CN103173752B - Plating solution formula, plating solution preparation method and application - Google Patents
Plating solution formula, plating solution preparation method and application Download PDFInfo
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- CN103173752B CN103173752B CN201310123705.8A CN201310123705A CN103173752B CN 103173752 B CN103173752 B CN 103173752B CN 201310123705 A CN201310123705 A CN 201310123705A CN 103173752 B CN103173752 B CN 103173752B
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Abstract
The invention relates to a plating solution formula, a plating solution preparation method and application. The plating solution prepared by the plating solution formula can be directly used for chemically plating tin on an oxygen-free copper matrix, and the plating solution formula comprises: 15-25? g/L, 85-95% of thiourea? g/L, 6-10% hydrochloric acid? mL/L, 75-85% sodium chloride? g/L, the purities of the stannous chloride, the thiourea and the sodium chloride are analytically pure, and the hydrochloric acid is 36-38% analytically pure. The plating solution prepared by the invention can directly chemically plate a compact tin layer on the oxygen-free copper matrix, has simple and quick operation, does not need to use an electroplating form, solves the problem that the oxygen-free copper matrix is easy to oxidize to achieve the effect of protecting the copper matrix, and simultaneously improves the weldability of the oxygen-free copper matrix. The invention also relates to a plating solution preparation method and application of the plating solution prepared according to the plating solution formula. < | 1- >)
Description
Technical field
The present invention relates to a kind of field of metal surface treatment technology, relate in particular to a kind of electroplate liquid formulation, platingLiquid and preparation method thereof and application.
Background technology
Metallic tin is a kind of silvery white, the good metal of plasticity, and metallic tin is because welding performance is fine,And be widely used in the solderable coating of electronic component and printed board; Meanwhile, metallic tin is at atmosphereIn very stable, there is higher chemical stability, work hardly with sulphur and sulfide. ?Chemical plating stannum on oxygen-free copper matrix, one side can improve the solderability of matrix, on the other hand canEffectively to protect matrix, avoid oxygen-free copper surface oxidation.
Summary of the invention
In view of this, be necessary to provide a kind of electroplate liquid formulation, plating solution preparation method and application, its formationDirectly chemical plating stannum on oxygen-free copper matrix of plating solution, and directly on oxygen-free copper matrix chemistryThe tin layer of plating one deck densification, solves oxygen-free copper matrix oxidizable and reach the effect of protection copper matrix, meanwhile, improved the solderability of oxygen-free copper matrix.
The present invention is achieved in that a kind of electroplate liquid formulation, and the plating solution of its preparation can be directly at oxygen-free copperChemical plating stannum on matrix, described electroplate liquid formulation comprises: stannous chloride 15 ~ 25g/L, thiocarbamide 85~ 95g/L, hydrochloric acid 6 ~ 10mL/L, sodium chloride 75 ~ 85g/L, described stannous chloride, instituteThe purity of stating thiocarbamide, described sodium chloride be analyze pure, the analysis that described hydrochloric acid is 36%～38%Pure.
The present invention also provides a kind of plating solution preparation method, and it adopts above-mentioned electroplate liquid formulation to prepare plating solution, instituteStating plating solution preparation method comprises the following steps:
Toward the deionized water of pouring 1/3 container volume specification in vessel into, container volume specification is according to oxygen-free copperBaseBody can be immersed in the principle in container completely;
By the formula ratio of described electroplate liquid formulation, take described stannous chloride, described thiocarbamide, described chlorinationSodium, described hydrochloric acid;
Described vessel are put into water-bath heating slot and be heated to 60 DEG C, successively by described stannous chloride, instituteState thiocarbamide, described hydrochloric acid, described sodium chloride and pour in described vessel and fully dissolve, then add surplusThe deionized water of remaining volume, maintains an equal level the graticule that solution face is corresponding with containers size, and forming can be straightBe connected on the described plating solution of chemical plating stannum on oxygen-free copper matrix.
