CN101591798B - Metal piece and method for processing surface of metal piece - Google Patents
Metal piece and method for processing surface of metal piece Download PDFInfo
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- CN101591798B CN101591798B CN2008100676184A CN200810067618A CN101591798B CN 101591798 B CN101591798 B CN 101591798B CN 2008100676184 A CN2008100676184 A CN 2008100676184A CN 200810067618 A CN200810067618 A CN 200810067618A CN 101591798 B CN101591798 B CN 101591798B
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Abstract
The invention relates to a metal piece, the roughness concentration of the surface of the metal piece is 0.02 micron to 0.1 micron, and the reflectivity of the surface is 65 percent to 90 percent. A method for processing the surface of the metal piece is used for obtaining the metal piece by polishing a metal substrate, and the polishing comprises the following steps: polishing pretreatment is carried out to the metal substrate; the metal substrate after the polishing pretreatment is dipped in polishing liquid containing ammonium salt and an addition agent, the metal substrate is put on a positive pole, and a pulse electric field with high frequency and high voltage is applied for plasma body polishing; and the metal piece is obtained after the polished metal substrate is washed and parched. Compared with the traditional polishing method, the method for processing the surface of the metal piece has the advantages that the electrochemistry leveling of the surface of the metal substrate is greatly increased, and the roughness concentration is reduced.
Description
Technical field
The present invention relates to a kind of metalwork and surface treatment method thereof.
Background technology
Now more and more higher to the appearance requirement of metalwork, in particular for the metalwork of electronic product, also more and more higher to its surfaceness and the isoparametric composite request of surface albedo.
The surface treatment of common metal spare comprises polishing, anodic oxidation, differential arc oxidation, plating etc.
Thereby polishing can be used as metalwork surface-treated end process and effectively improves the metalwork surface property and promote decorative effect, also can be used as the operation in early stage of various (comprising features) process for modifying surface, makes subsequent disposal very succinct, and is convenient.
More existing polishing means such as polishing and leveling technology such as laser, ultrasonic wave, electrospark machining, are polished the production demand efficiently because the restriction of factors such as output rating and tooling cost is difficult to realize big area.
Big area to products such as curved surface, position, dead angle and ultra-thin (wall) sheet material, the platinum of complicated form workpiece and slender tube material, special-shaped work piece inner surface, evenly, the especially disposable large-area polishing of high-efficiency high-accuracy mirror polish becomes the main difficult problem of polishing technology.
Electropolishing is a kind of as finishing method, and polishing effect and polishing efficiency are not very good; On the other hand, because the electrolytic polishing liquid composition mainly is a strong acid, the subsequent disposal difficulty of waste liquid easily causes environmental pollution, simultaneously also dangerous property in the process for preparation of polishing fluid.
Though adopt the direct current plasma polishing can improve the metalwork surface property, this treatment process current consumption is big, polishing efficiency is lower simultaneously.
Summary of the invention
The technical problem to be solved in the present invention is that the electrochemistry on metal substrate surface is inhomogeneous, and metal substrate surfaceness is higher, and each diversity and the surface gloss of the orientation that produces in the process of metal working are low.
The invention provides a kind of metalwork, the surfaceness of this metalwork is 0.02um-0.1um, and surface albedo is 65%-90%.
Obtain this metalwork by metal substrate passages through which vital energy circulates towards the plasma polishing processing.
A kind of surface treatment method of above-mentioned metalwork carries out polished finish to the metal substrate and obtains metalwork, and this polishing step comprises:
(a) the metal substrate is polished pre-treatment
(b) the metal substrate after the polishing pre-treatment is dipped in the polishing fluid of ammonium salt-containing and additive,
The metal substrate places anode, applies the hf and hv pulse electric field and carries out plasma polishing;
(c) washing of the metal substrate after the polishing, oven dry obtain metalwork.
Wherein, the ammonium salt in the polishing fluid is: the composition of one or more in ammonium oxalate, ammonium chloride, ammonium nitrate, Neutral ammonium fluoride, ammonium sulfate, ammonium acetate, ammonium tartrate, the diammonium hydrogen citrate.
Wherein, electrolyte temperature is 65～95 ℃.
Wherein, the formation condition of hf and hv pulse electric field is: the direct impulse voltage of 240～360V, pulse repetition frequency are 10K～20KHz, and the direct impulse voltage duty cycle is 20～90%.
Wherein, hf and hv pulse electric field time length 3min at least.
