CN101851470A - Chemical polishing liquid and polishing method - Google Patents
Chemical polishing liquid and polishing method Download PDFInfo
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- CN101851470A CN101851470A CN200910106611A CN200910106611A CN101851470A CN 101851470 A CN101851470 A CN 101851470A CN 200910106611 A CN200910106611 A CN 200910106611A CN 200910106611 A CN200910106611 A CN 200910106611A CN 101851470 A CN101851470 A CN 101851470A
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Abstract
The invention provides chemical polishing liquid, comprising sulfuric acid, hydrogen peroxide, acetic acid, an auxiliary oxidant, a brightening agent and an adjusting agent, and the PH of the polishing liquid is 1-3. The polishing liquid has simple components and easy control, the obtained chemical polishing surface has high brightness and smooth surface, and can achieve the mirror polishing effect. The polishing liquid can be widely applied in polishing of the surface of copper-zinc alloy.
Description
Technical field
The present invention relates to a kind of chemical brightening solution and finishing method thereof, relate in particular to a kind of copper zinc alloy chemical brightening solution and finishing method thereof.
Background technology
Alloy is widely used in making as copper zinc alloy, stainless steel etc. in the sophisticated product such as electronic product component, and producing the later stage at component usually needs to adopt technologies such as plating, welding, encapsulation.Yet alloy surface is easy to generate grease in early stage in the manufacturing processed to be adhered to, and alloy surface also can oxidation and is formed the dense oxide film of one deck, these all can directly have influence on the good article rate of alloy subsequent production, so before carrying out following process, must carry out surface treatment to alloy, remove surperficial grease, oxide film and improve the surfacing and the light of material, guarantee the final good article rate of product.
In the existing polishing technology, chemical rightenning, electrochemical etching and mechanical polishing are three kinds of main modes.Wherein chemical rightenning is widely used with advantages such as polishing effect are even, but the chemical rightenning technology of the nitric acid-hydrochloric acid system that is widely adopted at present can produce toxic and harmfuls such as " tobacco ", contaminate environment and being detrimental to health.
Summary of the invention
The technical problem to be solved in the present invention is that the chemical rightenning technology of nitric acid-hydrochloric acid system in the existing alloy polishing fluid can produce toxic and harmfuls such as " tobacco ", contaminate environment and the defective that is detrimental to health, thus a kind of polishing solution that can not produce " tobacco " is provided.
The invention provides a kind of chemical brightening solution, comprise sulfuric acid, hydrogen peroxide, acetate, secondary oxidizer, brightening agent and adjustment agent, the PH of described polishing fluid is 1～3.
The technical problem to be solved in the present invention is that the chemical rightenning technology of nitric acid-hydrochloric acid system in the existing alloy polishing fluid can produce toxic and harmfuls such as " tobacco ", contaminate environment and the defective that is detrimental to health, thus a kind of finishing method that can not produce " tobacco " is provided.
The present invention also provides a kind of chemically polishing method, mainly may further comprise the steps:
A. chemical rightenning: polished base material be impregnated in carry out polished finish in the chemical polishing soln;
B. aftertreatment: after polishing is finished, base material is carried out pickling, washing, oven dry;
Described chemical brightening solution is a chemical brightening solution of the present invention.
The present invention adopts sulfuric acid and hydrogen peroxide system, cooperates suitable secondary oxidizer, acetate and adjusts agent, has finished the chemical rightenning to alloy, has avoided the NO that produces in the polishing process
x, SO
2Deng obnoxious flavour, reduced to the pollution of environment with to the infringement of operator's health.In addition, use chemical brightening solution of the present invention that chemical polished surface luminance brightness height, the surfacing that chemical rightenning obtains carried out in the metallic surface, can reach the mirror polish effect.
Embodiment
A kind of chemical brightening solution comprises sulfuric acid, hydrogen peroxide, acetate, secondary oxidizer, brightening agent and adjustment agent, and the PH of described polishing fluid is 1～3.
According to chemical brightening solution provided by the invention, in the preferred case, in described chemical brightening solution, described vitriolic content is 15～70ml/L, the content of described hydrogen peroxide is 150～200ml/L, and the content of described acetate is 150～200ml/L, and the content of described secondary oxidizer is 40～80ml/L, the content of described brightening agent is 3～5g/L, and the content of described adjustment agent is 100～200ml/L.