The present invention also provides a kind of plating solution application, and its plating solution of making for above-mentioned plating solution preparation method is directChemical plating stannum application on oxygen-free copper matrix.
As the further improvement of such scheme, the applying step of described plating solution application is as follows:
A, oxygen-free copper matrix is fully deoiled;
B, described oxygen-free copper matrix is carried out to pickling, described oxygen-free copper matrix is put into pickling electrolyte,Part is put into described pickling electrolyte 5 ~ 15 seconds, then carry out clearly in mobile deionized waterWash 10 ~ 30 seconds, go to next step;
C, the oxygen-free copper matrix after cleaning is put into rapidly to described plating solution and carried out chemical plating, institute in processStating plating solution needs constantly to stir the appearance to prevent precipitation, after chemical plating finishes, going of flowingCleaning components 10 ~ 30 seconds in ionized water, and go to next step;
D, in absolute ethyl alcohol, plating piece is dewatered 2～5 seconds, and plating piece is dry.
Preferably, oxygen-free copper matrix is fully deoiled, be divided into two step processing: first, organic deoiling,It is the acetone soln of 40 ~ 60 DEG C that oxygen-free copper matrix is put into temperature, soaks 15 ~ 20 minutes; ItsInferior, chemical deoiling and degreasing, it is that 40 ~ 60 DEG C of chemistry go that the oxygen-free copper matrix after immersion treatment is put into temperatureIn oil solution, ultrasonic immersion 15 ~ 20 minutes, by the oxygen-free copper matrix after immersion treatment in hot waterSoak and after 0.5 ~ 1 minute, put in the container that fills cold water and rinse (0.25～0.5) minute, turnTo next step.
Again preferably, the proportioning of described chemical deoiling and degreasing solution is: sodium carbonate (Na2CO3）20g/l, sodium phosphate (Na3PO4) 20g/l, emulsifying agent (OP-10) 3g/l.
Preferably, in step C, during chemical plating, described bath temperature: 55～65 DEG C, when plating solutionBetweenDetermine according to thickness of coating and tin layer deposition velocity 0.60～1.00 μ m/min.
Preferably, in step D, in absolute ethyl alcohol, plating piece is dewatered 2～5 seconds, with nitrogen generalAfter drying up, plating piece puts into baking oven, dry 10 ~ 20min under 80～100 DEG C of conditions.
Preferably, in step B, described pickling electrolyte is prepared by following composition and proportioning: 45 ~ 60Sulfuric acid (the H of ml/L2SO4), the chromium oxide (CrO of (250～300) g/L3）。
The invention has the advantages that: provide a kind of electroplate liquid formulation, plating solution preparation method and application, its phaseThe plating solution closing, directly the tin layer of chemical plating one deck densification on oxygen-free copper matrix, simple to operateFast, without using plating form; Solve oxygen-free copper matrix oxidizable and reach protection copper matrixEffect, meanwhile, improved the solderability of oxygen-free copper matrix.
Compared with preparing tin layer with traditional electro-plating method, on oxygen-free copper matrix, chemical plating stannum is without powering upOperation, has solved such as covering (the copper cabling on circuit board of discontinuous oxygen-free copper matrix on copper circuit boardBetween non-conductive) do not carrying out completing under interconnected situation the object of tin coating simultaneously, fastThe field that makes circuit provides shortcut. Meanwhile, chemical plating stannum operation letter on oxygen-free copper matrixSingle, cost of manufacture is low, and reaction fast, can be prepared fine and close tin bismuth chemical deposit fast.
Detailed description of the invention
In order to make object of the present invention, technical scheme and advantage clearer, below in conjunction with enforcementExample, is further elaborated to the present invention. Should be appreciated that concrete reality described hereinExecute example only in order to explain the present invention, be not intended to limit the present invention.
