CN101805917B - Preparation method of titanium alloy black anode oxidation treatment liquid - Google Patents
Preparation method of titanium alloy black anode oxidation treatment liquid Download PDFInfo
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- CN101805917B CN101805917B CN2010101314756A CN201010131475A CN101805917B CN 101805917 B CN101805917 B CN 101805917B CN 2010101314756 A CN2010101314756 A CN 2010101314756A CN 201010131475 A CN201010131475 A CN 201010131475A CN 101805917 B CN101805917 B CN 101805917B
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- titanium alloy
- treatment liquid
- oxidation treatment
- anode oxidation
- distilled water
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Abstract
The present invention relates to an oxidation process, in particular to a preparation method of a titanium alloy black anode oxidation treatment liquid, which is characterized in that the anode oxidation treatment liquid is prepared from the following components in parts by weight: 20 to 60 parts of potassium dichromate (K2Cr2O7), 10 to 20 parts of manganese sulfate (MnSO4), 2 to 4 parts of blackening agent, 25 to 55 parts of ammonium sulfate (NH4)2SO4 and 1000 parts of distilled water. The titanium alloy black anode oxidation process of the present invention ensures a black, uniform and firm oxidation film to be formed on the surface of a titanium alloy part, and satisfies a special requirement that a titanium alloy surface applied in an optical system needs extinction.
Description
Technical field:
The present invention relates to a kind of oxidizing process, particularly a kind of at titanium alloy black anode oxidation treatment liquid compound method, belong to metal finishing anodizing technology field.
Background technology:
Titanium alloy has good comprehensive mechanical properties, and the structure stability height is widely used in the shell of rocket engine, high-end scientific and technological industrys such as aero-engine compressor dish, impeller assembly, fastening piece.The anodised technology of general employing during titanium alloy is made at the oxide film of its surface formation one deck densification, is protected its matrix.Present common titanium alloy anode oxidation technique, can form the oxide film (as cyan) of different colours or the oxidation film layer of many colors at titanium alloy surface, make when titanium alloy is used for optical system, can influence the precision of optical system or become phase effect, and exist rete insecure, easily come off, influence the one-tenth phase effect of optical system, and then influence the quality of product.
Summary of the invention:
Technical problem to be solved by this invention is: the compound method that a kind of titanium alloy black anode oxidation treatment liquid is provided, form firm oxidation film layer black, even on the titanium alloy component surface, satisfied the particular requirement of the titanium alloy surface needs delustring that is applied in the optical system.
For solving the problems of the technologies described above, the technical solution used in the present invention is: design a kind of compound method of titanium alloy black anode oxidation treatment liquid, it is characterized in that: anode oxidation treatment liquid is by potassium bichromate K
2Cr
2O
7, manganous sulfate MnSO
4, blackening agent for surface, ammonium sulfate (NH
4)
2SO
4, distilled water, by following weight part preparation: potassium bichromate K
2Cr
2O
7Be 20-60 part, manganous sulfate MnSO
4Be 10-20 part, blackening agent for surface 2-4 part, ammonium sulfate (NH
4)
2SO
4Be 25-55 part, 1000 parts of distilled water.
A kind of compound method of titanium alloy black anode oxidation treatment liquid, its flow process are to carry out according to the following steps:
1), uses Solvent degreasing;
2), dress is hung;
3), electrochemical deoiling;
4), washing;
5), pickling, sandblast;
6), washing;
7), anodic oxidation;
8), washing;
9), drying;
10), deliver for a check.
Chemical solvents is prepared by following weight part in the process of described electrochemical deoiling: technical pure sodium hydroxide NaOH 30-40 part, technical pure yellow soda ash Na
2CO
320-30 part, technical pure sodium phosphate Na
3PO
41000 parts of 50-70 parts, technical pure water glass 10-15 part, distilled water.
Described anodised treatment condition are: anodic current density is 0.1 ~ 0.3A/dm2,5 ℃＜30 ℃ of temperature, and 45-55 minute anode time, negative electrode is a stainless steel plate, and hanger is the aluminum hanger, can also be titanium material and titanium alloy, and giving electric mode is staged.
Described anodised treatment condition are: anodic current density is 0.2A/dm2,25 ℃ of temperature, and 50 minutes anode time, negative electrode is a stainless steel plate, and hanger is the aluminum hanger, can also be titanium material and titanium alloy, and giving electric mode is staged.
The collocation method of described anode oxidation treatment liquid is: add potassium bichromate K in distilled water sequentially successively
2Cr
2O
7, manganous sulfate MnSO
4, blackening agent for surface, ammonium sulfate (NH
4)
2SO
4, and stir.
Described potassium bichromate K
2Cr
2O
7Be chemical pure, manganous sulfate MnSO
4Be chemical pure, blackening agent for surface is a technical pure, ammonium sulfate (NH
4)
2SO
4Be technical pure.
