CN102995092A - Blue titan-alloy microarc oxidation coloring solution and preparation method thereof - Google Patents
Blue titan-alloy microarc oxidation coloring solution and preparation method thereof Download PDFInfo
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- CN102995092A CN102995092A CN201210497134XA CN201210497134A CN102995092A CN 102995092 A CN102995092 A CN 102995092A CN 201210497134X A CN201210497134X A CN 201210497134XA CN 201210497134 A CN201210497134 A CN 201210497134A CN 102995092 A CN102995092 A CN 102995092A
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Abstract
The invention belongs to the field of metal coloring and dyeing in surface treatment technology, and particularly relates to a blue titan-alloy microarc oxidation coloring solution and a preparation method thereof, and the blue titan-alloy microarc oxidation coloring solution is used for overcoming the defects of an electrolytic coloring coating. The coloring solution comprises a microarc oxidation spark discharge introducing agent for causing microarc oxidation, a blue microarc oxidation coloring agent, a blue coasting compact accelerator, a blue microarc oxidation coating color homogenizing agent, a blue coating stabilizer and a bath solution stabilizer. The blue titan-alloy microarc oxidation coloring solution provided by the invention is applicable to microarc oxidation coloring, the resulting coating is up to 20 microns in thickness, and the coating with the thickness of 2 to 0 microns is blue as required, and the prepared coating is stable in color and luster and has the characteristic of resistance to touch and wear; the coating is compact and cannot absorb the splotch; and the coating has the excellent characteristics that no organic matter is contained, and the ultraviolet light can be resisted for a long duration. The coating is at temperature below 600 DEG C and is free from discoloring.
Description
Technical field
Patent of the present invention belongs to metal coloring and the dyeing field in the process for treating surface.Relate to a kind ofly for titanium alloy component, on titanium alloy substrate, directly produce the solution of blue ceramic layer by the differential arc oxidation coloring process.Be specially a kind of blue series titanium alloy differential arc oxidation coloring solution and preparation method thereof.
Background technology
Metal coloring and dyeing are to instigate metal self surface to produce and original different tones, and keep the technique of metalluster.The titanium alloy dye technology of open report has the electrolytic coloring technology at present, such as patent CN102080247 cigarette yellow titanium alloy colouring processing method, is a kind of electrolytic coloring technology.Its rete is noncrystalline membrane, and thicknesses of layers is less than 1 micron.Rete is not wear-resisting, touches easy generation decolouring with hand, easily adsorbs stain, more than 200 ℃, and rete can not stop the oxidation of titanium matrix and variable color.The advantage that titanium alloy has is anti-corrosion, specific tenacity is high, and more and more be widely used in, for the industry with high-grade decoration demand, such as titanium alloy spectacle frame etc. in the urgent need to a kind of high-quality blue series dye technology, make painted rete have the advantages such as anti-corrosion, heat-resisting, ultraviolet resistance, can keep simultaneously the gloss of metal, realize that really painted rete has the decorative effect of actual application value.
Differential arc oxidation is the process for treating surface of a kind of metallic surface growth in situ ceramic layer of growing up on the anodic oxidation basis the nearly more than ten years.Namely in certain electrolyte solution, adopt higher operating voltage, the work area is incorporated into the high tension spark electrical discharge zone by the faraday zone of common anode oxidation, utilize arc discharge so that the compact oxidation layer that anodic oxidation forms is breakdown, produce arc discharge and moment high temperature (＞2000 ℃), oxide film melting under the High Temperature High Pressure effect, after the ion arc disappeared, the melts Quench formed ceramic membrane.Owing in liquid phase medium, by plasma discharge growth and the ceramic deposition rete of surface of metal electrode, be also referred to as plasma body liquid phase electrolytic deposition technology.
Because the rete chromogenic mechanism is complicated, it is quite large particularly to produce pure rifle look difficulty.The collocation method of solution composition and solution plays the essence effect to the rete color and luster.Therefore, need carry out the lot of experiments screening to tank liquor prescription and collocation method.
Summary of the invention
The object of the present invention is to provide a kind of blue series titanium alloy differential arc oxidation coloring solution and preparation method thereof, overcome the defective of electrolytic coloring rete.
