CN111940947A - Halogen-free solder paste and preparation method thereof - Google Patents
Halogen-free solder paste and preparation method thereof Download PDFInfo
- Publication number
- CN111940947A CN111940947A CN202010827877.3A CN202010827877A CN111940947A CN 111940947 A CN111940947 A CN 111940947A CN 202010827877 A CN202010827877 A CN 202010827877A CN 111940947 A CN111940947 A CN 111940947A
- Authority
- CN
- China
- Prior art keywords
- halogen
- solder paste
- weight
- free
- free solder
- 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.)
- Granted
Links
- 229910000679 solder Inorganic materials 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 35
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 31
- 239000000956 alloy Substances 0.000 claims abstract description 31
- 239000000843 powder Substances 0.000 claims abstract description 31
- 239000011347 resin Substances 0.000 claims abstract description 28
- 229920005989 resin Polymers 0.000 claims abstract description 28
- 239000003784 tall oil Substances 0.000 claims abstract description 26
- 239000003960 organic solvent Substances 0.000 claims abstract description 21
- 239000013008 thixotropic agent Substances 0.000 claims abstract description 20
- 230000003213 activating effect Effects 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims description 27
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 24
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 7
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 claims description 6
- LCTONWCANYUPML-UHFFFAOYSA-N Pyruvic acid Chemical compound CC(=O)C(O)=O LCTONWCANYUPML-UHFFFAOYSA-N 0.000 claims description 6
- ZFOZVQLOBQUTQQ-UHFFFAOYSA-N Tributyl citrate Chemical compound CCCCOC(=O)CC(O)(C(=O)OCCCC)CC(=O)OCCCC ZFOZVQLOBQUTQQ-UHFFFAOYSA-N 0.000 claims description 6
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 5
- 239000012190 activator Substances 0.000 claims description 5
- 229920000728 polyester Polymers 0.000 claims description 5
- 229920000570 polyether Polymers 0.000 claims description 5
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 claims description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 4
- KQNPFQTWMSNSAP-UHFFFAOYSA-N isobutyric acid Chemical compound CC(C)C(O)=O KQNPFQTWMSNSAP-UHFFFAOYSA-N 0.000 claims description 4
- 229910052709 silver Inorganic materials 0.000 claims description 4
- 239000004332 silver Substances 0.000 claims description 4
- VXQBJTKSVGFQOL-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethyl acetate Chemical compound CCCCOCCOCCOC(C)=O VXQBJTKSVGFQOL-UHFFFAOYSA-N 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 125000000217 alkyl group Chemical group 0.000 claims description 3
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052797 bismuth Inorganic materials 0.000 claims description 3
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 3
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 claims description 3
- 150000002148 esters Chemical class 0.000 claims description 3
- 229910021485 fumed silica Inorganic materials 0.000 claims description 3
- 239000004310 lactic acid Substances 0.000 claims description 3
- 235000014655 lactic acid Nutrition 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 229940107700 pyruvic acid Drugs 0.000 claims description 3
- 229910052714 tellurium Inorganic materials 0.000 claims description 3
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims description 3
- 229940116411 terpineol Drugs 0.000 claims description 3
- IFPMZBBHBZQTOV-UHFFFAOYSA-N 1,3,5-trinitro-2-(2,4,6-trinitrophenyl)-4-[2,4,6-trinitro-3-(2,4,6-trinitrophenyl)phenyl]benzene Chemical compound [O-][N+](=O)C1=CC([N+](=O)[O-])=CC([N+]([O-])=O)=C1C1=C([N+]([O-])=O)C=C([N+]([O-])=O)C(C=2C(=C(C=3C(=CC(=CC=3[N+]([O-])=O)[N+]([O-])=O)[N+]([O-])=O)C(=CC=2[N+]([O-])=O)[N+]([O-])=O)[N+]([O-])=O)=C1[N+]([O-])=O IFPMZBBHBZQTOV-UHFFFAOYSA-N 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000004359 castor oil Substances 0.000 claims description 2
- 235000019438 castor oil Nutrition 0.000 claims description 2
- 239000004927 clay Substances 0.000 claims description 2
- CCIVGXIOQKPBKL-UHFFFAOYSA-M ethanesulfonate Chemical compound CCS([O-])(=O)=O CCIVGXIOQKPBKL-UHFFFAOYSA-M 0.000 claims description 2
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 2
- 229940098779 methanesulfonic acid Drugs 0.000 claims description 2
- 235000019260 propionic acid Nutrition 0.000 claims description 2
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 2
- 238000003466 welding Methods 0.000 abstract description 13