Wherein, the additive in the polishing fluid is complexing agent, electric current dispersion agent, leveling agent, brightening agent.
The electric current dispersion agent is a kind of in glycerine, ethylene glycol, the propylene glycol, and its content is 1～3ml/L.
Complexing agent is one or more in ethylenediamine tetraacetic acid (EDTA), b diammonium disodium edta, ammonium citrate, Trisodium Citrate, the citric acid, and the content of complexing agent is 0.5g/L～10g/L; Leveling agent is a kind of in trolamine, urea, the thiocarbamide, and the content of leveling agent is 0.5g/L～5g/L; Brightening agent is a kind of in Sunmorl N 60S, asccharin, starch, the benzotriazole, and the content of brightening agent is 0.5g/L～3g/L.
Under the hf and hv pulse electric field, make and produce nonequilibrium plasma in the polishing fluid.By adjusting the waveform and the pulse parameter of pulsed electrical field, make that the energy state of each point all is in the fusion on the polished part surface on time and space, away from equilibrium process, this moment, plasma body produced intensive handing-over effect on polishing body surface, made workpiece surface microscopic protrusions position be hit flat rapidly and reached polishing effect.Can not only save the electric energy that the course of processing consumes, also can improve polishing efficiency, thereby improve production capacity.Can be to stainless steel, titanium, nickel, multiple metal such as molybdenum are that the metal substrate or the alloy components of raw material realized the high precision polishing.
Therefore, compare traditional finishing method, can increase substantially the electrochemistry homogeneity on metal substrate surface, reduced surfaceness, remove metalwork surface tramp material and obnoxious flavour pollution layer, each diversity of the orientation that produces in the process of metal working has also obtained eliminating effectively, improves when being in particular in surfaceness and surface albedo.
Embodiment
A kind of surface treatment method of above-mentioned metalwork carries out polished finish to the metal substrate and obtains metalwork, and this polishing step comprises:
(a) the metal substrate is polished pre-treatment
(b) the metal substrate after the polishing pre-treatment is dipped in the polishing fluid of ammonium salt-containing and additive, and the metal substrate places anode, applies the hf and hv pulse electric field and carries out plasma polishing; Be preferably square-wave pulse;
(c) washing of the metal substrate after the polishing, oven dry obtain metalwork.
Wherein, pre-treatment described in the step (a), its technology is conventionally known to one of skill in the art.The present invention does not have particular requirement to the method for pre-treatment, and generally speaking, pre-treatment comprises carries out ultrasonic oil removing and pickling successively with the metalwork workpiece surface.
Ultrasonic oil removing in the described pre-treatment, purpose are grease and the oxide compounds thereof of removing the metalwork surface.The method of ultrasonic oil removing is ultrasonic oil removing known in those skilled in the art.Adopt among the present invention: metalwork is placed sodium salt solution, be heated to 40 ℃, ultrasonic cleaning 3～5 minutes; The pure water washing promptly obtains the metalwork after the ultrasonic oil removing.Described sodium salt solution comprises Na
2CO
3With Na
3(PO
3)
2Mixing solutions, Na wherein
2CO
3Concentration be 20g.L
-1, Na
3(PO
3)
2Concentration be 25g.L
-1
Pickling in the described pre-treatment is to carry out pickling with immersing in the pickle solution through the metalwork after the ultrasonic oil removing, and purpose is to remove the oxide film and the metamorphic layer on surface, makes the metalwork surface active.The method of pickling is conventionally known to one of skill in the art.Among the present invention, will embathe 30～50 seconds in the metalwork workpiece immersion pickle solution.Described pickle solution is the solution that contains nitric acid and sodium hydrogen fluoride, and wherein the concentration of nitric acid is 4.12g.L
-1, NH
4HF
2Concentration be 85g.L
-1
Described pulse plasma polishing is the polishing fluid that the metalwork material after the pre-treatment is placed ammonium salt-containing and additive, is anode with the metalwork, is negative electrode with the stainless steel plate in the polishing trough, carries out plasma polishing under the hf and hv pulse electric field;
Additive in the polishing fluid is complexing agent, electric current dispersion agent, leveling agent, brightening agent.
Complexing agent of the present invention is the known complexing agent of those skilled in the art, and complexing agent is one or more in ethylenediamine tetraacetic acid (EDTA), b diammonium disodium edta, ammonium citrate, Trisodium Citrate, the citric acid, and the content of complexing agent is 0.5g/L～10g/L;
Leveling agent of the present invention is the known leveling agent of those skilled in the art, and leveling agent is a kind of in trolamine, urea, the thiocarbamide, and the content of leveling agent is 0.5g/L～5g/L;
Brightening agent of the present invention is the known brightening agent of those skilled in the art, and brightening agent is a kind of in Sunmorl N 60S, asccharin, starch, the benzotriazole, and the content of brightening agent is 0.5g/L～3g/L.