The technical solution adopted in the present invention is:
A kind of blue series titanium alloy differential arc oxidation coloring solution comprises the differential arc oxidation spark discharge introducing agent that produces differential arc oxidation, blue differential arc oxidation tinting material, the fine and close promotor of blue rete, blue differential arc oxidation film layer color and luster leveler, blue rete stablizer, tank liquor stablizer.Wherein:
It is phosphoric acid salt that agent is introduced in the differential arc oxidation spark discharge, and its content in coloring liquid is 4g/L～20g/L;
Blue differential arc oxidation tinting material is nickel salt or cobalt salt, and nickel or cobalt content in coloring liquid is 0.2g/L～1.1g/L;
The fine and close promotor of blue differential arc oxidation film layer is sodium wolframate, and its content in coloring liquid is 0.5g/L～2g/L;
Blue differential arc oxidation film layer color and luster leveler is glycerine, and content is 2ml/L～10ml/L in the coloring liquid;
Blue rete stablizer is disodium ethylene diamine tetraacetate, and content is 2g/L～20g/L;
The tank liquor stablizer is sodium hydroxide or potassium hydroxide, and content is 1g/L～3g/L;
Aforesaid a kind of blue series titanium alloy differential arc oxidation coloring solution, wherein: described coloring liquid use temperature is 15 ℃～65 ℃.
Aforesaid a kind of blue series titanium alloy differential arc oxidation coloring solution, wherein: it is any in tertiary sodium phosphate, Sodium phosphate dibasic, segregation sodium phosphate, trisodium phosphate, the inferior sodium phosphate that phosphoric acid salt that agent adopts is introduced in described differential arc oxidation spark discharge.
Aforesaid a kind of blue series titanium alloy differential arc oxidation coloring solution, wherein: described blue differential arc oxidation tinting material is single nickel salt or rose vitriol, and content is 1g/L～5g/L.
A kind of preparation method of blue series titanium alloy differential arc oxidation coloring solution comprises the steps:
Step 1: add deionized water;
Step 2: add blue rete stablizer;
Step 3: add the tank liquor stablizer;
Step 4: add the differential arc oxidation spark discharge and introduce agent;
Step 5: add blue differential arc oxidation tinting material;
Step 6: add the fine and close promotor of blue rete;
Step 7: add blue differential arc oxidation film layer color and luster leveler;
Step 8: additional deionized water is to the liquor capacity of drafting.
The preparation method of aforesaid a kind of blue series titanium alloy differential arc oxidation coloring solution, blue differential arc oxidation tinting material with deionized water dissolving after, slowly add, uninterruptedly stir in the adition process, otherwise easily cause muddiness, cause solution allocation to lose efficacy.
The preparation method of aforesaid a kind of blue series titanium alloy differential arc oxidation coloring solution, wherein: the painted groove that described preparation process adopts is polypropylene plastics hopper or stainless steel tank.
The preparation method of aforesaid a kind of blue series titanium alloy differential arc oxidation coloring solution, wherein: the stainless steel tank that holds described solution connects the negative pole of differential arc oxidation coloring power source.
The invention has the beneficial effects as follows:
The present invention is adapted to for the titanium alloy product with high-grade decoration demand, and that rete has is anti-corrosion, heat-resisting, ultraviolet resistance, the advantage such as wear-resisting, can keep the gloss of metal simultaneously, really realizes the decorative effect of painted rete.
The present invention is by adopting specific differential arc oxidation current waveform and processing parameter, make the titanium alloy body when differential arc oxidation generates ceramic membrane, make blue differential arc oxidation tinting material in the solution between the interface of titanium alloy material surface and solution, by forming the form of micelle, it is inner to arrive the ceramic membrane hole with electrophoretic, rely on the mechanism such as electrochemistry, plasma chemistry, thermochemistry in the rete hole, directly to generate coloured compound, make the color and luster that rete has to be needed.Since the plasma discharge temperature up to 2000 ℃～8000 ℃, this blueness compound and Oxide scale on Ti base alloys form complete uniform coloured ceramic membrane on the microcosmic level by sintering.Because differential arc oxidation generation ceramic layer is that one's own department or unit generates on titanium alloy substrate, determined that this colored ceramic layer has well and the bonding force of matrix.
