CN102785038B - Surface treatment method for protecting superfine raw solder powder, and superfine powder solder paste prepared according to method - Google Patents
Surface treatment method for protecting superfine raw solder powder, and superfine powder solder paste prepared according to method Download PDFInfo
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Abstract
The invention provides a surface treatment method for protecting superfine raw solder powder, a superfine powder solder paste prepared according to the method, and a preparation technology of the solder paste, and belongs to the technical field of welding materials. The surface treatment method comprises the following steps: a), preparing superfine raw solder powder; b), adopting an organic acid treating agent to treat oxide on the surface of superfine raw solder powder till the oxygen content of the superfine raw solder powder is lower than 150 ppm, so as to obtain a semi-finished product A;c), further treating the semi-finished product A with an anti-oxidant treating agent till a complex compound film is generated on the surface of the semi-finished product A, so as to obtain a semi-finished product B; and d), placing the semi-finished product B into a 30 to 40 DEG C oven for drying, and charging nitrogen during packing, so as to obtain the superfine solder powder. The superfine solder powder is compounded with scaling powder to form the superfine powder solder paste. According to the invention, the technical defects of more tin beads, poor wettability, narrow PCB printing interval, and high welding defective rate of the superfine powder solder paste in the prior art are overcome.
Description
Technical field
The present invention relates to a kind of processing method of solder powder and prepare, be specifically related to a kind of surface treatment method of ultra-fine solder powder and the superfine powder solder(ing) paste for preparing thus and the preparation technology of solder(ing) paste, belong to technical field of welding materials.
Background technology
At present, development in science and technology is maked rapid progress, and all electronic products are all towards compact trend development, and the appearance of network, communication, consumer electronics product thin space and ultra fine-pitch surface mounting technology has proposed higher challenge to solder(ing) paste.Under the correspondence of thin space, high precision die bonder, tiny element, superfine powder solder(ing) paste are used and are given birth to.
The solder powder model that is used in the market the solder(ing) paste preparation is Type2～Type4 powder, Type5～Type6 powder then is called superfine powder, the superfine powder model is larger, its particle diameter is less, its surface area is larger, and the solder powder oxygen content is just higher, and the superfine powder after the oxidation is followed the scaling powder generation chemical reaction of paste easily thus, thereby cause solder(ing) paste poor stability, weldability poor, and the tin ball occurs easily, the bad phenomenon such as cave in.These are perplexing SMT engineer such as problems such as the printing of thin space PCB and failure weldings always.Reduce the printing of thin space PCB and the again new revolution that failure welding becomes current SMT industry.For above-mentioned technical bottleneck, the oxygen content that effectively reduces in the ultra-fine solder powder is the printing issues of solution thin space PCB and the key of failure welding problem.
Treatment process report for ultra-fine solder powder in the prior art is also fewer.Publication number is the Chinese patent application of CN102357747A leadless soldering tin paste of having announced a kind of ultra-fine solder powder and preparation method thereof, but there is following problem in the processing of the ultra-fine solder powder of this patent: 1. the ratio of solder powder and surface conditioning agent is 88.5～87.0: 1.0～2.0, the consumption of surface conditioning agent is very few, can not be effectively when stirring operation the oxide on ultra-fine solder powder surface be removed, will easily be produced tin sweat(ing), wetability is poor, the failure welding rate is high phenomenon when the welding by the solder(ing) paste of its preparation.2. the solder powder after processing can not be deposited, and need to produce solder(ing) paste at once, has limited greatly the scope of application of ultra-fine solder powder.
The use of ultra-fine solder powder has become the trend of art technology development, and existing ultra-fine solder powder is little because of particle diameter, and the glass putty surface oxygen content is high, causes wetability poor.The oxide removal that it is surperficial improves its wetability through processing so the solder powder surface is essential, reduces tin sweat(ing), reduces printing and failure welding rate.
Summary of the invention
The inventor of the present patent application proves by experiment: when the oxygen content of solder powder surpassed 150ppm, in any case improve the prescription of scaling powder in the solder(ing) paste, tin sweat(ing), poor, the high defective of failure welding rate of wetability all can appear in the solder(ing) paste of producing.Solder powder Type5～Type6 oxygen content is all more than 150ppm as can be seen from Table 1.No matter the production process of ultra-fine solder powder is to adopt ultrasonic atomizatio method or centrifugal separation, all is difficult to Control for Oxygen Content with Type5～Type6 superfine powder below 150ppm.