Electric current dispersion agent of the present invention is the known electric current dispersion agent of those skilled in the art, as glycerine, ethylene glycol, propylene glycol.
The present invention adopts the polishing fluid that contains ammonium salt, the present inventor is surprised to find that, ammonium salt can further reduce metalwork surface roughness everywhere with the electric current dispersion agent, and this polishing fluid helps the realization of disposable large-area glossing with respect to the environmental protection of existing strong acid polishing fluid.
According to method provided by the invention, the formation condition of described hf and hv pulse electric field is: the direct impulse voltage of 240～360V, pulse repetition frequency is 10K～20KHz, and the direct impulse voltage duty cycle is 20～90%, and the hf and hv pulse electric field time length is 3min at least.
The implication of dutycycle is the implication of the known dutycycle of those skilled in the art, that is: in a string ideal pulse sequence (as square wave), and the ratio in the time length of positive pulse and total cycle of pulse.For example: pulse width 1 μ s, the pulse sequence dutycycle of signal periods 4 μ s is 0.25.
According to treatment process provided by the invention, this method also is included in the washing step between each treatment process, washing times between described each operation is not particularly limited, as long as the treatment solution on metalwork surface is fully removed clean, under the preferable case, the washing times that carries out after described pickling is 4-6 time; The washing times that carries out after described pulse plasma polishing is 1-3 time.The used water of washing step is various water of the prior art, and as municipal tap water, deionized water, distilled water, pure water or their mixture, the present invention is preferably deionized water.
The described method that polished finish is carried out on the metalwork surface also is included in the drying treatment after last washing is handled, and described exsiccant method can adopt the method for well known to a person skilled in the art, as vacuum-drying, seasoning, forced air drying.The present invention is preferably in temperature is 80 ℃ baking oven workpiece is dried.
Below by embodiment the present invention is described in more detail.
Embodiment 1
This embodiment is used for illustrating metalwork surface treatment method of the present invention.
(1) ultrasonic oil removing
With 20g.L
-1Na
2CO
3With 25g.L
-1Na
3(PO
3)
2Mixing solutions 1000mL be heated to 40 ℃.Be of a size of 60 * 40mm
2304 model stainless steels be the metal substrate, in above-mentioned solution with ultrasonic cleaning 5 minutes.Take out, be cooled to room temperature, again metalwork was soaked in deionized water 1 minute.
(2) pickling
In 1000mL concentration is 4.12g.L
-1HNO
3In the solution, add NH
4HE
285g is configured to pickle solution.With the metal substrate after the ultrasonic oil removing, be immersed in the above-mentioned pickle solution, soak time is 40 seconds.
(3) pulse plasma polishing
Polishing fluid, its component comprises: 10ml/L～50ml/L ammonium acetate as ammonium salt, 2ml/L glycerine as electric current dispersion agent, 3g/L ammonium citrate as complexing agent and 2g/L trolamine as leveling agent, 1g/L Sunmorl N 60S as brightening agent, surplus is a water, is configured to polishing fluid.
After the deionization washing of metal substrate process and pickling after the ultrasonic oil removing, put into using plasma polishing in the polishing trough.The polished finish condition: be negative electrode with the stainless steel plate in the polishing trough 1), the metal substrate is an anode, is conducting medium with above-mentioned polishing fluid, and tank liquor temperature is 90 ℃, polishes 5 minutes; 2) polishing condition is: and pulsed operation voltage is set at 320V, pulse-repetition is set at 10000Hz, and dutycycle is set at 90%.
Metal substrate washing after the polishing, oven dry obtain metalwork A.
Embodiment 2
This embodiment is used for illustrating metalwork surface treatment method of the present invention.
Be that with the difference of embodiment 1 polishing time is 4 minutes; Pulsed operation voltage is set at 280V.
Metal substrate washing after the polishing, oven dry obtain metalwork B.
Embodiment 3
This embodiment is used for illustrating metalwork surface treatment method of the present invention.
Be not contain electric current dispersion agent glycerine with the difference of embodiment 1.
Metal substrate washing after the polishing, oven dry obtain metalwork C.