Coloring solution stable chemical performance provided by the invention, use temperature is 15 ℃～65 ℃, can make the titanium alloy body when differential arc oxidation generates ceramic membrane, the differential arc oxidation tinting material, it is inner to arrive the ceramic membrane hole by the form that forms micelle with electrophoretic, rely on the mechanism such as electrochemistry, plasma chemistry, thermochemistry in the rete hole, directly to generate blue compound, make rete have the blue color and luster of light.In differential arc oxidation plasma discharge process, colored compound and Oxide scale on Ti base alloys form complete uniform coloured ceramic membrane on the microcosmic level by sintering, and rete has wear resistance, and is bright-coloured, careful, is rich in metalluster.Overcome generally and carried out painted rete defective by titanium alloy anode oxidation solution generation interference color.The interference color film layer thickness is below 1 micron, and is not wear-resisting, and hand is touched easy generation decolouring, easily adsorbs stain, and more than 200 ℃, rete can not stop the oxidation of titanium matrix and variable color.Film color is to oxidization time, voltage-sensitive in the production, and color and luster is difficult for reproduction.
It is painted to carry out differential arc oxidation by solution provided by the invention, and thicknesses of layers can reach 20 microns, and thicknesses of layers is the bluenesss that need at 2 microns～20 microns, and the rete color and luster that forms is stable, has anti-touching, wear-resisting characteristics, and the rete densification can not adsorbed stain.More excellent is that rete does not contain organism, for a long time ultraviolet resistance.Rete can variable color below 600 ℃.
Embodiment
Below in conjunction with embodiment a kind of blue series titanium alloy differential arc oxidation coloring solution provided by the invention is introduced:
A kind of blue series titanium alloy differential arc oxidation coloring solution comprises the differential arc oxidation spark discharge introducing agent that produces differential arc oxidation, blue differential arc oxidation tinting material, the fine and close promotor of blue rete, blue differential arc oxidation film layer color and luster leveler, blue rete stablizer, tank liquor stablizer.Wherein,
It is phosphoric acid salt that agent is introduced in the differential arc oxidation spark discharge, is preferably any in tertiary sodium phosphate, Sodium phosphate dibasic, segregation sodium phosphate, trisodium phosphate, the inferior sodium phosphate, and content is preferably 4g/L～20g/L.
Blue differential arc oxidation tinting material is dissolvable in water the nickelous of water or cobalt compound (comprise and can form compound water-soluble behind the complex compound with complexing agent) for not chloride or fluorine any.Nickel ion or cobalt ion content are preferably 0.2g/L～1.1g/L.For example can be with single nickel salt or rose vitriol.
The fine and close promotor of blue rete is sodium wolframate, and content is preferably 0.5g/L～2g/L.
Blue differential arc oxidation film layer color and luster leveler is glycerine, and content is preferably 2ml/L～10ml/L.
Blue rete stablizer is b diammonium disodium edta, and content is preferably 2g/L～20g/L.
The tank liquor stablizer is sodium hydroxide or potassium hydroxide, and content is preferably 1g/L～3g/L.
The solution use temperature is preferably 15 ℃～65 ℃.
Embodiment 1:
A kind of blue series titanium alloy differential arc oxidation coloring solution, filling a prescription is:
Tertiary sodium phosphate: 8g/L
Single nickel salt: 2g/L
Sodium wolframate: 1g/L
Glycerine: 5ml/L
Disodium ethylene diamine tetraacetate: 10g/L
Sodium hydroxide: 2g/L
Embodiment 2:
A kind of blue series titanium alloy differential arc oxidation coloring solution, filling a prescription is:
Trisodium phosphate: 15g/L
Rose vitriol: 2g/L
Sodium wolframate: 0.8g/L
Glycerine: 8ml/L
Disodium ethylene diamine tetraacetate: 15g/L
Sodium hydroxide: 3g/L.
Embodiment 3:
A kind of blue series titanium alloy differential arc oxidation coloring solution, filling a prescription is:
Sodium phosphate dibasic: 10g/L
Single nickel salt: 4g/L
Sodium wolframate: 1.2g/L
Glycerine: 8ml/L
Disodium ethylene diamine tetraacetate: 18g/L
Sodium hydroxide: 1.8g/L.