According to chemical brightening solution of the present invention, described brightening agent is at least two kinds in thiocarbamide, benzotriazole, tonka bean camphor, sulfanilamide (SN), primary zinc phosphate, polyoxyethylene nonylphenol ether, the fatty alcohol-polyoxyethylene ether.It is more even that brightening agent can play the substrate surface that makes after the polishing, increases luminance brightness and leveling effect.
According to of the present inventionization polishing fluid, described adjustment agent is one or more in silicone oil, Acetanilide, polyoxyethylene fatty amine, vinylcarbinol, glycerol, the liquid paraffin.Described adjustment agent makes the polishing sluggish and carries out uniformly, has guaranteed the surface effect after alloy polishes, and improves surface finish and luminance brightness after alloy polishes.
According to of the present inventionization polishing fluid, described secondary oxidizer is one or more in phosphoric acid, tetra-sodium, tripolyphosphate, oxalic acid, phenylformic acid, the citric acid.The adding of secondary oxidizer has not only reduced the usage quantity of oxygenant effectively, has reduced the dependency of solution reaction to oxygenant, the more important thing is the work-ing life that increases reaction soln, makes polishing time and the effect can be controlled.
As long as although contain sulfuric acid, hydrogen peroxide, acetate, secondary oxidizer, brightening agent and adjustment agent, and PH is that 1～3 polishing fluid can be realized purpose of the present invention, but in order to reach better polishing effect, in the preferred case, polishing fluid of the present invention also comprises inhibiter, and the content of described inhibiter is 10～20ml/L.Described inhibiter is one or more in oleic acid diethanolamine, water glass, imidazoles, sodium alkyl benzene sulfonate, trolamine, the benzotriazole.Described inhibiter is the speed that reduces polishing, helps the control of polishing time and effect.
As long as although contain sulfuric acid, hydrogen peroxide, acetate, secondary oxidizer, brightening agent and adjustment agent, and PH is that 1～3 polishing fluid can be realized purpose of the present invention, but in order to reach better polishing effect, in the preferred case, polishing fluid of the present invention also comprises stablizer, and the content of described stablizer is 50～100ml/L.Described stablizer is at least two kinds in ethylene glycol, sodium laurylsulfonate, thionamic acid, sodium oxalate, polyoxyethylene glycol, the lignin sulfonic acid.Described function of stabilizer be to reduce and stable polishing fluid in the decomposition rate of oxygenant, improve the luminance brightness after the alloy polishing simultaneously.
The present invention also provides a kind of chemically polishing method, mainly may further comprise the steps:
A. chemical rightenning: polished base material be impregnated in the chemical polishing soln polish;
B. aftertreatment: after polishing is finished, base material is carried out pickling, washing, oven dry;
Described chemical brightening solution is a chemical brightening solution of the present invention.
Before carrying out chemical rightenning, can treat polishing substrate and carry out pre-treatment, described pre-treatment comprises the initial surface cleaning to alloy such as oil removing, acid activation, three washings.
Described oil removing comprises once carries out all-round oil removing, electrolytic degreasing, acid deoiling.Slowly rock base material or stir polishing fluid in described chemical rightenning, the bubble that workpiece surface is formed is more even, thereby the surface after the polishing is more even.
Described polishing fluid and finishing method have guaranteed surface finish and the luminance brightness after the alloy workpiece polishing effectively, the physics and the chemical property of alloy are had no effect, for technologies such as follow-up plating or welding have been created favourable condition.
Polishing fluid of the present invention is applied to copper zinc alloy better effect, and embodiments of the invention are that example is illustrated with the copper zinc alloy.
Adopt the mode of embodiment that the present invention is described in further detail below.
Embodiment 1
1, according to following set of dispense inhibition and generation optical polishing liquid:
Sulfuric acid 50ml/L, hydrogen peroxide 150ml/L, acetate 150ml/L, phosphoric acid 80ml/L, thiocarbamide 2g/L, benzotriazole 1g/L, Acetanilide 150ml/L adds water to 1 liter, and recording PH is 2.1.
2, pre-treatment process
The examination and test of products: measure the copper zinc alloy workpiece size and do respective markers.
Last part: the copper zinc alloy workpiece is fixed on the hanger, stand-by.
The oil removing grease removal: (the size 19.00mm * 6.25mm * 1.325mm) before the polishing carries out all-round oil removing (10% all-round degreaser successively with the copper zinc alloy workpiece, processing 1min), electrolytic degreasing (60g/L degreaser, 45 ℃, processing 30s), acid deoiling (20% acid deoiling agent+3% phosphoric acid, handle 1min), through handling to remove surperficial grease and dirty.