- 229910052736 halogen Inorganic materials 0.000 abstract description 4
- 150000002367 halogens Chemical class 0.000 abstract description 4
- 238000004140 cleaning Methods 0.000 abstract description 3
- 239000000758 substrate Substances 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract 1
- 231100000956 nontoxicity Toxicity 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 4
- 238000005476 soldering Methods 0.000 description 4
- 239000000654 additive Substances 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- -1 alcohol ester Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- CCIVGXIOQKPBKL-UHFFFAOYSA-N ethanesulfonic acid Chemical compound CCS(O)(=O)=O CCIVGXIOQKPBKL-UHFFFAOYSA-N 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 125000005375 organosiloxane group Chemical group 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 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 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
- B23K35/26—Selection of soldering or welding materials proper with the principal constituent melting at less than 400 degrees C
- B23K35/262—Sn 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
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Electric Connection Of Electric Components To Printed Circuits (AREA)
Abstract
The invention belongs to the technical field of solder paste and preparation, and provides halogen-free solder paste and a preparation method thereof, wherein the halogen-free solder paste comprises 80-90 parts by weight of Sn-X alloy powder, 0.5-1.5 parts by weight of halogen-free activating agent, 2-4 parts by weight of organic solvent, 3-5 parts by weight of liquid rosin resin, 0.5-1 part by weight of thixotropic agent and 0.05-0.5 part by weight of flatting agent, so that the influence of halogen on the weldability after welding is solved, and the halogen-free solder paste has the advantages of less residues after welding, no cleaning, environmental protection, no toxicity, lower cost and strong market competitiveness. The halogen-free solder paste has good adhesion with the welding substrate, and the problem of poor welding performance of the conventional solder paste can be effectively solved.
Description
Technical Field
The invention belongs to the technical field of solder paste and preparation, and particularly relates to halogen-free solder paste and a preparation method thereof.
Background
Solder paste is a new type of soldering material which is produced along with SMT. The solder paste is a complex system and is a paste formed by mixing tin powder, soldering flux and other additives. The tin paste has certain viscosity at normal temperature, can initially adhere the electronic component to a set position, and welds the welded component and the printed circuit pad to form permanent connection along with the volatilization of the solvent and part of the additive at the welding temperature.
The Chinese patent application CN101143407A discloses a solder paste and a preparation method thereof, wherein the solder paste comprises the following components in percentage by weight; 80-90% of alloy welding powder; 6-8% of an organic solvent; 1-8% of organic acid; 2-10% of resin; 0.2 to 2 percent of surfactant. The alloy welding powder consists of 95.5 to 99.5 weight percent of tin, 0.3 to 4 weight percent of silver and 0.1 to 0.7 weight percent of copper. Although the soldering flux of the solder paste does not contain halide, the solder paste has strong adaptability, no residue is left around the soldered joint after soldering, and the solder paste is free from cleaning. But the alloy welding powder of the solder paste has poor thinning degree, uneven distribution, low elongation of the alloy welding powder and poor mechanical property of the solder paste.
Disclosure of Invention
In order to solve the above problems, the present invention provides a halogen-free solder paste and a method for preparing the same, wherein halogen is not detected in the halogen-free solder paste, and the adhesive force and the expansion rate are stronger than those of solder pastes composed of conventional formulations, and the present invention has the following technical scheme:
the invention aims to provide a halogen-free tin paste, which has the technical points that: the halogen-free tin paste is prepared by mixing 80-90 parts by weight of Sn-X alloy powder, 0.5-1.5 parts by weight of halogen-free activating agent, 2-4 parts by weight of organic solvent, 3-5 parts by weight of liquid rosin resin, 0.5-1 part by weight of thixotropic agent and 0.05-0.5 part by weight of leveling agent.
