CN101187050A - Non-corrosive steel low-temperature blacking method - Google Patents
Non-corrosive steel low-temperature blacking method Download PDFInfo
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- CN101187050A CN101187050A CNA2007100428781A CN200710042878A CN101187050A CN 101187050 A CN101187050 A CN 101187050A CN A2007100428781 A CNA2007100428781 A CN A2007100428781A CN 200710042878 A CN200710042878 A CN 200710042878A CN 101187050 A CN101187050 A CN 101187050A
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- stainless steel
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Abstract
The invention discloses a blackening method of stainless steel at low temperature, the front and back surfaces of 304 type stainless steel are polished until bright using 800 # -200 # waterproof abrasive paper, are cleaned by ultrasonic in alcohol, are washed by hot alkali solution for removing oil, and then are activated through being soaked in sulfate dilute solution which contains 5 percent HF about 5 minutes, at last are repeatedly leached by deionized water for later use. The invention is characterized in that the compositions of blackening solution comprise potassium dichromate which is 10-80 g/L, manganese sulfate which is 10-100 g/L, ammonium sulfate which is 20-50 g/L, boric acid which is 10-20 g/ L, and an additive which is 5 g/L, the temperature of the blackening solution is controlled between 30-50 DEG C, the current density is controlled between 0.15-30 Ampere/ decimeter 2, and the stainless steel is used as an anode of an electrode reaction to do a low temperature blackening process. The invention has the advantages of simple process, low temperature of the solution, less environmental pollution, dark darkness of obtained films, uniform color, and excellent binding force and wear resistance.
Description
Technical field
The present invention relates to the process of surface treatment of a kind of iron or ferrous alloy, more particularly relate to a kind of non-corrosive steel low-temperature blacking method.
Background technology
The method of stainless steel blackout is broadly divided into chemical method, electrochemical process and pyroprocess three major types, wherein, mainly based on chemical coloring process and electrochemical coloring method, the stainless steel that these two kinds of methods are handled, its surface color distinctness is sustained, and does not influence stainless other performance.But deficiencies such as these methods all exist, and environmental pollution is big, solution temperature is high, energy consumption is big, complex process, stainless steel rete color and luster homogeneity and color control instability.
Summary of the invention
Technical problem to be solved by this invention provides a kind of non-corrosive steel low-temperature blacking method, this method technology is simple, solution temperature is low, environmental pollution is little, gained rete blackness is dark, color and luster evenly, bonding force and wear resistance be good.
The technical solution used in the present invention: a kind of non-corrosive steel low-temperature blacking method, with 800
#～2000
#Waterproof abrasive paper is with 304 type stainless steel substrates surface finish lights, ultrasonic cleaning in alcohol removes oil solution with hot alkali and cleans, and immersion activated in about 5 minutes in containing the sulfuric acid dilute solution of 5%HF then, with deionized water drip washing repeatedly, electrolysis is turned black in blackening solution then at last.It is characterized in that: the composition of blackening solution comprises potassium bichromate 10～80g/L, manganous sulfate 10～100g/L, ammonium sulfate 20～50g/L, boric acid 10～20g/L, additive 5g/L forms, and the temperature of blackening solution is controlled between 5 ℃～50 ℃, and current density is controlled at 0.15～3A/dm
2Between, stainless steel substrates carries out the processing of low temperature blackout as the anode of electrode reaction.
The beneficial effect of the invention, technology of the present invention is simple, solution temperature is low, environmental pollution is little, gained rete blackness is dark, color and luster evenly, bonding force and wear resistance be good.Meet stainless steel surface passivation layer " dissolution-deposition " mechanism by microscopic examination in conjunction with the electromechanical blackening process of the growth mechanism analysis revealed stainless steel surface of the present invention of passivation for stainless steel rete.
Description of drawings
Fig. 1 a contains MnSO in the blackening solution
4Generate the microstructure figure of rete during 30g/L;
Fig. 1 b contains MnSO in the blackening solution
4Generate the microstructure figure of rete during 40g/L;
Fig. 1 c contains MnSO in the blackening solution
4Generate the microstructure figure of rete during 70g/L;
Fig. 1 d contains MnSO in the blackening solution
4Generate the microstructure figure of rete during 100g/L;
Fig. 2 a contains K in the blackening solution
2Cr
2O
7During 10g/L to the figure that influences of rete microscopic appearance;
Fig. 2 b contains K in the blackening solution
2Cr
2O
7During 30g/L to the figure that influences of rete microscopic appearance;
Fig. 2 c contains K in the blackening solution
2Cr
2O
7During 60g/L to the figure that influences of rete microscopic appearance;
Fig. 2 d contains K in the blackening solution
2Cr
2O
7During 80g/L to the figure that influences of rete microscopic appearance;
Embodiment
Below by embodiment the present invention is described in further detail, used stainless steel is 304 type stainless steels in the experiment, is cut into the sheet of 20mm * 50mm * 2mm size, and sample uses 800 successively
#～2000
#Waterproof abrasive paper is with stainless steel substrates pros and cons polishing light, then with its ultrasonic cleaning in alcohol, alkali with heat removes the oil solution cleaning at last, and immersion activated in about 5 minutes in containing the sulfuric acid dilute solution of 5%HF then, and drip washing is stand-by repeatedly with deionized water at last.Blackening solution is formed mainly by potassium bichromate 10～80g/L, manganous sulfate 10～100g/L, and ammonium sulfate 20～50g/L, boric acid 10～20g/L, additive 5g/L forms.Solution temperature is between 30 ℃～50 ℃.Current density is controlled at 0.15～3A/dm
2Between, stainless steel substrates is used as the negative electrode of electrode reaction.