Three washings: the copper zinc alloy workpiece after the oil removing grease removal is inserted in three washing baths, thoroughly remove the pollutent of copper zinc alloy workpiece surface through three rinsings.
Acid activation: the copper zinc alloy workpiece after will washing soaks 1min with the dilute sulphuric acid of 3% (volumn concentration), to remove copper zinc alloy workpiece surface oxide film and residue.
Three washings: the copper zinc alloy workpiece of acid activation is inserted in three washing baths, thoroughly remove copper zinc alloy workpiece surface pollutent and residue through three rinsings.
3, chemical rightenning: through after the pre-treatment, the copper zinc alloy sample be impregnated in 5min in the polishing fluid under room temperature (25 ℃), slightly swing copper zinc alloy, take out sample and be dipped in 10s in the dilution heat of sulfuric acid, water flushing, oven dry obtain mirror polish effect sample behind the acidifying striping.
Concrete steps are:
Chemical rightenning: the copper zinc alloy workpiece after three washings is inserted 3min in the chemical rightenning groove, keep slight swing simultaneously.
Pure water rinsing: the copper zinc alloy workpiece after the chemical rightenning is inserted in the pure water groove, remove the pollutent that the chemical rightenning operation is brought into through rinsing.
Pickling striping: with the dilute sulphuric acid immersion 10s of the copper zinc alloy workpiece after the pure water rinsing, to remove the oxide film that forms after the chemical rightenning of copper zinc alloy workpiece with 3% (volume ratio).
Three washings: the copper zinc alloy workpiece after the pickling is inserted in three washing baths, thoroughly remove pollutent and the surface residue that the front operation produces through three rinsings.
Cut water: the copper zinc alloy workpiece after will soaking blows surperficial water off with blower fan, makes the product surface drying.
Oven dry: will cut copper zinc alloy workpiece behind the water with the quick thorough drying of baking box.
Following part: the copper zinc alloy workpiece after the oven dry takes off from hanger.
Embodiment 2
1, according to following set of dispense inhibition and generation optical polishing liquid:
Sulfuric acid 15ml/L, hydrogen peroxide 180ml/L, acetate 200ml/L, tripolyphosphate 80ml/L, primary zinc phosphate 2g/L, nonyl phenol polyethenoxy ether 3g/L, glycerol 200ml/L, imidazoles 20ml/L, sodium oxalate 80ml/L adds water to 1 liter, and recording PH is 1.9.
2, through after the pre-treatment, the copper zinc alloy sample be impregnated in 3min in the polishing fluid under room temperature (25 ℃), slightly swing copper zinc alloy, take out sample and be dipped in 10s in the dilution heat of sulfuric acid, water flushing, oven dry obtain mirror polish effect sample behind the acidifying striping.
Chemical rightenning is tested concrete technical process with embodiment 1, the size 18.89mm * 6.17mm * 1.318mm before the polishing of the size of copper zinc alloy workpiece.
Embodiment 3
1, according to following set of dispense inhibition and generation optical polishing liquid:
Sulfuric acid 70ml/L, hydrogen peroxide 200ml/L, acetate 150ml/L, citric acid 60ml/L, tonka bean camphor 2g/L, sulfanilamide (SN) 2g/L, polyoxyethylene fatty amine 100ml/L, benzotriazole 15ml/L, lignin sulfonic acid 50ml/L adds water to 1 liter, and recording PH is 1.9.
2, through after the pre-treatment, the copper zinc alloy sample be impregnated in 3min in the polishing fluid under room temperature (25 ℃), slightly swing copper zinc alloy, take out sample and be dipped in 10s in the dilution heat of sulfuric acid, flushing with clean water, oven dry behind the acidifying striping obtain mirror polish effect sample.
Chemical rightenning is tested concrete technical process with embodiment 1, and the copper zinc alloy workpiece is of a size of standard workpiece size 18.97mm * 6.25mm * 1.328mm.
Embodiment 4
1, according to following set of dispense inhibition and generation optical polishing liquid:
Sulfuric acid 50ml/L, hydrogen peroxide 150ml/L, acetate 150ml/L, oxalic acid 80ml/L, thiocarbamide 2g/L, primary zinc phosphate 1g/L, silicone oil 150ml/L, sodium alkyl benzene sulfonate 15ml/L, thionamic acid 80ml/L adds water to 1 liter, and recording PH is 2.0.