In some embodiments of the present invention, the weight of the element X is 0.1 to 2 wt% based on 100 wt% of the Sn-X alloy powder.
In some embodiments of the present invention, the X element in the Sn-X alloy powder is at least one of a silver element, a bismuth element, an aluminum element, and a tellurium element.
In some embodiments of the present invention, the halogen-free activating agent is at least one of acetic acid, lactic acid, pyruvic acid, propionic acid, butyric acid, isobutyric acid, methanesulfonic acid, and ethanesulfonic acid.
In some embodiments of the present invention, the organic solvent is at least one of alcohol ester dodeca, terpineol, tributyl citrate and butyl carbitol acetate.
In some embodiments of the present invention, the liquid rosin resin has a density of 1 to 1.1g/cm2Said liquid pineThe solid content of the aromatic resin is 48-50 wt%, and the pH value is 4.5-6.5.
In some embodiments of the present invention, the thixotropic agent is at least one of fumed silica, clay particles, hydrogenated castor oil, and dodecahydroxystearic acid.
In some embodiments of the present invention, the leveling agent is at least one of polyether polyester modified organosiloxane and alkyl modified organosiloxane.
According to the formula, the invention aims to provide a preparation method of halogen-free tin paste, which has the technical points that: the preparation method of the halogen-free solder paste comprises the following steps:
the method comprises the following steps: accurately weighing the components of each raw material by using an analytical balance, and uniformly mixing an organic solvent, a halogen-free activating agent and liquid rosin resin in a stirrer to obtain a mixture A, wherein the rotating speed of the stirrer is 500-700rmp, and the stirring time is 10-20 min;
step two: placing Sn-X alloy powder into the mixture A prepared in the step one, and uniformly mixing in a homogenizer to obtain a mixture B, wherein the rotation speed of the homogenizer is 1000-1200rmp, and the homogenizing time is 3-5 min;
step three: and adding a thixotropic agent and a leveling agent into a homogenizer according to the condition of the mixture B, and uniformly mixing to obtain the halogen-free tin paste, wherein the rotation speed of the homogenizer is 1000-1200rmp, and the homogenizing time is 3-5 min.
In some embodiments of the present invention, the viscosity of the halogen-free solder paste at a rotation speed of 10rmp is 190-270 Pa.s/25 ℃.
Compared with the prior art, the invention has the beneficial effects that:
the halogen-free tin paste comprises Sn-X alloy powder, a halogen-free activating agent, an organic solvent, liquid rosin resin, a thixotropic agent and a leveling agent, solves the problem of influence of halogen on the weldability, has few residues after welding, is free of cleaning, is environment-friendly and non-toxic, has low cost and has strong market competitiveness. The halogen-free solder paste has good adhesion with the welding substrate, and the problem of poor welding performance of the conventional solder paste can be effectively solved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below so that those skilled in the art can better understand the advantages and features of the present invention, and thus the scope of the present invention will be more clearly defined. The embodiments described herein are only a few embodiments of the present invention, rather than all embodiments, and all other embodiments that can be derived by one of ordinary skill in the art without inventive faculty based on the embodiments described herein are intended to fall within the scope of the present invention.
Example 1
The halogen-free tin paste is prepared by mixing 85 parts by weight of Sn-X alloy powder, 1 part by weight of halogen-free activating agent, 3 parts by weight of organic solvent, 4 parts by weight of liquid rosin resin, 0.75 part by weight of thixotropic agent and 0.2 part by weight of leveling agent.
Wherein, the weight of the Sn-X alloy powder is 100 wt%, and the weight of the X element is 1 wt%.
Wherein, the X element in the Sn-X alloy powder is silver element.
Wherein the halogen-free activator is acetic acid.
Wherein, the organic solvent is alcohol ester twelve.