[embodiment 1]
Prepare chemical tin plating liquor (being plating solution): take stannous chloride by formula ratio (being electroplate liquid formulation), thiocarbamide, sodium chloride, hydrochloric acid, first toward the deionized water of pouring 1/3 volume in vessel into, by vesselPut into water-bath heating slot and be heated to 60 DEG C, successively by stannous chloride, thiocarbamide, hydrochloric acid, chlorinationSodium is poured in vessel and is fully dissolved, then adds the deionized water of residual volume, and container is put into waterIn bath heating tank, being heated to 60 DEG C stablizes rear for subsequent use. Bath composition is: stannous chloride 20g/L, sulphurUrea 90g/L, hydrochloric acid 7.5mL/L, sodium chloride 80g/L.
Prepare chemical degreasing solution, according to formula weighing sodium carbonate, sodium phosphate, emulsifier op-10, joinSystemBecome solution and be cooled to room temperature, the chemical deoiling and degreasing solution composition and the content that are mixed with are: sodium carbonate20g/L, sodium phosphate 20g/L, emulsifying agent (OP-10) 3g/L.
Prepare oxygen-free copper Acidwash solution (being pickling electrolyte): measure chromium oxide by formula, pour into approximatelyIn the deionized water of 2/3 volume, dissolve, sulfuric acid is added slowly and stir cooling, finally according toSolution is prepared volume and is injected a small amount of deionized water. Acid solution component is: sulfuric acid (H2SO4）50ml/L, chromium oxide (CrO3）275g/L。
Tie up oxygen-free copper part with copper conductor, it is that the acetone soln of 50 DEG C soaks that part is put into temperature15 minutes; By the oxygen-free copper matrix after immersion treatment in hot water, soak put into after 30 seconds fill coldIn the container of water and rinse 15 seconds; Part is put into chemical deoiling and degreasing solution, and utilize ultrasonic enterRow cleans, and ultrasonic power can take the circumstances into consideration to regulate according to actual conditions, scavenging period 15 minutes, subsequentlyPart is put into hot water to be soaked 30 seconds;
Oxygen-free copper matrix is carried out to pickling, oxygen-free copper matrix is put into pickling electrolyte, part is put intoIn Acidwash solution 10 seconds, then in mobile deionized water, clean 15 seconds, go to next stepSuddenly;
Oxygen-free copper matrix after cleaning is put into rapidly to chemical tin plating liquor and carry out chemical plating, molten in processLiquid needs constantly to stir the appearance to prevent precipitation; Bath temperature: 60 DEG C, hold time: 5mIn, after chemical plating finishes, cleaning components 30 seconds in mobile deionized water, and go to nextStep.
In absolute ethyl alcohol, plating piece is dewatered 5 seconds. After plating piece being dried up with nitrogen, put into baking oven,Dry 20min under 100 DEG C of conditions.
Finally, through microscopic appearance, coating even compact, is 4. through step instrument test thickness of coating02 μ m welds test to plating piece on the heating platform that is set to 120 DEG C, and plating piece hasSolderability preferably; So far, a kind of on oxygen-free copper matrix the flow process of chemical plating stannum all complete。
[embodiment 2]
Prepare chemical tin plating liquor: take stannous chloride, thiocarbamide, sodium chloride, hydrochloric acid by formula ratio, firstToward the deionized water of pouring 1/3 volume in vessel into, vessel are put into water-bath heating slot and be heated to 60 DEG C, successively stannous chloride, thiocarbamide, hydrochloric acid, sodium chloride are poured in vessel and fully dissolved, thenAdd the deionized water of residual volume, by container put into water-bath heating slot be heated to 60 DEG C stableFor subsequent use afterwards. Bath composition is: stannous chloride 15g/L, thiocarbamide 85g/L, hydrochloric acid 6mL/L, chlorineChange sodium 75g/L.
