wetting agent into a stirring kettle, and stirring at 45.5 ℃ and 401rpm for 26 minutes to obtain a soldering flux;
s202, sequentially adding the solder, the soldering flux, the auxiliary agent and the solvent into a vacuum stirring kettle, and stirring for 5.6 hours under the conditions that the temperature is 29.5 ℃ and the rpm is 544rpm and the vacuum degree is 0.035MPa, thus obtaining the high-precision nano soldering paste.
Example 3
The preparation method of the nano copper-antimony alloy comprises the following steps:
s101, placing the copper-antimony alloy block in a crucible at 42 ℃, and preheating and drying for 19min;
s102, placing the dried copper-antimony alloy into an arc plasma evaporator, vacuumizing to the vacuum degree of 0.055MPa by using a vacuum pump, and standing for 18min;
s103, mixing hydrogen, argon and helium according to the volume ratio of 3:8:1, introducing the mixed gas into an arc plasma evaporator under the condition of 0.05MPa, evaporating copper-antimony alloy under the condition of cathode current 589A, and cooling to obtain crude nano copper-antimony alloy with the particle size of 215 nm;
s104, adding the crude nano copper-antimony alloy obtained in the step S103 into a material containing BTA, oxalic acid, absolute ethyl alcohol and polyethylene glycol in a mass ratio of 1:1:3:1, stirring for 20min at 42.5 ℃ and 1288rpm in a magnetic stirrer of the mixture to obtain the nano copper-antimony alloy.
The preparation method of the nano tin comprises the following steps:
sequentially adding tin powder, citric acid and ethanol into an ultrasonic ball mill, and at 315rpm and 29 ℃, the ball-to-material ratio is 110:1, carrying out ball milling for 33 hours under the condition that ultrasonic vibration frequency is 25kHz, power is 350W, an ultrasonic ball mill grinding ball is a stainless steel grinding ball with the diameter of 1.8mm, and then filtering and drying to obtain nano tin with the particle size of 402 nm;
the preparation method of the liquid solder comprises the following steps of:
sequentially adding the nano copper-antimony alloy, nano tin, silver, acrylic resin and isophorone diluent into a magnetic stirrer, and stirring at 1100rpm and 28 ℃ for 1.2 hours to obtain the nano copper-antimony alloy.
The preparation method of the high-precision nano soldering paste comprises the following steps of:
s201, sequentially adding a film forming agent, an activating agent, a thixotropic agent, a slow etching agent and a wetting agent into a stirring kettle, and stirring for 28min at 42 ℃ and 411rpm to obtain a soldering flux;
s202, sequentially adding the solder, the soldering flux, the auxiliary agent and the solvent into a vacuum stirring kettle, and stirring for 6.3 hours under the conditions of 25-35 ℃ and 541rpm and 0.035MPa of vacuum degree to obtain the high-precision nano soldering paste.
Table 1 examples 1-3 liquid solder compositions in parts by weight
| Liquid solder | Example 1 | Example 2 | Example 3 |
| Nano copper-antimony alloy | 3.1 | 3.8 | 4.2 |
| Nano tin | 29.3 | 30.9 | 31.6 |
| Silver (Ag) | 1.1 | 1.5 | 1.7 |
| Acrylic resin | 12.7 | 13.5 | 16.2 |
| Isophorone diluent | 28.5 | 30.1 | 31.2 |
TABLE 2 EXAMPLES 1-3 solder paste compositions by weight
Examples 1 to 3 and comparative examples 1 to 2 were subjected to solder paste performance tests according to the IPC-TM-650.6.3.7:2007, IPC J-STD-004-B, IPC-TM-650 2.4.34.3l:1995, IPC-TM-650.4.45:1995, JIS-Z-31976.6.1, IPC-TM-650.3.32 D:2004, IPC-TM-650.4.46 A:2004, IEC 62149-2-21, IPC-TM-650.3.13:2004, IPC-TM-650 2.2.14.1:1995 standards, and the test results are shown in Table 3 below.