Wherein the density of the liquid rosin resin is 1.05/cm2The solid content of the liquid rosin ester is 49 wt%, and the pH value is 5.5.
Wherein the thixotropic agent is fumed silica.
Wherein the leveling agent is polyether polyester modified organic siloxane.
According to the formula, the invention aims to provide a preparation method of the halogen-free tin paste, which comprises the following steps:
the method comprises the following steps: accurately weighing the components of each raw material by using an analytical balance, and uniformly mixing an organic solvent, a halogen-free activating agent and liquid rosin resin in a stirrer to obtain a mixture A, wherein the rotating speed of the stirrer is 600rmp, and the stirring time is 15 min;
step two: placing Sn-X alloy powder into the mixture A prepared in the step one, and uniformly mixing in a homogenizer to obtain a mixture B, wherein the rotation speed of the homogenizer is 1100rmp, and the homogenizing time is 4 min;
step three: and adding a thixotropic agent and a leveling agent into a homogenizer according to the condition of the mixture B, and uniformly mixing to obtain the halogen-free tin paste, wherein the rotation speed of the homogenizer is 1100rmp, and the homogenizing time is 5 min.
Wherein the viscosity of the halogen-free solder paste at a rotation speed of 10rmp is 230 pas/25 ℃.
Example 2
The halogen-free tin paste is prepared by mixing 90 parts by weight of Sn-X alloy powder, 1.5 parts by weight of halogen-free activating agent, 4 parts by weight of organic solvent, 5 parts by weight of liquid rosin resin, 1 part by weight of thixotropic agent and 0.5 part by weight of leveling agent.
Wherein, the weight of the Sn-X alloy powder is 100 wt%, and the weight of the X element is 2 wt%.
Wherein, the X element in the Sn-X alloy powder is bismuth element.
Wherein the halogen-free activator is lactic acid.
Wherein the organic solvent is terpineol.
Wherein the density of the liquid rosin resin is 1g/cm2The solid content of the liquid rosin resin is 48 wt%, and the pH value is 4.5.
Wherein the thixotropic agent is argil particles.
Wherein the leveling agent is alkyl modified organic siloxane.
According to the formula, the invention aims to provide a preparation method of the halogen-free tin paste, which comprises the following steps:
the method comprises the following steps: accurately weighing the components of each raw material by using an analytical balance, and uniformly mixing an organic solvent, a halogen-free activating agent and liquid rosin resin in a stirrer to obtain a mixture A, wherein the rotating speed of the stirrer is 700rmp, and the stirring time is 10 min;
step two: placing Sn-X alloy powder into the mixture A prepared in the step one, and uniformly mixing in a homogenizer to obtain a mixture B, wherein the rotation speed of the homogenizer is 1000rmp, and the homogenizing time is 5 min;
step three: and adding a thixotropic agent and a leveling agent into a homogenizer according to the condition of the mixture B, and uniformly mixing to obtain the halogen-free tin paste, wherein the rotating speed of the homogenizer is 1000rmp, and the homogenizing time is 5 min.
Wherein the viscosity of the halogen-free solder paste at a rotation speed of 10rmp is 270 pas/25 ℃.
Example 3
The halogen-free tin paste is prepared by mixing 80 parts by weight of Sn-X alloy powder, 0.5 part by weight of halogen-free activating agent, 2 parts by weight of organic solvent, 3 parts by weight of liquid rosin resin, 0.5 part by weight of thixotropic agent and 0.05 part by weight of leveling agent.
Wherein the weight of the Sn-X alloy powder is 100 wt%, and the weight of the X element is 0.1 wt%.
Wherein, the X element in the Sn-X alloy powder is an aluminum element.
Wherein the halogen-free activator is pyruvic acid.
Wherein the organic solvent is tributyl citrate.
Wherein the density of the liquid rosin resin is 1g/cm2The solid content of the liquid rosin resin is 48 wt%, and the pH value is 4.5.
Wherein the thixotropic agent is gas-phase dodecahydroxystearic acid.