The test of the unleaded Sn96.5Ag3.0Cu0.5 solder powder of table 1. different-grain diameter oxygen content
The present invention definition, the former powder of ultra-fine solder powder be not yet through the following treatment process of the present invention process and oxygen content above 150ppm and the particle diameter ultra-fine solder powder less than 25 μ m.
Tin sweat(ing) to occur in use many in order to solve the superfine powder solder(ing) paste, wetability is too poor, the problems such as failure welding rate height, the invention provides the treatment process of the former powder of a kind of ultra-fine solder powder, oxygen content in the former powder of the ultra-fine solder powder of decrease, thus make the use of 1～25 μ m superfine powder solder(ing) paste that is applicable to ultra fine-pitch PCB printing and welding become possibility.The present invention also provides solder(ing) paste and the preparation technology thereof by the ultra-fine solder powder preparation of described processing.
The oxygen content of ultra-fine solder powder declined to a great extent after the treatment process of ultra-fine solder powder provided by the present invention can make and process, be down to below the 150ppm, and all than prior art significantly lifting arranged with its solder(ing) paste for preparing in wetability, tin sweat(ing) and failure welding rate method.
One of the object of the invention provides the surface treatment method of the former powder of a kind of ultra-fine solder powder, and it comprises following four steps:
A) prepare the former powder of ultra-fine solder powder;
B) use the organic acid inorganic agent to process the oxide on the former powder of ultra-fine solder powder surface, make the oxygen content of the former powder of ultra-fine solder powder be lower than 150ppm and get semi-finished product A;
C) semi-finished product A is further processed with the anti-oxidant treatment agent, make semi-finished product A Surface Creation complex compound film, get semi-finished product B; The purpose of this step is to prevent that semi-finished product A again be oxidized.
D) semi-finished product B is put into 30～40 ℃ of baking boxs dryings, the inflated with nitrogen packing gets ultra-fine solder powder.
In the above-mentioned surface treatment method, described organic acid inorganic agent forms 100% by organic acid and organic solvent, and wherein the organic acid inorganic agent preferably contains the organic acid of 3.0%～15.0% weight fraction and the organic solvent of 97.0%～85.0% weight fraction.
Wherein, described organic acid is monoacid or binary acid, controls easily in order to make ultra-fine solder powder oxide on surface removal amount, and the organic acid in the described organic acid inorganic agent is preferably binary acid.For example its can in malonic acid, succinic acid, glutaric acid, suberic acid, decanedioic acid, tartaric acid, itaconic acid, dodecoic acid, tetradecylic acid, palmitic acid and the stearic acid one or more.Described organic solvent can for alcohols, ethers or ester class commonly used, be preferably as follows solvent: alcohols such as methyl alcohol, ethanol, isopropyl alcohol, n-butanol, 2-ethyl (1-) hexanol, diethylene glycol (DEG), terpinol, ethylene glycol, polyethylene glycol etc.; Ethers such as butyl oxide, diethylene glycol dimethyl ether, dibutyl ethylene glycol ether, diethylene glycol octyl ether etc.; Ester class such as Ethyl formate, butyl formate, amyl formate, ethyl acetate, pentaerythritol fatty acid ester etc., solvent can be one or more mixtures.
In the above-mentioned surface treatment method, described anti-oxidant treatment agent forms 100% by antioxidant and organic solvent, preferably contains the antioxidant of 1.0%～7.0% weight fraction and the organic solvent of 99.0%～93.0% weight fraction.Wherein, described antioxidant is one or more in BTA, methyl benzotriazazole, methylimidazole, ethyl imidazol(e), imidazoles, benzimidazole, tolimidazole, lactic acid and the disodium ethylene diamine tetraacetate.The antioxidant such as benzotriazole and imidazoles and superfine powder metallic atom form covalent bond and coordinate bond, generate network polymers, at the complex compound film of solder powder Surface Creation one deck densification, thereby the superfine powder surface are not again be oxidized at normal temperatures.Described organic solvent is low boiling effumability solvent, is preferably in methyl alcohol, ethanol, isopropyl alcohol, benzene, toluene, the acetoneand ethyl acetate one or more.