Table 3 test results for examples 1-3
As can be seen from Table 3, in the actual use process, the copper-antimony alloy is placed in an arc plasma evaporator, the copper-antimony alloy is evaporated into copper-antimony vapor, after hydrogen, argon and helium mixed gas are introduced, the copper-antimony vapor is activated by the hydrogen, and is nucleated after colliding with the helium and the argon, and is settled to form coarse nano copper-antimony alloy, the hydrogen, the argon and the helium mixed gas are continuously introduced, however, the copper-antimony vapor is fully activated and is fully impacted with inert gas to nucleate, incomplete reaction of the copper-antimony alloy is avoided, and the nano copper-antimony alloy is continuously protected from oxidation after complete reaction, compared with the traditional nano metal particle preparation method, the arc plasma evaporation valve can obviously improve the purity of metal, reduce the contact of nano metal particles and oxygen, reduce the content of metal oxides, and the nano tin and the nano copper-antimony alloy in the welding process can not be oxidized too early, the actual use performance accords with the industry standard, and can meet the requirements of high-precision electronic equipment and nano-level welding;
in the actual use process, the mixture of BTA, oxalic acid, absolute ethyl alcohol and polyethylene glycol is used for modification, on one hand, a medium with reducibility is used for coating the nano copper-antimony alloy, so that the oxidation resistance under the aerobic environment is improved, and the storage time of the soldering paste is prolonged; on the other hand, after the coating by using a reducing medium, the compatibility of the nano copper-antimony alloy and other components in the soldering flux is improved, the dispersion degree is improved, the nano copper-antimony alloy is placed for sedimentation and aggregation, and the nano particle size distribution is destroyed;
in the actual use process, nano tin is the main component of the solder, the cost of the solder can be effectively reduced by using a ball milling process, the tin activity is higher, the risk coefficient is high in a severe hydrogen activating process, the tin hardness is low, the ball milling process is convenient to implement, and the safety coefficient is high;
in the practical use process, the nanometer copper-antimony alloy, nanometer tin and silver are further coated by acrylic resin, the contact of the nanometer copper-antimony alloy, nanometer tin and silver with oxygen is further isolated, after the acrylic resin is coated, the content of metal oxide is further reduced, the wettability and the libido expansion rate of the soldering paste are obviously improved, the welding effect is obviously improved, furthermore, after the nanometer copper-antimony alloy, nanometer tin and silver are coated by the acrylic resin, auxiliary agents and solvents are matched, after the welding is finished, the hydrophilicity of residual substances on a welding plate is strong, and after the soldering residues are soaked in 78-90% ethanol solution for 3-5min, the soldering residues can be removed.
The application provides a high-precision nano soldering paste and a preparation method thereof, the high-precision nano soldering paste consists of liquid solder, soldering flux, an auxiliary agent and a solvent, wherein the liquid solder consists of nano copper-antimony alloy, nano tin, silver, acrylic resin and isophorone diluent, and the nano copper-antimony alloy and the nano tin are used as main components of the liquid solder, so that the size and the specification of a welding spot are further reduced after the soldering paste is welded, the requirement of the high-precision welding of the existing electronic equipment is met, and the high-precision nano soldering paste has the advantages of small solder particle size, high antioxidation degree, longer shelf life and convenience in popularization and implementation.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (10)
1. The high-precision nano soldering paste is characterized by comprising, by weight, 75-82 parts of liquid solder, 10-17 parts of soldering flux, 6-8 parts of solvent and 1-2 parts of auxiliary agent;
the liquid solder consists of, by weight, 3-5 parts of nano copper-antimony alloy, 28-35 parts of nano tin, 1-3 parts of silver, 12-18 parts of acrylic resin and 28-33 parts of isophorone diluent;
the soldering flux consists of, by weight, 5-7 parts of a film forming agent, 2-3 parts of an activating agent, 1-2 parts of a thixotropic agent, 0.5-1 part of a slow etching agent and 0.5-1 part of a wetting agent.
2. The high-precision nano solder paste according to claim 1, wherein the preparation method of the nano copper-antimony alloy comprises the following steps:
s101, placing the copper-antimony alloy block in a crucible at 40-60 ℃ for preheating and drying for 5-20min;
s102, placing the dried copper-antimony alloy into an arc plasma evaporator, vacuumizing to the vacuum degree of 0.03-0.056MPa by using a vacuum pump, and standing for 10-20min;
s103, introducing mixed gas of hydrogen, argon and helium into an arc plasma evaporator under the condition of 0.05-0.08MPa, evaporating copper-antimony alloy under the condition of 580-650A cathode current, and cooling to obtain crude nano copper-antimony alloy;
s104, performing passivation modification on the crude nano copper-antimony alloy obtained in the step S103 to obtain the nano copper-antimony alloy.
3. The high-precision nano solder paste according to claim 2, wherein the volume ratio of hydrogen, argon and helium in the step S103 is 1-3:5-8:1.
4. The high-precision nano solder paste according to claim 2, wherein the passivation modification in step S104 comprises the steps of: and (3) putting the crude nano copper-antimony alloy obtained in the step (S103) into a magnetic stirrer containing a modifier, and stirring for 10-20min at 40-55 ℃ and 1200-1800 rpm.
5. The high-precision nano solder paste according to claim 4, wherein the modifier is BTA, oxalic acid, absolute ethanol and polyethylene glycol in a mass ratio of 1-3:1:2-3: 1.
6. The high-precision nano solder paste according to claim 1, wherein the nano tin preparation method comprises the following steps: sequentially adding tin powder, citric acid and ethanol into an ultrasonic ball mill, ball-milling for 20-48 hours under the conditions of 200-350rpm,25-35 ℃ and ultrasonic vibration, and then filtering and drying to obtain the finished product.
7. The high-precision nano solder paste according to claim 6, wherein the ball-to-material ratio of the ultrasonic ball mill is 100-150:1, and the ultrasonic vibration frequency is 15-30kHz.
8. The high-precision nano solder paste according to claim 1, wherein the method for preparing the liquid solder comprises the following steps: sequentially adding the nano copper-antimony alloy, nano tin, silver, acrylic resin and isophorone diluent into a magnetic stirrer, and stirring at 500-1400rpm and 25-30 ℃ for 1-2 hours to obtain the nano copper-antimony alloy.