Embodiment 4
This embodiment is used for illustrating metalwork surface treatment method of the present invention.
Be with the difference of embodiment 1: pulsed operation voltage is set at 230V, and the direct impulse voltage duty cycle is 15%.
Metal substrate washing after the polishing, oven dry obtain metalwork D.
Embodiment 5
This embodiment is used for illustrating metalwork surface treatment method of the present invention.
Be with the difference of embodiment 1: the burst length is 2min.
Metal substrate washing after the polishing, oven dry obtain metalwork E.
Comparative Examples 1
Be with the difference of embodiment 1: polishing fluid does not contain ammonium salt.
Metal substrate washing after the polishing, oven dry obtain metalwork F.
Comparative Examples 2
Be with the difference of embodiment 1: adopt direct supply to carry out the plasma polishing, rather than the pulse power, the parameter of direct supply is 260V, polishing time 2min.
Metal substrate washing after the polishing, oven dry obtain metalwork G.
Performance test
Surfaceness
Adopt GB/T 3505-2000 to carry out the surfaceness test, measured with the TR200 hand-held roughmeter of Beijing Time Incorporation.
Surface albedo
Adopt GB2680-1994 to carry out the surface albedo test, the ETF-05A type surface albedo tester that adopts Shenzhen to open special Science and Technology Ltd. is measured.
Metalwork A-F is carried out performance test, and test result is as shown in table 1:
Table 1
| The metalwork numbering | Surfaceness (μ m) | Surface albedo (%) |
| A (embodiment 1) | 0.025 | 90 |
| B (embodiment 2) | 0.04 | 84 |
| C (embodiment 3) | 0.085 | 75 |
| D (embodiment 4) | 0.10 | 68 |
| E (embodiment 5) | 0.10 | 65 |
| F (Comparative Examples 1) | 0.3 | 45 |
| G (Comparative Examples 2) | 0.15 | 65 |
By finding out in the table 2, the pulse plasma polishing not only can be economized on electricity, and can further improve the surface treatment effect of metalwork than the direct current plasma polishing of Comparative Examples 2 correspondences.Embodiments of the invention 1 show with the test result of embodiment 3, and the roughness that the electrolytic solution that the present invention contains ammonium salt and electric current dispersion agent can further reduce the metalwork surface improves surface albedo simultaneously.
Claims (5)
1. the surface treatment method of a metalwork carries out polished finish to the metal substrate and obtains metalwork, and this polishing step comprises:
(a) the metal substrate is polished pre-treatment
(b) the metal substrate after the polishing pre-treatment is dipped in the polishing fluid of ammonium salt-containing and additive, and the metal substrate places anode, applies the hf and hv pulse electric field and carries out plasma polishing;
(c) washing of the metal substrate after the polishing, oven dry obtain metalwork;
The surfaceness of this metalwork is 0.02um-0.1um, and surface albedo is 65%-90%; The formation condition of hf and hv pulse electric field is: the direct impulse voltage of 240～360V, pulse repetition frequency are 10K～20KHz, and the direct impulse voltage duty cycle is 20～90%; The hf and hv pulse electric field time length is 3min at least; Additive in the described polishing fluid is complexing agent, electric current dispersion agent, leveling agent, brightening agent.
2. the surface treatment method of the described metalwork of claim 1, wherein, the ammonium salt in the polishing fluid is: the composition of one or more in ammonium oxalate, ammonium chloride, ammonium nitrate, Neutral ammonium fluoride, ammonium sulfate, ammonium acetate, ammonium tartrate, the diammonium hydrogen citrate.
3. the surface treatment method of the described metalwork of claim 1, wherein, electrolyte temperature is 65～95 ℃.
4. the surface treatment method of the described metalwork of claim 1, wherein, the electric current dispersion agent is a kind of in glycerine, ethylene glycol, the propylene glycol, its content is 1～3ml/L.
5. the surface treatment method of the described metalwork of claim 1, wherein, complexing agent is one or more in ethylenediamine tetraacetic acid (EDTA), b diammonium disodium edta, ammonium citrate, Trisodium Citrate, the citric acid, the content of complexing agent is 0.5g/L～10g/L; Leveling agent is a kind of in trolamine, urea, the thiocarbamide, and the content of leveling agent is 0.5g/L～5g/L; Brightening agent is a kind of in Sunmorl N 60S, asccharin, starch, the benzotriazole, and the content of brightening agent is 0.5g/L～3g/L.
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|---|---|
| CN101591798A (en) | 2009-12-02 |
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