The former powder surface treatment method of above-mentioned ultra-fine solder powder preferred embodiment a kind of, the former powder surface treatment method of described ultra-fine solder powder comprises the steps:
A) prepare the former powder of ultra-fine solder powder;
B) with organic acid and solvent by weight (3.0%～15.0%): (97.0%～85.0%) stirs the organic pickling agent of preparation with dispersion machine; The former powder of ultra-fine solder powder is poured in the rustless steel container, pour again the organic acid treatment fluid into, slowly stirred 3～5 minutes with stirring rod, the treatment fluid addition is with the former powder of the ultra-fine solder powder of submergence and the former powder of ultra-fine solder powder is not exposed in the air be as the criterion, processing time decides according to organic acid type and consumption, preferred 1～3 day; Semi-finished product A finishes dealing with to get.
Supernatant liquor is separated, as use difficult volatile solvent treatment fluid, available effumability organic solvent cleans superfine powder, described easy volatile solvent be in hexane, cyclohexane, methyl alcohol, ethanol, isopropyl alcohol, Ethyl formate, butyl formate, ethyl acetate, benzene, toluene, the acetone one or more; Separation of supernatant after cleaning is finished; Cleaning and separation circuit can be repeatedly;
C) with antioxidant and solvent by weight (1.0%～7.0%): (99.0%～93.0%) stirs into homogeneous transparent liquid with dispersion machine; With step b) in the semi-finished product A that obtains pour in the rustless steel container, pour again antioxidant solution into, slowly stirred 3～5 minutes with stirring rod, the antioxidant addition is with submergence semi-finished product A and semi-finished product A is not exposed in the air be as the criterion, processing time decides according to type and the consumption of antioxidant, preferred 8～36h; Get semi-finished product B after finishing dealing with.
D) after antioxidant is finished dealing with supernatant is separated, it is dry that semi-finished product B is put into 30～40 ℃ of baking boxs, is preferably 2-3h drying time, can obtain ultra-fine solder powder after the drying.Ultra-fine solder powder can directly use or sealing bag packing inflated with nitrogen is preserved.
Two of the object of the invention provides a kind of superfine powder solder(ing) paste, this solder(ing) paste is mixed by ultra-fine solder powder and the scaling powder that above-mentioned surface treatment method prepares, and wherein said superfine powder solder(ing) paste forms 100% by the ultra-fine solder powder of 87～91% percetages by weight and the scaling powder of 9～13% percetages by weight.
Ultra-fine solder powder form is spherical in the above-mentioned solder(ing) paste, and its particle diameter is 1～25 μ m, more preferably 5～20 μ m.Above-mentioned ultra-fine solder powder is alloy or the alloy mixture that comprises tin, can be among SnAgCu, SnAg, SnZn, SnBi, SnCu, SnBiCu, SnBiAg and the SnBiCuSb one or more such as it.
Form 100% by the raw material of following weight fraction in the scaling powder in the superfine powder soldering paste described above:
Rosin 25～55%;
Thixotropic agent 3～15%;
Activating agent 3～15%; With
The solvent surplus.
Preferably, described scaling powder forms 100% by the raw material of following quality percentage composition:
Rosin 48%;
Thixotropic agent 8%;
Activating agent 8%;
Solvent 36%.
Wherein, above-mentioned thixotropic agent is rilanit special or organobentonite;
Above-mentioned activating agent is carbon number more than or equal to 8, saturated or unsaturated, the monobasic less than or equal to 30 or binary of fatty acids class, such as C
nH
2nO
2, C
nH
2n-2O
2, C
nH
2n-4O
2, C
nH
2n-6O
4, 8≤n≤30 wherein; Such as sad, dodecenylsuccinic acid, 18 carbon, three diluted acids, methyl stearic acid, lumequeic acid etc.; The perhaps halogen acid salt of organic amine;
The halogen acid salt of above-mentioned organic amine refers to hydrochloride or the hydrobromate of organic amine, and wherein organic amine can be primary amine, such as ethamine; Secondary amine is such as diethylamine; Tertiary amine is such as triethylamine; Also can use heterocyclic amine, such as pyridine; Aromatic amine is such as aniline; Fatty amine is such as cyclohexylamine; With the compound that contains two or more amino, such as diphenylguanidine.