9. The high-precision nano solder paste according to claim 1, wherein the film forming agent is one or a combination of more than two of hydrogenated rosin, disproportionated rosin, maleated rosin and polymerized rosin.
10. The method for preparing high-precision nano solder paste according to any of claims 1 to 9, comprising the steps of:
s201, sequentially adding a film forming agent, an activating agent, a thixotropic agent, a slow etching agent and a wetting agent into a stirring kettle, and stirring for 20-30min at the temperature of 40-50 ℃ and the speed of 300-420rpm to obtain a soldering flux;
s202, sequentially adding the solder, the soldering flux, the auxiliary agent and the solvent into a vacuum stirring kettle, and stirring for 3-7h at the temperature of 25-35 ℃ and the speed of 400-620rpm to obtain the environment-friendly low-residue easy-cleaning soldering paste.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310342519.7A CN116140859A (en) | 2023-04-03 | 2023-04-03 | High-precision nano soldering paste and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310342519.7A CN116140859A (en) | 2023-04-03 | 2023-04-03 | High-precision nano soldering paste and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116140859A true CN116140859A (en) | 2023-05-23 |
Family
ID=86358416
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310342519.7A Pending CN116140859A (en) | 2023-04-03 | 2023-04-03 | High-precision nano soldering paste and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116140859A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101745636A (en) * | 2008-12-16 | 2010-06-23 | 北京有色金属研究总院 | Method for preparing antioxidant soldering powder |
| CN104002061A (en) * | 2014-05-21 | 2014-08-27 | 广州柏仕达新材料有限公司 | High-performance high-stability nanometer soldering paste and preparation method thereof |
| CN112496333A (en) * | 2020-11-26 | 2021-03-16 | 大连理工大学 | Preparation method and application of Si-Ti alloy nano powder |
-
2023
- 2023-04-03 CN CN202310342519.7A patent/CN116140859A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101745636A (en) * | 2008-12-16 | 2010-06-23 | 北京有色金属研究总院 | Method for preparing antioxidant soldering powder |
| CN104002061A (en) * | 2014-05-21 | 2014-08-27 | 广州柏仕达新材料有限公司 | High-performance high-stability nanometer soldering paste and preparation method thereof |
| CN112496333A (en) * | 2020-11-26 | 2021-03-16 | 大连理工大学 | Preparation method and application of Si-Ti alloy nano powder |
Non-Patent Citations (1)
| Title |
|---|
| 万少华: "《电子产品结构与工艺》", 29 February 2008, 北京：北京邮电大学出版社, pages: 35 - 36 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111590235B (en) | Low-dielectric-loss high-reliability soldering paste and preparation method thereof | |
| CA2781958C (en) | Flux for solder paste and solder paste | |
| CN102528327B (en) | High-temperature lead-free solder paste and preparation method | |
| CN107570911B (en) | Lead-free high-temperature soldering paste for mobile phone and computer mainboard and preparation method thereof | |
| CN108555474B (en) | Halogen-free environment-friendly lead-free tin paste and preparation method thereof | |
| CN111015011B (en) | High-stability soldering paste and preparation method thereof | |
| CN112719694B (en) | Soldering flux composition, preparation method of soldering flux composition, gold-tin soldering paste for spray printing and preparation method of gold-tin soldering paste | |
| CN102513735A (en) | Flux paste for high-bismuth content solder paste and preparation method thereof | |
| JP4780527B2 (en) | Flux composition for soldering, cream solder composition, and electronic component | |
| CN113510406A (en) | Microelectronic assembly solder paste and preparation method thereof | |
| CN116140859A (en) | High-precision nano soldering paste and preparation method thereof | |
| CN113070604B (en) | Double-layer solder sheet and preparation process thereof | |
| CN109014656A (en) | A kind of halogen-free scaling powder and its preparation method and application | |
| CN115781098B (en) | High-temperature-resistant and oxidation-resistant soldering tin powder and solder paste containing metal indium and preparation methods thereof | |
| CN117548901B (en) | Low-cavity halogen-free solder paste and preparation method thereof | |
| CN109909639A (en) | A kind of solder(ing) paste and preparation method thereof | |
| CN114985750B (en) | Preparation method of tin-silver-copper alloy nano powder, tin-silver-copper nano alloy low-temperature slurry, preparation method and application thereof | |
| CN112621024B (en) | Soldering flux material composition and preparation method of soldering flux | |
| CN118342159A (en) | Formic acid high-lead solder paste and application thereof | |
| CN116787023B (en) | Preformed soldering lug and preparation method thereof | |
| CN112872521B (en) | Data line interface welding process and preparation method thereof | |
| CN116900553B (en) | Preparation method of lead-free composite soldering paste with high spreading rate | |
| CN114367760B (en) | High-reliability halogen-free lead-free soldering paste and preparation method thereof | |
| CN113210931A (en) | Soldering flux for solder paste, preparation method thereof and halogen-free and lead-free solder paste | |
| CN116213996A (en) | Gold-based alloy soldering paste with good dispensing performance and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |