CN101851470B - Chemical polishing liquid and polishing method - Google Patents
Chemical polishing liquid and polishing method Download PDFInfo
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- CN101851470B CN101851470B CN 200910106611 CN200910106611A CN101851470B CN 101851470 B CN101851470 B CN 101851470B CN 200910106611 CN200910106611 CN 200910106611 CN 200910106611 A CN200910106611 A CN 200910106611A CN 101851470 B CN101851470 B CN 101851470B
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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 ormolu chemical brightening solution and finishing method thereof.
Background technology
Alloy is widely used in making such as ormolu, stainless steel etc. in the sophisticated product such as electronic product parts, and producing the later stage at parts usually needs to adopt the techniques such as plating, welding, encapsulation.Yet alloy surface produces grease in early stage in the manufacture process easily 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 yields of alloy subsequent production, so before carrying out following process, must carry out surface treatment by alloy, remove surperficial grease, oxide-film and improve surfacing and the light of material, guarantee the final yields of product.
In the existing polishing technology, chemical polishing, electrochemical polish and mechanical polishing are three kinds of main modes.Wherein chemical polishing is widely used with advantages such as polishing effect are even, but the surface with chemical polishing technology of the nitric acid-hydrochloric acid system that is widely adopted at present can produce toxic and harmfuls such as " tobacco ", contaminated environment and being detrimental to health.
Summary of the invention
The technical problem to be solved in the present invention is that the surface with chemical polishing technology of nitric acid-hydrochloric acid system in the existing alloy polishing fluid can produce toxic and harmfuls such as " tobacco ", contaminated 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, acetic acid, cooxidant, brightener and adjusting agent, the PH of described polishing fluid is 1～3.
The technical problem to be solved in the present invention is that the surface with chemical polishing technology of nitric acid-hydrochloric acid system in the existing alloy polishing fluid can produce toxic and harmfuls such as " tobacco ", contaminated 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 polishing: polished base material be impregnated in carry out polishing in the chemical polishing soln;
B. reprocessing: after polishing is finished, base material is carried out pickling, washing, oven dry;
Described chemical brightening solution is chemical brightening solution of the present invention.
The present invention adopts sulfuric acid and hydrogen peroxide system, cooperates suitable cooxidant, acetic acid and adjusting agent, has finished the chemical polishing of alloy, has avoided the NO that produces in the polishing process
x, SO
2Deng pernicious gas, reduced to the pollution of environment with to the infringement of operating personnel's health.In addition, use chemical brightening solution of the present invention that high, the surfacing of chemical polished surface brightness that chemical polishing obtains is carried out in the metal surface, can reach the mirror finish effect.
Embodiment
A kind of chemical brightening solution comprises sulfuric acid, hydrogen peroxide, acetic acid, cooxidant, brightener and adjusting 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, the content of described sulfuric acid is 15～70ml/L, the content of described hydrogen peroxide is 150～200ml/L, and the content of described acetic acid is 150～200ml/L, and the content of described cooxidant is 40～80ml/L, the content of described brightener is 3～5g/L, and the content of described adjusting agent is 100～200ml/L.
According to chemical brightening solution of the present invention, described brightener is at least two kinds in thiocarbamide, BTA, cumarin, sulfanilamide (SN), zinc dihydrogen phosphate, NPE, the AEO.It is more even that brightener can play the substrate surface that makes after the polishing, increases brightness and leveling effect.
According to of the present inventionization polishing fluid, described adjusting agent is one or more in silicone oil, antifebrin, polyoxyethylene fatty amine, propenyl, glycerol, the liquid paraffin.Described adjusting agent makes the polishing sluggish and carries out uniformly, has guaranteed the surface effect after alloy polishes, and improves surface smoothness and brightness after alloy polishes.
According to of the present inventionization polishing fluid, described cooxidant is one or more in phosphoric acid, pyrophosphoric acid, tripolyphosphate, oxalic acid, benzoic acid, the citric acid.The adding of cooxidant has not only reduced the use amount of oxidant effectively, has reduced the dependence of solution reaction to oxidant, the more important thing is the useful life that increases reaction solution, makes polishing time and the effect can be controlled.
As long as although contain sulfuric acid, hydrogen peroxide, acetic acid, cooxidant, brightener and adjusting 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 corrosion inhibiter, and the content of described corrosion inhibiter is 10～20ml/L.Described corrosion inhibiter is one or more in oleic acid diethanol amine, sodium metasilicate, imidazoles, sodium alkyl benzene sulfonate, triethanolamine, the benzotriazole.Described corrosion inhibiter is the speed that reduces polishing, is conducive to the control of polishing time and effect.
As long as although contain sulfuric acid, hydrogen peroxide, acetic acid, cooxidant, brightener and adjusting 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 stabilizer, and the content of described stabilizer is 50～100ml/L.Described stabilizer is at least two kinds in ethylene glycol, dodecyl sodium sulfate, sulfamic acid, sodium oxalate, polyethylene glycol, the lignosulfonic acid.The effect of described stabilizer be to reduce and stable polishing fluid in the decomposition rate of oxidant, improve simultaneously the brightness after the alloy polishing.