Above-mentioned solvent is diethylene glycol hexyl ether, polyethylene glycol or aromatic ester.
The present invention also provides a kind of preparation method of superfine powder solder(ing) paste, and it comprises the steps:
1) surface treatment method according to the former powder of the present invention's ultra-fine solder powder described above obtains the ultra-fine solder powder of 1～25 μ m;
2) scaling powder and the ultra-fine solder powder of 1～25 μ m are fully mixed in de-airing mixer, namely get the superfine powder solder(ing) paste.
The superfine powder solder(ing) paste quality that the preparation method of the above-mentioned superfine powder solder(ing) paste of employing the present invention makes is high, and the failure welding rate is low, is applicable to thin space surface soldered technology.
Ultra-fine solder powder treatment process of the present invention and prepare the superfine powder solder(ing) paste compared with prior art has following technical advantage:
1) adopt the ultra-fine solder powder of the present invention can effectively reduce oxygen content in the solder powder to 150ppm, having overcome this field wants to solve and unsolved technical barrier for a long time, and the ultra-fine solder powder after processing can directly use also and can save backup its good stability.
2) adopt superfine powder solder(ing) paste that the ultra-fine solder powder for the treatment of process of the present invention prepares all significantly being better than 1 group of reference embodiment and 2 groups aspect wetability, tin sweat(ing) and the failure welding rate, and cause the reason of this performance difference to be that after all the present invention is to the process of surface treatment of solder powder.
3) ultra-fine solder powder is the technological trend of field of welding material development, utilizes the ultra-fine solder powder treatment process of the present invention to expand the range of application of ultra-fine solder powder, has important practical significance.
The specific embodiment
Following content is the further description of the present invention being done in conjunction with concrete preferred embodiment, can not assert that implementation of the present invention is confined to these explanations.For the general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, can also make some simple deduction or replace, all should be considered as belonging to protection scope of the present invention.Following embodiment and reference embodiment employed " part " refer to weight portion, and percentage refers to percetage by weight.
The surface treatment method of the former powder of the ultra-fine solder powder of embodiment 1～embodiment 6 the present invention
Step is as follows:
A) prepare the former powder of ultra-fine solder powder;
B) use the organic acid inorganic agent to process the oxide on the former powder of ultra-fine solder powder surface, make the oxygen content of the former powder of ultra-fine solder powder be lower than 150ppm and get semi-finished product A;
C) semi-finished product A is further processed with the anti-oxidant treatment agent, make super semi-finished product A Surface Creation complex compound film, get semi-finished product B; The purpose of this step is to prevent that semi-finished product A again be oxidized.
D) semi-finished product B is put into 30～40 ℃ of baking boxs dryings, the inflated with nitrogen packing gets ultra-fine solder powder.Described organic acid inorganic agent and processing time, described antioxidant and anti-oxidant treatment were with reference to table 3 with reference to table 2.
The organic acid on the surface of the former powder of the ultra-fine solder powder of table 2 embodiment of the invention 1-6 is processed
The antioxidant on the surface of the former powder of the ultra-fine solder powder of table 3 embodiment of the invention 1-6 is processed
In order to make those skilled in the art fully understand the surface treatment method of the former powder of the ultra-fine solder powder of the present invention and the preparation technology of ultra-fine solder(ing) paste, only details are as follows with the process of surface treatment of the former powder of ultra-fine solder powder and the preparation technology of ultra-fine solder(ing) paste among embodiment 1 and the embodiment 3 for the inventor, and the preparation technology of the process of surface treatment of the former powder of ultra-fine solder powder and ultra-fine solder(ing) paste can be with reference to technique described in embodiment 1 and the embodiment 3 among other embodiment.