Wherein, the leveling agent is a mixture of polyether polyester modified organic siloxane and alkyl modified organic siloxane.
According to the formula, the invention aims to provide a preparation method of the halogen-free tin paste, which comprises the following steps:
the method comprises the following steps: accurately weighing the components of each raw material by using an analytical balance, and uniformly mixing an organic solvent, a halogen-free activating agent and liquid rosin resin in a stirrer to obtain a mixture A, wherein the rotating speed of the stirrer is 700rmp, and the stirring time is 10 min;
step two: placing Sn-X alloy powder into the mixture A prepared in the step one, and uniformly mixing in a homogenizer to obtain a mixture B, wherein the rotation speed of the homogenizer is 1200rmp, and the homogenizing time is 3 min;
step three: and adding a thixotropic agent and a leveling agent into a homogenizer according to the condition of the mixture B, and uniformly mixing to obtain the halogen-free tin paste, wherein the rotation speed of the homogenizer is 1200rmp, and the homogenizing time is 3 min.
Wherein the viscosity of the halogen-free solder paste at a rotation speed of 10rmp is 190 pas/25 ℃.
Example 4
The halogen-free tin paste is prepared by mixing 88 parts by weight of Sn-X alloy powder, 1.2 parts by weight of halogen-free activating agent, 3.5 parts by weight of organic solvent, 4.5 parts by weight of liquid rosin resin, 0.9 part by weight of thixotropic agent and 0.35 part by weight of leveling agent.
Wherein, the weight of the Sn-X alloy powder is 100 wt%, and the weight of the X element is 1.5 wt%.
Wherein, the X element in the Sn-X alloy powder is tellurium element.
Wherein the halogen-free activator is a mixture of butyric acid and ethylsulfonic acid.
Wherein the organic solvent is butyl carbitol acetate.
Wherein the density of the liquid rosin resin is 1.03g/cm2The solid content of the liquid rosin resin is 49 wt%, and the pH value is 5.
Wherein the thixotropic agent is dodecahydroxystearic acid.
Wherein the leveling agent is polyether polyester modified organic siloxane.
According to the formula, the invention aims to provide a preparation method of the halogen-free tin paste, which comprises the following steps:
the method comprises the following steps: accurately weighing the components of each raw material by using an analytical balance, and uniformly mixing an organic solvent, a halogen-free activating agent and liquid rosin resin in a stirrer to obtain a mixture A, wherein the rotating speed of the stirrer is 550rmp, and the stirring time is 18 min;
step two: placing Sn-X alloy powder into the mixture A prepared in the step one, and uniformly mixing in a homogenizer to obtain a mixture B, wherein the rotation speed of the homogenizer is 1000rmp, and the homogenizing time is 5 min;
step three: and adding a thixotropic agent and a leveling agent into a homogenizer according to the condition of the mixture B, and uniformly mixing to obtain the halogen-free tin paste, wherein the rotating speed of the homogenizer is 1000rmp, and the homogenizing time is 5 min.
Wherein the viscosity of the halogen-free solder paste at a rotation speed of 10rmp is 200 pas/25 ℃.
Comparative example 1
The same procedure as in example 1 was repeated except that "liquid rosin resin" in example 1 was changed to "rosin resin" of the same quality.
Comparative example 2
The operation was carried out in the same manner as in example 1 except that "Sn-X alloy powder" in example 1 was changed to "tin powder".
Examples of the experiments
The mechanical green content and the spreading rate of the solder paste prepared in the embodiments 1 to 4 are measured, and the adhesive force of the solder paste after welding is detected, and the specific results are shown in the table 1:
TABLE 1
Halogen content | Expansion ratio/% | adhesion/N | |
Example 1 | Not detected out | 82.2 | 4.2 |
Example 2 | Not detected out | 83.5 | 4.3 |
Example 3 | Not detected out | 86.1 | 4.6 |
Example 4 | Not detected out | 82.1 | 4.2 |
Comparative example 1 | Not detected out | 75.3 | 4.1 |
Comparative example 2 | Not detected out | 84.2 | 3.5 |
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. A halogen-free solder paste is characterized in that: the halogen-free tin paste is prepared by mixing 80-90 parts by weight of Sn-X alloy powder, 0.5-1.5 parts by weight of halogen-free activating agent, 2-4 parts by weight of organic solvent, 3-5 parts by weight of liquid rosin resin, 0.5-1 part by weight of thixotropic agent and 0.05-0.5 part by weight of leveling agent.