The electrode surface microscopic appearance adopts observation by light microscope.The sticking power of rete adopts the scratch method test: draw parallel lines with draw point at the good stainless steel surface of blackout, distance between the parallel lines drops from the black coating that 1cm reduces gradually between parallel lines, distance when dropping is spaced apart the standard of weighing sticking power, as 0.5mm in the distance of observing with microscope between the cut.The wear resistance of rete adopts the test of rubber wipe method: with rubber covered rollers (the constant pressure 500g/cm that designs voluntarily
2) roll at the good stainless steel surface of blackout, the number of times when disappearing with black film is differentiated the fine or not degree of wear resistance.
The concentration of manganous sulfate is reacted film forming influence to stainless steel electrode in the blackening solution, and manganous sulfate is one of main component of coloring liquid.In Stainless Steel Watch surface anode film process, one side Mn
2+Ion generates the high oxide of manganese in stainless steel surface generation oxidation, on the other hand, and electrode surface Mn
2+Oxidation products to the promoter action that is dissolved with of the passive film of stainless steel surface, make the metal ion generation oxidation dissolution of stainless steel surface, metal ion that produces and surperficial chromate ion generation redox reaction, when these redox products of stainless steel surface reached a certain threshold value, the reduzate of the oxide compound of manganese, the oxide compound of dissolved metal ions and chromate ion was together in the stainless steel surface film forming.Manganous sulfate content is crossed when hanging down, under identical condition, the dissolution rate of stainless steel surface metal is lower, can not make the original passive film dissolving of stainless steel surface fully, under such situation, the redox product that generates is just on original passive film surface " accumulation ", and is relatively poor with combining of stainless steel base; And because speed of response is slower, and all redox products can not reach the needed threshold value of film forming, reaction separately just progressively takes place, form simple settling.Therefore, under such condition, stainless steel surface just forms one of floating ash sample and wipes the brown or the grey black rete that promptly fall; And when manganous sulfate content is higher, because Mn
2+Oxidation products the promoter action of stainless steel surface oxidation dissolution is strengthened, make the dissolving metal of stainless steel surface speed up, produces excessive metal ion and can not in time participate in film process, enter hydrolysis take place in solution in the solution, form and precipitate.Simultaneously, because film forming speed is too fast, make that the compactness extent of rete is not high, loss of adhesion.Therefore, under such condition, the rete blackness that stainless steel surface generates descends to some extent, and solution occurs muddy, and the surface easily produces floating ash.Fig. 1 a, Fig. 1 b, Fig. 1 c, Fig. 1 d are the microstructure figure of rete under the different condition, can obviously find out from each figure of Fig. 1 and work as MnSO
4Sticking power can descend when concentration increased gradually, and white portion is stainless matrix among the figure, can see obviously that the middle white portion of publishing picture is along with MnSO
4Concentration increases more and more, and excessive MnSO is described
4Can reduce the adhesive ability of black oxide film.
The concentration of potassium bichromate is reacted film forming influence to stainless steel electrode, and potassium bichromate is one of filmogen, and it mainly acts on is the metal ion that the electrolysis of oxidation stainless steel surface produces.In film process, the chromate ion on stainless steel electrode surface and stainless steel surface dissolved metal ion generation redox reaction, the reduzate of self has also participated in the generation of film.So potassium bichromate concentration will guarantee to have at electrode surface the chromate ion of appropriate amount in the solution.The concentration of potassium bichromate is low excessively in the solution, then can not be in time with the oxidation of dissolved metal ion and metal ion enters into solution, or form gelationus tectum at surface hydrolysis, in this case, the sticking power and the wear resistance of rete are relatively poor; And when in the solution during potassium bichromate excessive concentration, its oxidisability can make stainless steel surface constantly generate passivation layer, influenced combining of metallic surface metal ion settled layer and matrix, simultaneously, under the situation that other condition satisfies, the speed of growth of rete is too fast, makes the compactness of rete be affected.Fig. 2 a, Fig. 2 b, Fig. 2 c, Fig. 2 d, be the microscopic appearance figure that changes the concentration gained rete of potassium bichromate under the constant situation of other condition.From each figure of Fig. 2, can find out: work as K
2Cr
2O
7Concentration increases gradually, and the sticking power of film can descend, and white portion is stainless matrix among the figure, illustrates if K
2Cr
2O
7Amount too much can reduce the adhesive ability of black oxide film.