2, through after the pre-treatment, the copper zinc alloy sample be impregnated in 3min in the polishing fluid under room temperature (25 ℃), slightly swing copper zinc alloy, take out sample and be dipped in 10s in the dilution heat of sulfuric acid, flushing with clean water, oven dry behind the acidifying striping obtain mirror polish effect sample.
Chemical rightenning is tested concrete technical process with embodiment 1, is of a size of 19.10mm * 6.30mm * 1.280mm before the polishing of copper zinc alloy workpiece.
Embodiment 5
With embodiment 4, the copper zinc alloy workpiece is of a size of 19.00mm * 6.24mm * 1.330mm.
Embodiment 6-10
With embodiment 4, polishing time is 5min, and the size before the copper zinc alloy polishing is respectively 19.19mm * 6.20mm * 1.340mm, 18.99mm * 6.25mm * 1.318mm, 19.00mm * 6.25mm * 1.326mm, 19.07mm * 6.23mm * 1.320mm, 19.00mm * 6.24mm * 1.340mm.
Comparative Examples 1
1. according to following set of dispense inhibition and generation optical polishing liquid:
Nitric acid 300～400ml/L, sulfuric acid 300～400ml/L, hydrochloric acid 50～100ml/L, urea 40～60g/L adds water to 1L.
2. through pretreated copper zinc alloy workpiece, at room temperature to soak and place polishing fluid, reaction is violent, follows a large amount of bubbles to produce, and has micro-irritant gas and tobacco to produce; Because the too fast excessive erosion phenomenon that very easily produces of reaction.
Workpiece size before the polishing is 19.00mm * 6.25mm * 1.350mm, the reflectivity data before and after the reaction after size numerical value and the polishing.
Testing method
1. adopt length, the width of miking workpiece, the numerical value change of three directions of thickness, each direction is tested 3 times at least, and averages.
2. adopt the reflectivity values after the albedo measurement instrument is levied surface polishing of metallic workpiece, reflectivity values is directly proportional with luminance brightness.
Table 1
In embodiment 1～embodiment 10, the front and back dimensional change of all directions is all less than 0.10mm as known from Table 1; In the Comparative Examples 1 in the front and back dimensional change of all directions, wherein length direction be changed to 0.12mm, serious corrosion is described.
Can draw from the comparison of embodiment 1-10 and Comparative Examples, compare with Comparative Examples, embodiments of the invention can not produce " tobacco ".
Claims (10)
1. a chemical brightening solution comprises sulfuric acid, hydrogen peroxide, acetate, secondary oxidizer, brightening agent and adjustment agent, and the PH of described polishing fluid is 1～3.
2. chemical brightening solution according to claim 1, each components contents is respectively,
Sulfuric acid 15～70ml/L,
Hydrogen peroxide 150～200ml/L,
Acetate 150～200ml/L,
Secondary oxidizer 40～80ml/L,
Stablizer 50～100ml/L,
Brightening agent 3～5g/L,
Adjust agent 100～200ml/L.
3. chemical brightening solution according to claim 1, described brightening agent are at least two kinds in thiocarbamide, benzotriazole, tonka bean camphor, sulfanilamide (SN), primary zinc phosphate, nonyl phenol polyethenoxy ether, the fatty alcohol-polyoxyethylene ether.
4. chemical brightening solution according to claim 1, described adjustment agent are one or more in silicone oil, Acetanilide, polyoxyethylene fatty amine, vinylcarbinol, glycerol, the liquid paraffin.
5. chemical brightening solution according to claim 1, described secondary oxidizer are one or more in phosphoric acid, tetra-sodium, tripolyphosphate, oxalic acid, phenylformic acid, the citric acid.
6. chemical brightening solution according to claim 1 also comprises inhibiter, and the content of described inhibiter is 10～20ml/L.
7. chemical brightening solution according to claim 6, described inhibiter are one or more in oleic acid diethanolamine, water glass, imidazoles, sodium alkyl benzene sulfonate, trolamine, the benzotriazole.
8. chemical brightening solution according to claim 1 also comprises stablizer, and the content of described stablizer is 50～100ml/L.
9. chemical brightening solution according to claim 8, described stablizer are at least two kinds in ethylene glycol, sodium laurylsulfonate, thionamic acid, sodium oxalate, polyoxyethylene glycol, the lignin sulfonic acid.
10. a chemically polishing method is characterized in that, mainly may further comprise the steps:
A. chemical rightenning: polished base material be impregnated in the chemical polishing soln polish;
B. aftertreatment: after polishing is finished, base material is carried out pickling, washing, oven dry;
Described chemical brightening solution is any described chemical brightening solution of claim 1-9.
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