2. The halogen-free solder paste as claimed in claim 1, wherein: the weight of the Sn-X alloy powder is 100 wt%, and the weight of the X element is 0.1-2 wt%.
3. The halogen-free solder paste according to claim 1 or 2, wherein: and the X element in the Sn-X alloy powder is at least one of silver element, bismuth element, aluminum element and tellurium element.
4. The halogen-free solder paste as claimed in claim 1, wherein: the halogen-free activator is at least one of acetic acid, lactic acid, pyruvic acid, propionic acid, butyric acid, isobutyric acid, methanesulfonic acid and ethanesulfonic acid.
5. The halogen-free solder paste as claimed in claim 1, wherein: the organic solvent is at least one of alcohol ester dodeca, terpineol, tributyl citrate and butyl carbitol acetate.
6. The halogen-free solder paste as claimed in claim 1, wherein: the density of the liquid rosin resin is 1-1.1g/cm2The solid content of the liquid rosin resin is 48-50 wt%, and the pH value is 4.5-6.5.
7. The halogen-free solder paste as claimed in claim 1, wherein: the thixotropic agent is at least one of fumed silica, clay particles, hydrogenated castor oil and dodecahydroxystearic acid.
8. The halogen-free solder paste as claimed in claim 1, wherein: the leveling agent is at least one of polyether polyester modified organic siloxane and alkyl modified organic siloxane.
9. The halogen-free solder paste as claimed in claims 1 to 8, wherein: the preparation method of the halogen-free solder paste comprises the following steps:
the method comprises the following steps: accurately weighing the components of each raw material by using an analytical balance, and uniformly mixing an organic solvent, a halogen-free activating agent and liquid rosin resin in a stirrer to obtain a mixture A, wherein the rotating speed of the stirrer is 500-700rmp, and the stirring time is 10-20 min;
step two: placing Sn-X alloy powder into the mixture A prepared in the step one, and uniformly mixing in a homogenizer to obtain a mixture B, wherein the rotation speed of the homogenizer is 1000-1200rmp, and the homogenizing time is 3-5 min;
step three: and adding a thixotropic agent and a leveling agent into a homogenizer according to the condition of the mixture B, and uniformly mixing to obtain the halogen-free tin paste, wherein the rotation speed of the homogenizer is 1000-1200rmp, and the homogenizing time is 3-5 min.
10. The halogen-free solder paste as claimed in claim 9, wherein: the viscosity of the halogen-free tin paste at the rotation speed of 10rmp is 190-270 Pa.s/25 ℃.