The surface treatment of the former powder of ultra-fine solder powder among the embodiment 1
At first, with 10 weight portion succinic acid, 90 parts by weight of ethanol with the dispersion machine organic pickling agent of preparation that stirs.Then be that the former powder of 1～25 ultra-fine solder powder of μ m Sn96.5Ag3.0Cu0.5 is poured in the rustless steel container with particle diameter, pour again the organic acid treatment fluid of aforementioned preparation into, the treatment fluid addition is with the former powder of the ultra-fine scolding tin of submergence and the former powder of ultra-fine scolding tin is not exposed in the air be as the criterion, slowly stir static processing 24h after 3～5 minutes with stirring rod, after finishing dealing with supernatant liquor poured out and to obtain semi-finished product A; Pour the 3% methylimidazole ethanolic solution that stirs into, addition is with submergence semi-finished product A and semi-finished product A is not exposed in the air be as the criterion again, and slowly stirs static processing 8h after 5 minutes with stirring rod; Pour out supernatant liquor after finishing dealing with and can obtain semi-finished product B, semi-finished product B is put into 35 ℃ of dry 2h of baking oven, can obtain particle diameter is the ultra-fine solder powder of 1～25 μ m.The former powder process of surface treatment of the ultra-fine solder powder of the present invention is finished.
The processing of the former powder of ultra-fine solder powder among the embodiment 3
At first, with 8 weight portion glutaric acids, 92 weight portion dibutyl ethylene glycol ethers with the dispersion machine organic pickling agent of preparation that stirs.Then be that the former powder of 1～25 ultra-fine solder powder of μ m Sn99.0Ag0.3Cu0.7 is poured in the rustless steel container with particle diameter, pour again the organic acid treatment fluid of aforementioned preparation into, the treatment fluid addition is with the former powder of the ultra-fine scolding tin of submergence and the former powder of ultra-fine scolding tin is not exposed in the air be as the criterion, slowly stir static processing 50h after 3～5 minutes with stirring rod, after finishing dealing with supernatant liquor poured out and to obtain semi-finished product A; Pour 5% methylimidazole, 50% acetone, 45% ethanolic solution that stirs into, addition is with submergence semi-finished product A and semi-finished product A is not exposed in the air be as the criterion again, and slowly stirs static processing 20h after 5 minutes with stirring rod; Pour out supernatant liquor after finishing dealing with and can obtain semi-finished product B, semi-finished product B is put into 35 ℃ of dry 2h of baking oven, can obtain particle diameter is the ultra-fine solder powder of 1～25 μ m.The former powder process of surface treatment of the ultra-fine solder powder of the present invention is finished.
Embodiment 7 superfine powder solder(ing) pastes of the present invention and preparation method thereof
The preparation method is as follows:
The prescription of scaling powder: scaling powder forms 100% by the raw material of following quality percentage composition:
Rosin 48%;
Rilanit special 8%;
Diethylamine hydrobromide 8%;
Diethylene glycol hexyl ether 36%.
The preparation of scaling powder: the rilanit special of the diethylene glycol hexyl ether of the rosin of 48 mass fractions, 36 mass fractions, 8 mass fractions weighed up put into rustless steel container and be heated to 150 ℃, and be stirred to fully fusing.Then, make rustless steel container cool to 130 ℃, then the diethylamine hydrobromide with 8 mass fractions joins in the rustless steel container, and is stirred to fully fusing.Cooling namely gets the used scaling powder of present embodiment, puts into 2 ℃ of freezers and saves backup
The preparation of solder(ing) paste: with the weight ratio of the dried ultra-fine solder powder 88.5% of embodiment 1 gained and scaling powder 11.5% stirring at low speed 7 minutes in de-airing mixer, the inflated with nitrogen middling speed stirred 40 minutes again, ultra-fine solder powder and scaling powder are fully mixed, vacuumize again middling speed and stirred 7 minutes, can make superfine powder solder(ing) paste of the present invention.
Embodiment 8 superfine powder solder(ing) pastes of the present invention and preparation method thereof
The preparation method is with embodiment 7, as different from Example 7,
The preparation of solder(ing) paste: with the weight ratio of the dried ultra-fine solder powder 88.5% of embodiment 3 gained and scaling powder 11.5% stirring at low speed 8 minutes in de-airing mixer, the inflated with nitrogen middling speed stirred 30-50 minute again, ultra-fine solder powder and scaling powder are fully mixed, vacuumize again middling speed and stirred 8 minutes, can make superfine powder solder(ing) paste of the present invention.
Reference embodiment 1
Use the former powder of ultra-fine solder powder (Sn96.5Ag3.0Cu0.5) of 1～25 μ m to reach identical with scaling powder embodiment 1 in the solder(ing) paste, the former powder of ultra-fine solder powder is also identical with embodiment 1 with the mixed proportion of scaling powder in the solder(ing) paste, and difference only is that the former powder of ultra-fine solder powder is through process of surface treatment of the present invention among the reference embodiment 1.