Embodiment 4:
A kind of blue series titanium alloy differential arc oxidation coloring solution, filling a prescription is:
Tertiary sodium phosphate: 10g/L
Single nickel salt: 4.5g/L
Sodium wolframate: 1.8g/L
Glycerine: 6ml/L
Disodium ethylene diamine tetraacetate: 18g/L
Potassium hydroxide: 2g/L.
It is painted that solution provided by the invention carries out differential arc oxidation, and thicknesses of layers can reach 20 microns, and thicknesses of layers is the bluenesss that need at 2 microns～20 microns, and the rete color and luster that forms is stable, have anti-ly touch, wear-resisting characteristics.The rete densification can not adsorbed stain.More excellent is that rete does not contain organism, for a long time ultraviolet resistance.Rete can variable color below 600 ℃.
Introduce agent by phosphate system as the spark that differential arc oxidation generates ceramic membrane, phosphate concn is selected 4g/L～20g/L.Advantage is when generating ceramic membrane, spark is evenly distributed, and has also just guaranteed differential of the arc energy being evenly distributed on complicated shape, can guarantee complicated shape different sites even thickness, and this ceramic membrane porous nickel that forms becomes the tinting material uniformly good carrier that adds lustre in ceramic membrane.
Blue differential arc oxidation tinting material is selected water-soluble nickel salt and cobalt salt, and nickel or cobalt contents are 0.2g/L～1.1g/L, can add lustre in the ceramic membrane of part different sites evenly by fine assurance tinting material, and is blue soft, other interference colors can not occur.
The fine and close promotor of rete that adapts with blue differential arc oxidation film layer is sodium wolframate, and content is 0.5g/L～2g/L in the coloring liquid.Add this densification promotor and can guarantee the ceramic film porous nickel, the small and dense collection of hole is conducive to the active site concentration that tinting material adsorbs in ceramic membrane, guarantees chroma blue.
Differential arc oxidation film layer color and luster leveler is glycerine, and content is 2ml/L～10ml/L in the coloring liquid.Can better guarantee the complicated shape edge, the differential arc oxidation high current densities such as most advanced and sophisticated position zone can be because local roughness appear in overcurrent, and rete is loose.Can not cause because rete is loose aberration.
Blue rete stablizer is disodium ethylene diamine tetraacetate, and content is 2g/L～20g/L, and its cobalt ion or nickel ion in can the complexing tinting material avoids it to precipitate in basic solution, causes tinting material loss in the colouring slot liquid.
The tank liquor stablizer is sodium hydroxide or potassium hydroxide, and content is 1g/L～3g/L, and it can guarantee that on the one hand differential arc oxidation forms the solution of ceramic layer requirement and is the condition of alkalescence.Can avoid on the other hand in the tank liquor other compositions with Precipitation, increase Stability of Bath Solution.Increase simultaneously the electroconductibility of tank liquor, the reduction bath voltage is arranged, reduce the energy consumption effect.
Painted groove can be selected acrylic plastering groove or stainless steel tank.As select stainless steel tank, and stainless steel tank can connect the negative pole of differential arc oxidation coloring power source, and stainless steel trough body just can doublely be done the painted negative electrode of differential arc oxidation like this.
Blue differential arc oxidation colouring slot liquid collocation method is:
In pre-configured painted groove, add the deionized water of prewired liquor capacity 2/3.Add 1g/L～3g/L sodium hydroxide or potassium hydroxide, be stirred to dissolving.Add the chemical pure disodium ethylene diamine tetraacetate of 2g/L～20g/L, be stirred to dissolving.Agent (such as sodium phosphate or Sodium phosphate dibasic) is introduced in the chemical pure differential arc oxidation spark discharge that adds 4g/L～20g/L, after the stirring and dissolving, add with deionized water dissolving contain cobalt or the nickel amount is chemical pure cobalt salt or the nickel salt solution of 0.2g/L～1.1g/L, the limit adds, the limit stirring.Then add the chemical pure sodium wolframate of 0.5g/L～2g/L, the chemical pure glycerine of 2ml/L～10ml/L, stirring and dissolving.Replenish deionized water to the liquid level of prewired volume.
A kind of preparation method of blue series titanium alloy differential arc oxidation coloring solution comprises the steps:
Step 1: add deionized water
In pre-configured painted groove.If prewired volume is the V liter, add the deionized water of 2V/3.