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202010827877.3A CN111940947B (en) | 2020-08-17 | 2020-08-17 | Halogen-free tin paste and preparation method thereof |
PCT/CN2020/135738 WO2022036950A1 (en) | 2020-08-17 | 2020-12-11 | Halogen-free solder paste and preparation method therefor |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202010827877.3A CN111940947B (en) | 2020-08-17 | 2020-08-17 | Halogen-free tin paste and preparation method thereof |
Publications (2)
Publication Number | Publication Date |
---|---|
CN111940947A true CN111940947A (en) | 2020-11-17 |
CN111940947B CN111940947B (en) | 2022-05-13 |
Family
ID=73342557
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202010827877.3A Expired - Fee Related CN111940947B (en) | 2020-08-17 | 2020-08-17 | Halogen-free tin paste and preparation method thereof |
Country Status (2)
Country | Link |
---|---|
CN (1) | CN111940947B (en) |
WO (1) | WO2022036950A1 (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2022036950A1 (en) * | 2020-08-17 | 2022-02-24 | 惠州市源德智科技有限公司 | Halogen-free solder paste and preparation method therefor |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN115091079A (en) * | 2022-06-16 | 2022-09-23 | 深圳市兴鸿泰锡业有限公司 | Antioxidant solder paste and preparation method thereof |
CN115091074B (en) * | 2022-07-19 | 2023-08-15 | 深圳市鑫富锦新材料有限公司 | Solder paste with variable viscosity under heating and device for preventing solder paste from dripping |
CN117548901B (en) * | 2023-12-29 | 2024-07-05 | 深圳市华远金属有限公司 | Low-cavity halogen-free solder paste and preparation method thereof |
Citations (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1876311A (en) * | 2006-04-30 | 2006-12-13 | 北京市航天焊接材料厂 | Lead-free and halogen-free soldering paste and preparation method thereof |
CN101966632A (en) * | 2010-09-29 | 2011-02-09 | 广州瀚源电子科技有限公司 | Wash-free soldering flux for leadless low-temperature soldering paste and preparation method thereof |
CN102489898A (en) * | 2011-11-30 | 2012-06-13 | 昆山成利焊锡制造有限公司 | Low-silver lead-free flux paste and preparation method thereof |
CN102489899A (en) * | 2011-12-16 | 2012-06-13 | 昆山成利焊锡制造有限公司 | Lead-free soldering paste and preparation method thereof |
CN103706961A (en) * | 2012-09-28 | 2014-04-09 | 钟广飞 | Halogen-free tin paste |
CN103706968A (en) * | 2012-09-28 | 2014-04-09 | 钟广飞 | Halogen-free soldering flux |
JP2015039718A (en) * | 2013-08-22 | 2015-03-02 | 株式会社タムラ製作所 | Cold-heat shock flux composition, solder paste composition, and electronic circuit board |
CN104476016A (en) * | 2014-11-05 | 2015-04-01 | 苏州赛普特电子科技有限公司 | Lead-free and halogen-free soldering paste for semiconductors |
TW201607992A (en) * | 2014-08-29 | 2016-03-01 | 昇貿科技股份有限公司 | Solder flux composition |
CN106312361A (en) * | 2016-10-12 | 2017-01-11 | 哈尔滨工业大学(威海) | Ceramic substrate and copper clad foil low-temperature connecting soldering paste and production process thereof |
Family Cites Families (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101653876B (en) * | 2009-08-19 | 2012-05-02 | 浙江一远电子材料研究院 | Low-silver halogen free soldering paste |
CN101642855B (en) * | 2009-08-19 | 2012-02-22 | 浙江一远电子材料研究院 | Rear-earth-containing halogen free Sn-Ag-C series tinol |
CN102248321A (en) * | 2011-07-06 | 2011-11-23 | 江西理工大学 | Lead-free solder paste used for halogen-free LED (light-emitting diode) lamp |
CN102581523B (en) * | 2012-03-21 | 2015-06-17 | 北京鹏瑞中联科技有限公司 | Halogen-free solder paste |
CN104476007B (en) * | 2014-12-17 | 2015-10-28 | 东莞永安科技有限公司 | A kind of high-melting point lead-free halogen-free soldering tin paste and preparation method thereof |
CN104668818B (en) * | 2015-01-16 | 2017-07-07 | 北京鹏瑞中联科技有限公司 | A kind of semiconductor die package low voidage soldering paste and preparation method thereof |
JP6230674B2 (en) * | 2016-09-20 | 2017-11-15 | 株式会社タムラ製作所 | Lead-free solder alloy, electronic circuit board and electronic control device |
CN111940947B (en) * | 2020-08-17 | 2022-05-13 | 惠州市源德智科技有限公司 | Halogen-free tin paste and preparation method thereof |
-
2020