Reference embodiment 2
Use the former powder of ultra-fine solder powder (1～25 μ m Sn99.0Ag0.3Cu0.7) and identical with scaling powder embodiment 2 in the solder(ing) paste, the former powder of ultra-fine solder powder is also identical with embodiment 2 with the mixed proportion of scaling powder in the solder(ing) paste, and difference only is that the former powder of ultra-fine solder powder is through process of surface treatment of the present invention among the reference embodiment 2.
The performance test of the ultra-fine solder(ing) paste that test example one the present invention is prepared
According to industry standard to the present invention to ultra-fine soldering paste carry out performance test and with reference embodiment 1 and reference embodiment 2 in soldering paste carry out performance comparison, the result is as shown in table 3 for its performance comparison.
Soldering paste characteristic test among table 4 embodiment 1-6 and the reference embodiment example 1-2
Oxygen content contrast before and after processing,
*P＜0.01; Embodiment compares with reference,
#P＜0.01
As shown in table 4, process the solder powder oxygen content of front and back from adopting treatment process of the present invention, treatment process of the present invention can significantly reduce the oxygen content in the solder powder, and oxygen content difference has the utmost point significant difference (P＜0.01) on the statistical significance before and after processing.From adopting solder(ing) paste and scaling powder to prepare the performance test of solder(ing) paste, the tin sweat(ing) of the superfine powder solder(ing) paste among the reference embodiment is many, is lower than 2 grade standards that JIS requires, and wetability also is lower than 2 grade standards that JIS requires, and the failure welding rate is higher.And the tin sweat(ing) of the superfine powder tin cream of making according to the present invention and preparation method all reaches more than 2 grades, and wetability also reaches more than 2 grades, and the failure welding rate reduces greatly.As seen, the preparation-obtained solder(ing) paste of the present invention all significantly is being better than 1 group of reference embodiment and 2 groups aspect wetability, tin sweat(ing) and the failure welding rate, and causes the reason of this performance difference to be that after all the present invention is to the process of surface treatment of solder powder.
Above-described embodiment only is preferred embodiment of the present invention, and it is not that technical scope of the present invention is imposed any restrictions, so any trickle modification of every foundation technical spirit of the present invention, equivalent variations and modification all still belong in the scope of technical solution of the present invention.
Claims (7)
1. the surface treatment method of the former powder of ultra-fine solder powder, the former powder of described ultra-fine solder powder is one or more among SnAgCu, SnAg, SnZn, SnBi, SnCu, SnBiCu, SnBiAg and the SnBiCuSb, the particle diameter of the former powder of described ultra-fine solder powder is 1～25 μ m, it is characterized in that this surface treatment method comprises the steps:
A) prepare the former powder of ultra-fine solder powder;
B) use the organic acid inorganic agent to process the oxide on the former powder of ultra-fine solder powder surface, make the oxygen content of the former powder of ultra-fine solder powder be lower than 150ppm and get semi-finished product A, wherein, described organic acid inorganic agent forms 100% by the component of following weight percentage:
Organic acid 3.0%～15.0%, wherein said organic acid are one or more in malonic acid, succinic acid, glutaric acid, suberic acid, decanedioic acid, tartaric acid, itaconic acid, dodecoic acid, tetradecylic acid, palmitic acid and the stearic acid; With
Solvent 97.0%～85.0%, described solvent are one or more in methyl alcohol, ethanol, isopropyl alcohol, n-butanol, 2-ethyl-1-hexanol, diethylene glycol (DEG), terpinol, ethylene glycol, polyethylene glycol, butyl oxide, diethylene glycol dimethyl ether, dibutyl ethylene glycol ether, diethylene glycol octyl ether, Ethyl formate, butyl formate, amyl formate, ethyl acetate and the pentaerythritol fatty acid ester;
C) semi-finished product A is further processed with the anti-oxidant treatment agent, make semi-finished product A Surface Creation complex compound film, get semi-finished product B, wherein, described anti-oxidant treatment agent forms 100% by the component of following weight percentage:
Antioxidant 1.0%～7.0%, wherein said antioxidant are one or more in BTA, methyl benzotriazazole, methylimidazole, ethyl imidazol(e), imidazoles, benzimidazole, tolimidazole, lactic acid and the disodium ethylene diamine tetraacetate; With
Solvent 99.0%～93.0%, wherein said solvent are one or more in methyl alcohol, ethanol, isopropyl alcohol, benzene, toluene, the acetoneand ethyl acetate;
D) semi-finished product B is put into 30～40 ℃ of baking boxs dryings, the inflated with nitrogen packing, getting particle diameter is the ultra-fine solder powder of 1～25 μ m.