The present invention also provides a kind of chemically polishing method, mainly may further comprise the steps:
A. chemical polishing: polished base material be impregnated in the chemical polishing soln polish;
B. reprocessing: after polishing is finished, base material is carried out pickling, washing, oven dry;
Described chemical brightening solution is chemical brightening solution of the present invention.
Before carrying out chemical polishing, can treat polishing substrate and carry out pre-treatment, described pre-treatment comprises the initial surface cleaning of the alloys 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 polishing, the bubble that surface of the work is formed is more even, thereby the surface after the polishing is more even.
Described polishing fluid and finishing method have guaranteed surface smoothness and the brightness after the alloy workpiece polishing effectively, and the physics and chemistry performance of alloy has no effect, for the techniques such as follow-up plating or welding have been created advantage.
Polishing fluid of the present invention is applied to ormolu better effect, and embodiments of the invention are illustrated as an example of ormolu example.
The below adopts the mode of embodiment that the present invention is described in further detail.
Embodiment 1
1, according to following set of dispense inhibition and generation optical polishing liquid:
Sulfuric acid 50ml/L, hydrogen peroxide 150ml/L, acetic acid 150ml/L, phosphoric acid 80ml/L, thiocarbamide 2g/L, BTA 1g/L, antifebrin 150ml/L adds water to 1 liter, and recording PH is 2.1.
2, pretreatment process
The examination and test of products: measure the ormolu workpiece size and do respective markers.
Upper: the ormolu workpiece is fixed on the hanger, stand-by.
The oil removing grease removal: (the size 19.00mm * 6.25mm before the polishing * 1.325mm) carries out all-round oil removing (10% all-round degreaser successively with the ormolu workpiece, processing 1min), electrolytic degreasing (60g/L degreaser, 45 ℃, processing 30s), acid deoiling (20% acid deoiling agent+3% phosphoric acid, process 1min), through processing to remove surperficial grease and dirty.
Three washings: the ormolu workpiece after the oil removing grease removal is inserted in three rinsing bowls, thoroughly remove the pollutant of ormolu surface of the work through three rinsings.
Acid activation: the ormolu workpiece after will washing soaks 1min with the dilute sulfuric acid of 3% (volumn concentration), to remove ormolu surface of the work oxide-film and residue.
Three washings: the ormolu workpiece of acid activation is inserted in three rinsing bowls, thoroughly remove ormolu surface of the work pollutant and residue through three rinsings.
3, chemical polishing: through after the preliminary treatment, the ormolu sample be impregnated in 5min in the polishing fluid under room temperature (25 ℃), slightly swing ormolu, take out sample and be dipped in 10s in the dilution heat of sulfuric acid, water flushing, oven dry obtain mirror finish effect sample behind the acidifying striping.
Concrete steps are:
Chemical polishing: the ormolu workpiece after three washings is inserted 3min in the chemical polishing bath, keep simultaneously slight and swing.
Pure water rinsing: the ormolu workpiece after the chemical polishing is inserted in the pure water groove, remove the pollutant that the chemical polishing operation is brought into through rinsing.
Pickling striping: with the dilute sulfuric acid immersion 10s of the ormolu workpiece after the pure water rinsing with 3% (volume ratio), to remove the oxide-film that forms after the chemical polishing of ormolu workpiece.
Three washings: the ormolu workpiece after the pickling is inserted in three rinsing bowls, thoroughly remove pollutant and the surface residue that the front operation produces through three rinsings.
Cut water: the ormolu workpiece after will soaking blows surperficial water off with blower fan, makes product surface dry.
Oven dry: the ormolu workpiece that will cut behind the water is fully dry fast with baking box.
Lower: the ormolu 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, acetic acid 200ml/L, tripolyphosphate 80ml/L, zinc dihydrogen 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 preliminary treatment, the ormolu sample be impregnated in 3min in the polishing fluid under room temperature (25 ℃), slightly swing ormolu, take out sample and be dipped in 10s in the dilution heat of sulfuric acid, water flushing, oven dry obtain mirror finish effect sample behind the acidifying striping.
Chemical polishing experiment concrete technology flow process is with embodiment 1, and the size of ormolu workpiece is polished front size 18.89mm * 6.17mm * 1.318mm.
Embodiment 3
1, according to following set of dispense inhibition and generation optical polishing liquid:
Sulfuric acid 70ml/L, hydrogen peroxide 200ml/L, acetic acid 150ml/L, citric acid 60ml/L, cumarin 2g/L, sulfanilamide (SN) 2g/L, polyoxyethylene fatty amine 100ml/L, benzotriazole 15ml/L, lignosulfonic acid 50ml/L adds water to 1 liter, and recording PH is 1.9.
2, through after the preliminary treatment, the ormolu sample be impregnated in 3min in the polishing fluid under room temperature (25 ℃), slightly swing ormolu, take out sample and be dipped in 10s in the dilution heat of sulfuric acid, clear water flushing, oven dry obtain mirror finish effect sample behind the acidifying striping.