- 2020-08-17 CN CN202010827877.3A patent/CN111940947B/en not_active Expired - Fee Related
- 2020-12-11 WO PCT/CN2020/135738 patent/WO2022036950A1/en active Application Filing
Patent Citations (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1876311A (en) * | 2006-04-30 | 2006-12-13 | 北京市航天焊接材料厂 | Lead-free and halogen-free soldering paste and preparation method thereof |
CN101966632A (en) * | 2010-09-29 | 2011-02-09 | 广州瀚源电子科技有限公司 | Wash-free soldering flux for leadless low-temperature soldering paste and preparation method thereof |
CN102489898A (en) * | 2011-11-30 | 2012-06-13 | 昆山成利焊锡制造有限公司 | Low-silver lead-free flux paste and preparation method thereof |
CN102489899A (en) * | 2011-12-16 | 2012-06-13 | 昆山成利焊锡制造有限公司 | Lead-free soldering paste and preparation method thereof |
CN103706961A (en) * | 2012-09-28 | 2014-04-09 | 钟广飞 | Halogen-free tin paste |
CN103706968A (en) * | 2012-09-28 | 2014-04-09 | 钟广飞 | Halogen-free soldering flux |
JP2015039718A (en) * | 2013-08-22 | 2015-03-02 | 株式会社タムラ製作所 | Cold-heat shock flux composition, solder paste composition, and electronic circuit board |
TW201607992A (en) * | 2014-08-29 | 2016-03-01 | 昇貿科技股份有限公司 | Solder flux composition |
CN104476016A (en) * | 2014-11-05 | 2015-04-01 | 苏州赛普特电子科技有限公司 | Lead-free and halogen-free soldering paste for semiconductors |
CN106312361A (en) * | 2016-10-12 | 2017-01-11 | 哈尔滨工业大学(威海) | Ceramic substrate and copper clad foil low-temperature connecting soldering paste and production process thereof |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2022036950A1 (en) * | 2020-08-17 | 2022-02-24 | 惠州市源德智科技有限公司 | Halogen-free solder paste and preparation method therefor |
Also Published As
Publication number | Publication date |
---|---|
CN111940947B (en) | 2022-05-13 |
WO2022036950A1 (en) | 2022-02-24 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN111940947B (en) | Halogen-free tin paste and preparation method thereof | |
US6592020B1 (en) | Lead-free solder paste | |
US4960236A (en) | Manufacture of printed circuit board assemblies | |
CN110961829A (en) | Soldering flux and preparation method thereof, and solder paste and preparation method thereof | |
CN105014253A (en) | Lead-free tin solder paste and preparation method thereof | |
CN111590235B (en) | Low-dielectric-loss high-reliability soldering paste and preparation method thereof | |
CN108555474B (en) | Halogen-free environment-friendly lead-free tin paste and preparation method thereof | |
JP2019042805A (en) | Solder composition and electronic substrate | |
JP2017064758A (en) | Flux composition, solder composition and electronic substrate | |
CN101088695A (en) | SMT no-lead tinol | |
JP2015047616A (en) | Solder composition for jet dispenser | |
JP6895213B2 (en) | Method for manufacturing solder composition and electronic board | |
JP2500018B2 (en) | Low residue solder paste | |
US11992901B1 (en) | Lead-free and halogen-free solder paste | |
JP6136851B2 (en) | Solder flux and solder paste | |
CN110091094A (en) | A kind of halogen-free environmental solder(ing) paste and preparation method thereof | |
JP6940565B2 (en) | Solder composition and electronic board | |
CN109877484B (en) | No-clean and no-residue soldering paste and preparation method thereof | |
JP2019130566A (en) | Flux composition, solder composition and electronic substrate | |
EP0413540A2 (en) | Manufacture of printed circuit board assemblies | |
CN107695567A (en) | A kind of stamp-mounting-paper diode welds the preparation method of special solder(ing) paste | |
JPH01157798A (en) | Cream solder | |
CN114378483B (en) | Soldering flux for no-clean gold-tin soldering paste and preparation method and application thereof | |
CN105598602A (en) | Halogen-free soldering flux for high-activity tin wire and preparation method thereof | |
JP7066798B2 (en) | Solder composition |
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 | ||
GR01 | Patent grant | ||
GR01 | Patent grant | ||
CF01 | Termination of patent right due to non-payment of annual fee | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20220513 |