Step 2: add blue rete stablizer
In the tank of step 1, according to prewired coloring liquid volume V liter, 1g/L～3g/L calculated amount adds chemical pure sodium hydroxide or potassium hydroxide, stirs until dissolving.
When sodium hydrate content or potassium hydroxide less than 1g/L, the sodium wolframate in the solution is separated out in differential arc oxidation easily, causes tank liquor muddy.When sodium hydroxide or potassium hydroxide content greater than 3g/L, to a certain degree corrosion phenomenon can appear in ceramic film, affects Film color.
Step 3: add the tank liquor stablizer
In the aqueous solution that step 2 obtains, according to prewired coloring liquid volume V liter, add the chemical pure disodium ethylene diamine tetraacetate with 2g/L～20g/L calculated amount, stir until dissolving.
When disodium ethylene diamine tetraacetate content less than 2g/L, the tinting material in the solution is separated out in the differential arc oxidation process easily, causes tank liquor muddy, rete is coarse.
When disodium ethylene diamine tetraacetate content greater than 20g/L, can affect the pigmentation of toner, cause the rete color and luster partially light.
Step 4: add the differential arc oxidation spark discharge and introduce agent
In the aqueous solution that step 3 obtains, according to prewired coloring liquid volume V liter, slowly add any in chemical pure tertiary sodium phosphate with 4g/L～20g/L calculated amount, Sodium phosphate dibasic, segregation sodium phosphate, trisodium phosphate, the inferior sodium phosphate, the limit edged stirs, until dissolving.
When phosphate content less than 4g/L, inhomogeneous at the ceramic layer thicknesses of layers that complicated shape form, when phosphate content greater than 20g/L, it is coarse even burn out part edge that rete appears in large galvanic areas easily on complicated shape.
Step 5: add blue series differential arc oxidation tinting material
According to prewired coloring liquid volume V liter, with the chemical pure single nickel salt of 1g/L～5g/L calculated amount or rose vitriol dissolving, the solution that then dissolving is obtained slowly joins in the aqueous solution that step 4 obtains with deionized water, and the limit edged stirs.
When single nickel salt or rose vitriol content less than 1g/L, the ceramic layer rete color and luster of formation is partially light, when single nickel salt or rose vitriol content greater than 5g/L, can affect the wear resistance of ceramic film and the compactness of rete.
Step 6: add blue rete compact agent
In the aqueous solution that step 5 obtains, according to prewired coloring liquid volume V liter, add the chemical pure sodium wolframate with 0.5g/L～2g/L calculated amount, stir until dissolving.
When sodium wolframate content less than 0.5g/L, it is slow to form ceramic layer speed, hole is excessive, is unfavorable for that painted thing sintering in ceramic membrane forms blueness.When sodium wolframate content greater than 2g/L, can stop the absorption of painted thing in ceramic film, the rete color and luster can be thin out.
Step 7: add blue differential arc oxidation film layer color and luster leveler
In the aqueous solution that step 6 obtains, according to prewired coloring liquid volume V liter, add glycerine with 2ml/L～10ml/L, stir.
When glycerol content less than 2ml/L, it is inhomogeneous to form the ceramic layer color and luster, it is coarse that rete appears in complicated shape large galvanic areas easily, the partially light situation of color and luster; When glycerol content greater than 10ml/L, form ceramic layer and dissolving trend can occur, film forming speed is slow.
Step 8: replenish deionized water to intending joining the volume V of solution
Replenish deionized water to volume V, stir.
The technical scheme that the present invention protects is not limited to the given embodiment of embodiment part, has alternative composition and the array mode of same nature and effect and contained other.
Claims (8)
1. a blue series titanium alloy differential arc oxidation coloring solution comprises the differential arc oxidation spark discharge introducing agent that produces differential arc oxidation, blue differential arc oxidation tinting material, the fine and close promotor of blue rete, blue differential arc oxidation film layer color and luster leveler, blue rete stablizer, tank liquor stablizer.Wherein:
It is phosphoric acid salt that agent is introduced in the differential arc oxidation spark discharge, and content is 4g/L～20g/L;
Blue differential arc oxidation tinting material is any nickel salt or cobalt salt that is dissolvable in water water of not chloride or fluorine.Nickel ion or cobalt ion content are 0.2g/L～1.1g/L;
The fine and close promotor of blue rete is that the fine and close promotor of blue rete is sodium wolframate, and content is 0.5g/L～2g/L;
Blue differential arc oxidation film layer color and luster leveler is glycerine, and content is 2ml/L～10ml/L;
Blue rete stablizer is disodium ethylene diamine tetraacetate, and content is 2g/L～20g/L;
The tank liquor stablizer is sodium hydroxide or potassium hydroxide, and content is 1g/L～3g/L.