Chemical polishing experiment concrete technology flow process is with embodiment 1, and the ormolu 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, acetic acid 150ml/L, oxalic acid 80ml/L, thiocarbamide 2g/L, zinc dihydrogen phosphate 1g/L, silicone oil 150ml/L, sodium alkyl benzene sulfonate 15ml/L, sulfamic acid 80ml/L adds water to 1 liter, and recording PH is 2.0.
2, through after the preliminary treatment, the ormolu sample be impregnated in 3min in the polishing fluid under room temperature (25 ℃), slightly swing ormolu, take out sample and be dipped in 10s in the dilution heat of sulfuric acid, clear water flushing, oven dry obtain mirror finish effect sample behind the acidifying striping.
Chemical polishing experiment concrete technology flow process is of a size of 19.10mm * 6.30mm * 1.280mm with embodiment 1 before the polishing of ormolu workpiece.
Embodiment 5
With embodiment 4, the ormolu 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 ormolu 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 ormolu workpiece, at room temperature to soak and place polishing fluid, reaction is violent, follows a large amount of Bubble formations, has micro-irritative 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.
Method of testing
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 reflectivity instrument characterizing metal surface of the work polishes, reflectivity values is directly proportional with brightness.
Table 1
| Embodiment | Size (l * w * h, unit: mm) before the polishing | Polishing time | Size (l * w * h, unit: mm) after the polishing | Reflectivity (%) |
| Embodiment 1 | 19.00×6.25×1.325 | 5min | 18.94×6.19×1.286 | 83 |
| Embodiment 2 | 18.89×6.17×1.318 | 3min | 18.89×6.14×1.300 | 80 |
| Embodiment 3 | 18.97×6.25×1.328 | 3min | 18.95×6.23×1.305 | 77 |
| Embodiment 4 | 19.10×6.30×1.280 | 3min | 19.07×6.27×1.260 | 79 |
| Embodiment 5 | 19.00×6.24×1.330 | 3min | 18.97×6.21×1.300 | 81 |
| Embodiment 6 | 19.19×6.20×1.340 | 5min | 19.14×6.15×1.297 | 84 |
| Embodiment 7 | 18.99×6.25×1.318 | 5min | 18.94×6.19×1.288 | 82 |
| Embodiment 8 | 19.00×6.25×1.326 | 5min | 18.90×6.20×1.274 | 87 |
| Embodiment 9 | 19.07×6.23×1.320 | 5min | 19.06×6.19×1.300 | 78 |
| Embodiment 10 | 19.00×6.24×1.340 | 5min | 18.92×6.20×1.300 | 86 |
| Comparative Examples 1 | 19.00×6.25×1.350 | 20s | 18.88×6.17×1.300 | 82 |
In embodiment 1～embodiment 10, the front and back change in size of all directions is all less than 0.10mm as known from Table 1; In the Comparative Examples 1 in the front and back change in size of all directions, wherein length direction be changed to 0.12mm, serious corrosion is described.
From embodiment 1-10 and Comparative Examples relatively can draw, compare with Comparative Examples, embodiments of the invention can not produce " tobacco ".
Claims (9)
1. a chemical brightening solution comprises sulfuric acid, hydrogen peroxide, acetic acid, cooxidant, brightener and adjusting agent, and the pH of described polishing fluid is 1～3; Described cooxidant is one or more in phosphoric acid, pyrophosphoric acid, tripolyphosphate, oxalic acid, benzoic acid, the citric acid.
2. chemical brightening solution according to claim 1, the content of each component is respectively,
Sulfuric acid 15～70ml/L,
Hydrogen peroxide 150～200ml/L,
Acetic acid 150～200ml/L,
Cooxidant 40～80ml/L,
Stabilizer 50～100ml/L,
Brightener 3～5g/L,
Adjusting agent 100～200ml/L.
3. chemical brightening solution according to claim 1, described brightener is at least two kinds in thiocarbamide, BTA, cumarin, sulfanilamide (SN), zinc dihydrogen phosphate, nonyl phenol polyethenoxy ether, the AEO.
4. chemical brightening solution according to claim 1, described adjusting agent is one or more in silicone oil, antifebrin, polyoxyethylene fatty amine, propenyl, glycerol, the liquid paraffin.
5. chemical brightening solution according to claim 1 also comprises corrosion inhibiter, and the content of described corrosion inhibiter is 10～20ml/L.
6. chemical brightening solution according to claim 5, described corrosion inhibiter is one or more in oleic acid diethanol amine, sodium metasilicate, imidazoles, sodium alkyl benzene sulfonate, triethanolamine, the benzotriazole.
7. chemical brightening solution according to claim 1 also comprises stabilizer, and the content of described stabilizer is 50～100ml/L.
8. chemical brightening solution according to claim 7, described stabilizer is at least two kinds in ethylene glycol, dodecyl sodium sulfate, sulfamic acid, sodium oxalate, polyethylene glycol, the lignosulfonic acid.
9. a chemically polishing method is characterized in that, mainly may further comprise the steps:
A. chemical polishing: polished base material be impregnated in the chemical brightening solution polish;
B. reprocessing: after polishing is finished, base material is carried out pickling, washing, oven dry;
Described chemical brightening solution is the described chemical brightening solution of claim 1-8 any one.
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