According to the one-tenth film theory of passivation for stainless steel, the prerequisite that generates passive film is might generate solid reaction in electrode reaction, forms nucleus at stainless steel surface, forms oxide film along with the formation of nucleus and epitaxy.
Adopt scratch method to test the stainless sticking power in blackout back, table 1 is the test result to blackout sample sticking power under the different tests condition.From test result, K
2Cr
2O
7, and MnS0
4Content the sticking power of rete is had very big influence.Along with the increase of the two content, the sticking power of rete is variation gradually.
The test result of blackout sample sticking power under the table 1 stainless steel different tests condition
Adopt the friction of rubber wheel that the stainless wear resistance in back of turning black is tested, the result shows: K
2Cr
2O
7And MnSO
4Amount conference cause the wear resistance of black film to reduce, black film is wiped out easily.This is because K
2Cr
2O
7And MnSO
4The excessive speed of growth that makes rete of amount accelerate the short texture of oxide compound in the rete.By optimizing the processing condition black stainless steel substrates effective and that bonding force is strong that can obtain to turn black, as shown in table 2.
The test result of blackout sample wear resistance under the table 2 stainless steel different tests condition
Above said content only is the basic explanation of the present invention under conceiving, and according to any equivalent transformation that technical scheme of the present invention is done, all should belong to protection scope of the present invention.
Claims (1)
1. non-corrosive steel low-temperature blacking method is with 800
#～2000
#Waterproof abrasive paper is with 304 type stainless steel substrates pros and cons polishing light, ultrasonic cleaning in alcohol, alkali with heat removes the oil solution cleaning, immersion activated in about 5 minutes in containing the sulfuric acid dilute solution of 5%HF then, at last with deionized water drip washing repeatedly, carry out the low temperature blackout with stainless steel substrates as the anode of electrode reaction then and handle.It is characterized in that: the composition of blackening solution comprises potassium bichromate 10～80g/L, manganous sulfate 10～100g/L, ammonium sulfate 20～50g/L, boric acid 10～20g/L, additive 5g/L forms, and the temperature of blackening solution is controlled between 5 ℃～50 ℃, and current density is controlled at 0.15～3A/dm
2Between, stainless steel substrates carries out the processing of low temperature blackout as the anode of electrode reaction.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100428781A CN101187050A (en) | 2007-06-27 | 2007-06-27 | Non-corrosive steel low-temperature blacking method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100428781A CN101187050A (en) | 2007-06-27 | 2007-06-27 | Non-corrosive steel low-temperature blacking method |
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| CN101187050A true CN101187050A (en) | 2008-05-28 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102965652A (en) * | 2012-11-07 | 2013-03-13 | 浙江博海金属制品科技有限公司 | Stainless steel plate surface blackening treatment process |
| CN103122473A (en) * | 2011-11-21 | 2013-05-29 | 比亚迪股份有限公司 | Electrochemical colouring liquid for stainless steel and electrochemical blacking method for stainless steel |
| CN106086995A (en) * | 2016-06-07 | 2016-11-09 | 安阳工学院 | A kind of stainless steel electrochemical the method for color spectrum |
| CN112071946A (en) * | 2019-05-21 | 2020-12-11 | 北京铂阳顶荣光伏科技有限公司 | Preparation method of thin-film solar cell |
-
2007
- 2007-06-27 CN CNA2007100428781A patent/CN101187050A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103122473A (en) * | 2011-11-21 | 2013-05-29 | 比亚迪股份有限公司 | Electrochemical colouring liquid for stainless steel and electrochemical blacking method for stainless steel |
| CN103122473B (en) * | 2011-11-21 | 2016-06-01 | 比亚迪股份有限公司 | A kind of stainless steel electrochemical coloring liquid and a kind of stainless steel electrochemical blackening method |
| CN102965652A (en) * | 2012-11-07 | 2013-03-13 | 浙江博海金属制品科技有限公司 | Stainless steel plate surface blackening treatment process |
| CN102965652B (en) * | 2012-11-07 | 2014-11-05 | 浙江博海金属制品科技有限公司 | Stainless steel plate surface blackening treatment process |
| CN106086995A (en) * | 2016-06-07 | 2016-11-09 | 安阳工学院 | A kind of stainless steel electrochemical the method for color spectrum |
| CN112071946A (en) * | 2019-05-21 | 2020-12-11 | 北京铂阳顶荣光伏科技有限公司 | Preparation method of thin-film solar cell |
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Open date: 20080528 |