2. a kind of blue series titanium alloy differential arc oxidation coloring solution according to claim 1, it is characterized in that: described coloring liquid use temperature is 15 ℃～65 ℃.
3. a kind of blue series titanium alloy differential arc oxidation coloring solution according to claim 2 is characterized in that: it is any in tertiary sodium phosphate, Sodium phosphate dibasic, segregation sodium phosphate, trisodium phosphate, the inferior sodium phosphate that phosphoric acid salt that agent adopts is introduced in described differential arc oxidation spark discharge.
4. a kind of blue series titanium alloy differential arc oxidation coloring solution according to claim 3, it is characterized in that: described blue differential arc oxidation tinting material is single nickel salt or rose vitriol, and content is 1g/L～5g/L.
5. the preparation method of a blue series titanium alloy differential arc oxidation coloring solution comprises the steps:
Step 1: add deionized water;
Step 2: add blue rete stablizer;
Step 3: add the tank liquor stablizer;
Step 4: add the differential arc oxidation spark discharge and introduce agent;
Step 5: add blue differential arc oxidation tinting material;
Step 6: add the fine and close promotor of blue rete;
Step 7: add blue differential arc oxidation film layer color and luster leveler;
Step 8: additional deionized water is to the liquor capacity of drafting.
6. the preparation method of a kind of blue series titanium alloy differential arc oxidation coloring solution according to claim 5 after blue differential arc oxidation tinting material is used deionized water dissolving, slowly adds, and should uninterruptedly stir in the adition process.
7. the preparation method of a kind of blue series titanium alloy differential arc oxidation coloring solution according to claim 5 is characterized in that: the painted groove that described preparation process adopts is polypropylene plastics hopper or stainless steel tank.
8. the preparation method of a kind of blue series titanium alloy differential arc oxidation coloring solution according to claim 7 is characterized in that: the described negative pole that holds the stainless steel tank connection differential arc oxidation coloring power source of solution.
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| CN103233258A (en) * | 2013-04-28 | 2013-08-07 | 哈尔滨工业大学 | Method for preparing dense enhancement type ceramic membrane based on micro-arc oxidizing and laser remelting |
| CN104651907A (en) * | 2014-10-08 | 2015-05-27 | 孟源 | Preparation process of titanium alloy having Ca and S micro-arc oxidation ceramic films |
| CN106435691A (en) * | 2016-11-18 | 2017-02-22 | 南昌航空大学 | One-step preparing method for TiAl-system-alloy micro-arc-oxidation BN composite membrane |
| CN106868568A (en) * | 2017-02-21 | 2017-06-20 | 中国船舶重工集团公司第七二五研究所 | Turn blue anodic oxidation device and the method for a kind of ultra-large type titanium alloy member |
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| CN103233258A (en) * | 2013-04-28 | 2013-08-07 | 哈尔滨工业大学 | Method for preparing dense enhancement type ceramic membrane based on micro-arc oxidizing and laser remelting |
| CN103233258B (en) * | 2013-04-28 | 2016-02-17 | 哈尔滨工业大学 | A kind of preparation method of the compactness enhancement type ceramic film based on differential arc oxidation and laser remolten |
| CN104651907A (en) * | 2014-10-08 | 2015-05-27 | 孟源 | Preparation process of titanium alloy having Ca and S micro-arc oxidation ceramic films |
| CN106435691A (en) * | 2016-11-18 | 2017-02-22 | 南昌航空大学 | One-step preparing method for TiAl-system-alloy micro-arc-oxidation BN composite membrane |
| CN106868568A (en) * | 2017-02-21 | 2017-06-20 | 中国船舶重工集团公司第七二五研究所 | Turn blue anodic oxidation device and the method for a kind of ultra-large type titanium alloy member |
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