2. the surface treatment method of the former powder of ultra-fine solder powder according to claim 1 is characterized in that, the particle diameter of the former powder of described ultra-fine solder powder is 5～20 μ m, and the particle diameter of described ultra-fine solder powder is 5～20 μ m.
3. the surface treatment method of the former powder of ultra-fine solder powder according to claim 1, it is characterized in that, described step b) comprises the steps: the former powder of ultra-fine solder powder is poured in the rustless steel container, pour again the organic acid inorganic agent into, slowly stirred 3～5 minutes with stirring rod, the addition of organic acid inorganic agent is with the former powder of the ultra-fine solder powder of submergence and the former powder of ultra-fine solder powder is not exposed in the air be as the criterion, and the processing time of described organic acid inorganic agent is 24h-72h.
4. the surface treatment method of the former powder of ultra-fine solder powder according to claim 1, it is characterized in that, described step c) comprising the steps: step b) the semi-finished product A that obtains pours in the rustless steel container, pour again the antioxidant inorganic agent into, slowly stirred 3～5 minutes with stirring rod, the addition of anti-oxidant treatment agent is with submergence semi-finished product A and semi-finished product A is not exposed in the air be as the criterion, and the processing time of described anti-oxidant treatment agent is 8h-36h.
5. the surface treatment method of the former powder of ultra-fine solder powder as claimed in claim 1 is characterized in that described steps d) in dry required time be 2-3h.
6. superfine powder solder(ing) paste that is formed by ultra-fine solder powder claimed in claim 1 and scaling powder, it is characterized in that: described superfine powder solder(ing) paste forms 100% by the component of following weight percentage:
7. the preparation method of a superfine powder solder(ing) paste claimed in claim 6 is characterized in that, this preparation method comprises the steps:
1) surface treatment method according to the former powder of ultra-fine solder powder claimed in claim 1 obtains the ultra-fine solder powder of 1～25 μ m;
2) scaling powder and the ultra-fine solder powder of 1～25 μ m are fully mixed in de-airing mixer, namely get the superfine powder solder(ing) paste.
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| WO2017122341A1 (en) * | 2016-01-15 | 2017-07-20 | 千住金属工業株式会社 | Flux |
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| CN111482733B (en) * | 2020-04-21 | 2022-04-01 | 浙江力强科技有限公司 | Anti-oxidation soldering flux for tinned copper strip coating and preparation method thereof |
| CN111872599B (en) * | 2020-07-01 | 2022-02-22 | 潮州三环（集团）股份有限公司 | Modified tin powder and tin paste |
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| CN115709349A (en) * | 2021-08-20 | 2023-02-24 | 北京小米移动软件有限公司 | Tin powder, preparation method of tin powder, tin paste, welding method of circuit board and circuit board |
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| JP4362303B2 (en) * | 2003-03-28 | 2009-11-11 | シチズンホールディングス株式会社 | Thermoelectric element and manufacturing method thereof |
| JP2005066672A (en) * | 2003-08-27 | 2005-03-17 | Nippon Handa Kk | Solder alloy powder manufacturing method, solder powder and solder paste thereby |
| CN101269445A (en) * | 2007-03-21 | 2008-09-24 | 长沙泰辉网络科技有限公司 | Stannum-copper binary alloy leadless solder paste |
| CN101244491B (en) * | 2008-03-21 | 2010-09-29 | 天津市青禾科技发展有限公司 | Lead-free solder solder paste for electronic industry and method for manufacturing soldering fluid |
| CN102357747B (en) * | 2011-09-06 | 2016-08-10 | 云南锡业锡材有限公司 | Leadless soldering tin paste of ultra-fine solder powder and preparation method thereof |
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