Prepare chemical degreasing solution, according to formula weighing sodium carbonate, sodium phosphate, emulsifier op-10, joinMake solution and be cooled to room temperature, the chemical deoiling and degreasing solution composition and the content that are mixed with are: carbonic acidSodium 20g/L, sodium phosphate 20g/L, emulsifying agent (OP-10) 3g/L.
Prepare oxygen-free copper Acidwash solution: measure chromium oxide by formula, pour the deionized water of approximately 2/3 volume intoMiddle dissolving, sulfuric acid is added slowly and stir cooling, finally according to solution prepare volume injectA small amount of deionized water. Acid solution component is: sulfuric acid (H2SO4) 50ml/L, chromium oxide (CrO3）275g/L。
Tie up oxygen-free copper part with copper conductor, it is that the acetone soln of 50 DEG C soaks that part is put into temperature15 minutes; By the oxygen-free copper matrix after immersion treatment in hot water, soak put into after 30 seconds fill coldIn the container of water and rinse 15 seconds; Part is put into chemical deoiling and degreasing solution, and utilize ultrasonic enterRow cleans, and ultrasonic power can take the circumstances into consideration to regulate according to actual conditions, scavenging period 15 minutes, subsequentlyPart is put into hot water to be soaked 30 seconds.
Oxygen-free copper matrix is carried out to pickling, oxygen-free copper matrix is put into pickling electrolyte, part is put intoIn Acidwash solution 10 seconds, then in mobile deionized water, clean 15 seconds, go to next stepSuddenly.
Oxygen-free copper matrix after cleaning is put into rapidly to chemical tin plating liquor and carry out chemical plating, molten in processLiquid needs constantly to stir the appearance to prevent precipitation; Bath temperature: 60 DEG C, hold time: 5mIn, after chemical plating finishes, cleaning components 30 seconds in mobile deionized water, and go to nextStep.
In absolute ethyl alcohol, plating piece is dewatered 5 seconds. After plating piece being dried up with nitrogen, put into baking oven,Dry 20min under 100 DEG C of conditions.
Finally, through microscopic appearance, coating even compact, is 3. through step instrument test thickness of coating74 μ m, show that the concentration of chemical plating stannum solution is straight in the indeclinable situation of all the other processing technologysConnect the thickness that affects coating. On the heating platform that is set to 120 DEG C, plating piece is welded to test, plating piece has good solderability.
[embodiment 3]
Prepare chemical tin plating liquor: take stannous chloride, thiocarbamide, sodium chloride, hydrochloric acid by formula ratio, firstToward the deionized water of pouring 1/3 volume in vessel into, vessel are put into water-bath heating slot and be heated to 60 DEG C, successively stannous chloride, thiocarbamide, hydrochloric acid, sodium chloride are poured in vessel and fully dissolved, thenAdd residual volume go fromSub-water, by container put into water-bath heating slot be heated to 60 DEG C for subsequent use after stable. Bath composition is: stannous chloride 25g/L, thiocarbamide 90g/L, hydrochloric acid 8mL/L, sodium chloride 80g/L.
Prepare chemical degreasing solution, according to formula weighing sodium carbonate, sodium phosphate, emulsifier op-10, joinMake solution and be cooled to room temperature, the chemical deoiling and degreasing solution composition and the content that are mixed with are: carbonic acidSodium 20g/L, sodium phosphate 20g/L, emulsifying agent (OP-10) 3g/L.
Prepare oxygen-free copper Acidwash solution: measure chromium oxide by formula, pour the deionized water of approximately 2/3 volume intoMiddle dissolving, sulfuric acid is added slowly and stir cooling, finally according to solution prepare volume injectA small amount of deionized water. Acid solution component is: sulfuric acid (H2SO4) 50ml/L, chromium oxide (CrO3）275g/L。
Tie up oxygen-free copper part with copper conductor, it is that the acetone soln of 50 DEG C soaks that part is put into temperature15 minutes; By the oxygen-free copper matrix after immersion treatment in hot water, soak put into after 30 seconds fill coldIn the container of water and rinse 15 seconds; Part is put into chemical deoiling and degreasing solution, and utilize ultrasonic enterRow cleans, and ultrasonic power can take the circumstances into consideration to regulate according to actual conditions, scavenging period 15 minutes, subsequentlyPart is put into hot water to be soaked 30 seconds.
Oxygen-free copper matrix is carried out to pickling, oxygen-free copper matrix is put into pickling electrolyte, part is put intoIn Acidwash solution 10 seconds, then in mobile deionized water, clean 15 seconds, go to next stepSuddenly.
Oxygen-free copper matrix after cleaning is put into rapidly to chemical tin plating liquor and carry out chemical plating, molten in processLiquid needs constantly to stir the appearance to prevent precipitation; Bath temperature: 60 DEG C, hold time: 5mIn, after chemical plating finishes, cleaning components 30 seconds in mobile deionized water, and go to nextStep.
In absolute ethyl alcohol, plating piece is dewatered 5 seconds. After plating piece being dried up with nitrogen, put into baking oven,Dry 20min under 100 DEG C of conditions.
Finally, through microscopic appearance, coating even compact, is 4. through step instrument test thickness of coating26 μ m, show that the concentration of chemical plating stannum solution is straight in the indeclinable situation of all the other processing technologysConnect the thickness that affects coating. On the heating platform that is set to 120 DEG C, plating piece is welded to test, plating piece has good solderability.
Known in conjunction with above-described embodiment: plating solution of the present invention, directly chemical plating on oxygen-free copper matrixThe tin layer of one deck densification, simple and quick, without using plating form, solve oxygen-free copper baseBody is oxidizable and reach the effect of protection copper matrix, meanwhile, has improved welding of oxygen-free copper matrixProperty.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, allAny amendment of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., all shouldWithin being included in protection scope of the present invention.
Claims (9)
1. an electroplate liquid formulation, it is characterized in that, directly chemical plating stannum on oxygen-free copper matrix of the plating solution of its preparation, described electroplate liquid formulation comprises: stannous chloride 15～25g/L, thiocarbamide 85～95g/L, hydrochloric acid 6～10mL/L, sodium chloride 75～85g/L, it is pure that the purity of described stannous chloride, described thiocarbamide, described sodium chloride is analysis, and the analysis that described hydrochloric acid is 36%～38% is pure.
2. a plating solution preparation method, is characterized in that, it adopts electroplate liquid formulation as claimed in claim 1 to prepare plating solution, and described plating solution preparation method comprises the following steps:
Toward the deionized water of pouring 1/3 container volume specification in vessel into, container volume specification can be immersed in the principle in container completely according to oxygen-free copper matrix;
By the formula ratio of described electroplate liquid formulation, take described stannous chloride, described thiocarbamide, described sodium chloride, described hydrochloric acid;
Described vessel are put into water-bath heating slot and be heated to 60 DEG C, successively described stannous chloride, described thiocarbamide, described hydrochloric acid, described sodium chloride are poured in described vessel and fully dissolved, add again the deionized water of residual volume, the graticule that solution face is corresponding with containers size is maintained an equal level, form the directly described plating solution of chemical plating stannum on oxygen-free copper matrix.
3. a plating solution application, is characterized in that, the directly chemical plating stannum application on oxygen-free copper matrix of its plating solution of making for plating solution preparation method as claimed in claim 2.
4. plating solution application as claimed in claim 3, is characterized in that, the applying step of described plating solution application is as follows:
A, oxygen-free copper matrix is fully deoiled;
B, described oxygen-free copper matrix is carried out to pickling, described oxygen-free copper matrix is put into pickling electrolyte, part is put into described pickling electrolyte 5～15 seconds, then in mobile deionized water, clean 10～30 seconds, go to next step;
C, the oxygen-free copper matrix after cleaning is put into rapidly to described plating solution and carried out chemical plating, plating solution described in process needs constantly to stir the appearance to prevent precipitation, after chemical plating finishes, and cleaning components 10～30 seconds in mobile deionized water, and go to next step;
D, in absolute ethyl alcohol, plating piece is dewatered 2～5 seconds, and plating piece is dry.
5. plating solution application as claimed in claim 4, is characterized in that, oxygen-free copper matrix is fully deoiled, and is divided into two step processing:
First, organic deoiling, it is the acetone soln of 40～60 DEG C that oxygen-free copper matrix is put into temperature, soaks 15～20 minutes;
Secondly, chemical deoiling and degreasing, it is 40～60 DEG C of chemical deoiling and degreasing solution that oxygen-free copper matrix after immersion treatment is put into temperature, ultrasonic immersion 15～20 minutes, oxygen-free copper matrix after immersion treatment is soaked after 0.5～1 minute and puts in the container that fills cold water and rinse 0.25～0.5 minute in hot water, go to next step.
6. plating solution application as claimed in claim 5, is characterized in that, the proportioning of described chemical deoiling and degreasing solution is: sodium carbonate Na2CO320g/l, sodium phosphate Na3PO420g/L, OP-10 emulsifying agent 3g/L.
7. plating solution application as claimed in claim 4, is characterized in that, in step C, and during chemical plating, described bath temperature: 55～65 DEG C, the plating solution time is determined according to thickness of coating and tin layer deposition velocity 0.60～1.00 μ m/min.
8. plating solution application as claimed in claim 4, is characterized in that, in step D, in absolute ethyl alcohol, plating piece is dewatered 2～5 seconds, after with nitrogen, plating piece being dried up, puts into baking oven, dry 10～20min under 80～100 DEG C of conditions.
9. plating solution application as claimed in claim 4, is characterized in that, in step B, described pickling electrolyte is prepared by following composition and proportioning: the sulfuric acid H of 45～60ml/L2SO4, the chromium oxide CrO of 250～300g/L3。
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| CN103367184A (en) * | 2013-07-01 | 2013-10-23 | 浙江固驰电子有限公司 | Diode chip preparation technology |
| CN107460455A (en) * | 2017-07-25 | 2017-12-12 | 东莞聚顺环保科技有限公司 | The tin plating water-based process material of copper ecology and its tin plating method |
| CN107557764A (en) * | 2017-07-25 | 2018-01-09 | 东莞聚顺环保科技有限公司 | The tin plating water-based process material of iron ecology and its tin plating method |
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| CN102002738A (en) * | 2010-12-15 | 2011-04-06 | 安徽华东光电技术研究所 | Plating solution formulation for plating black chrome on oxygen-free copper matrix and electroplating method |
| CN102002742A (en) * | 2010-12-15 | 2011-04-06 | 安徽华东光电技术研究所 | Formula and preparation method of plating solution as well as method for plating aluminum base plate |
| CN102560452A (en) * | 2011-12-08 | 2012-07-11 | 广西师范大学 | Chemical tin plating solution, preparation method for tin plating solution, method for preparing tin/ carbon composite material by using tin plating solution and obtained product |
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| CN102286737A (en) * | 2011-09-13 | 2011-12-21 | 无锡市嘉邦电力管道厂 | Tin plating copper alloy wire |
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| CN102002738A (en) * | 2010-12-15 | 2011-04-06 | 安徽华东光电技术研究所 | Plating solution formulation for plating black chrome on oxygen-free copper matrix and electroplating method |
| CN102002742A (en) * | 2010-12-15 | 2011-04-06 | 安徽华东光电技术研究所 | Formula and preparation method of plating solution as well as method for plating aluminum base plate |
| CN102560452A (en) * | 2011-12-08 | 2012-07-11 | 广西师范大学 | Chemical tin plating solution, preparation method for tin plating solution, method for preparing tin/ carbon composite material by using tin plating solution and obtained product |
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