Described blackening agent for surface 2-4 part specifically is Potassium Persulphate K
2S
2O
8Be 0.2-0.6 part, Sodium Fluoride NaF is 0.02-0.08 part, and distilled water is 1.78-3.32 part.
The configuration of described anode oxidation treatment liquid: get distillation 1000kg, add chemical pure potassium bichromate K earlier
2Cr
2O
7After the 33 kg dissolving, again by adding chemical pure manganous sulfate MnSO successively in proper order
414 kg, technical pure blackening agent for surface 3 kg, technical pure ammonium sulfate (NH
4)
2SO
440 kg, and stir; Wherein contain 0.36kg Potassium Persulphate K among blackening agent for surface 3 kg
2S
2O
8, 0.045kg Sodium Fluoride NaF, 2.595kg distilled water.
The oxide thickness of the titanium alloy surface black after the processing is 3-8 μ m.
The advantage of a kind of titanium alloy black anode oxidation process of the present invention is: owing to adopted titanium alloy black anode oxidation process of the present invention, make titanium alloy surface form firm oxidation film layer black, even, sticking power is good, difficult drop-off, firmly wipe examination with clean fine cloth and do not fall, better satisfied the particular requirement of the titanium alloy surface needs delustring that is applied in the optical system.
Embodiment:
Embodiment 1
1, the configuration of anode oxidation treatment liquid: get distillation 1000kg, add chemical pure potassium bichromate K earlier
2Cr
2O
7After the 33 kg dissolving, again by adding chemical pure manganous sulfate MnSO successively in proper order
414 kg, technical pure blackening agent for surface 3 kg, technical pure ammonium sulfate (NH
4)
2SO
440 kg, and stir; Wherein contain 0.36kg Potassium Persulphate K among blackening agent for surface 3 kg
2S
2O
8, 0.045kg Sodium Fluoride NaF, 2.595kg distilled water.
2, the configuration of chemical solvents: get distilled water 1000 kg, after the adding technical pure sodium hydroxide NaOH 35 kg dissolving earlier, again by adding technical pure yellow soda ash Na successively in proper order
2CO
325 kg, technical pure sodium phosphate Na
3PO
460 kg, technical pure water glass 12 kg, and stir.
3, anodic oxidation treatment
With titanium alloy component in turn through 1), use Solvent degreasing: it is with clean gasoline 23 ℃ of temperature, also can be that other organic solvent soaks titanium alloy component 4 minutes, can brush away greasy dirt with fine, soft fur for the bigger screw thread of other greasy dirt or the part of stria shape, oil removing relief titanium alloy component seasoning or dry up with pressurized air; 2), dress is hung; 3), electrochemical deoiling: titanium alloy component is put into chemical solvents when temperature is 78 ℃, soaked 6.5 minutes; 4), washing: with the flushing of mobile water; 5), pickling (sandblast); 6), washing: with the flushing of mobile water; 7) anodic oxidation, titanium alloy component hangs with the aluminum hanger, hanger is used for the titanium alloy component contact position and will contacts well, put into the anode oxidation treatment liquid that configures then, maintenance treatment solution temperature＜30 ℃, negative electrode adopts stainless steel plate, and anodic current density is controlled at 0.2A/dm2, give electricity, anodizing time 50 minutes in the staged mode.
This kind prescription and condition are best, and under this technical recipe and the condition, titanium alloy component is after anodic oxidation treatment, and its oxide thickness is 5.5 μ m, and black is evenly fine and closely woven, covers complete; Again through 8) washing: with the flushing of mobile water; 9) drying: dry or dry up with pressurized air; 10) deliver for a check: titanium alloy component surface forms the black oxidation rete and firmly wipes repeatedly with clean fine cloth and try, without any coming off or the phenomenon of peeling.
Embodiment 2
1, the configuration of anode oxidation treatment liquid: get distillation 1000kg, add chemical pure potassium bichromate K earlier
2Cr
2O
7After the 20 kg dissolving, again by adding chemical pure manganous sulfate MnSO successively in proper order
410 kg, technical pure blackening agent for surface 2kg, technical pure ammonium sulfate (NH
4)
2SO
425 kg, and stir; Wherein contain 0.2kg Potassium Persulphate K among blackening agent for surface 2 kg
2S
2O
8, 0.02kg Sodium Fluoride NaF, 1.78kg distilled water.
2, the configuration of chemical solvents: get distilled water 1000 kg, after the adding technical pure sodium hydroxide NaOH 30kg dissolving earlier, again by adding technical pure yellow soda ash Na successively in proper order
2CO
320 kg, technical pure sodium phosphate Na
3PO
450 kg, technical pure water glass 10 kg, and stir.
3, anodic oxidation treatment
With titanium alloy component in turn through 1), use Solvent degreasing: it is with clean gasoline 10 ℃ of temperature, also can be that other organic solvent soaks titanium alloy component 3 minutes, can brush away greasy dirt with fine, soft fur for the bigger screw thread of other greasy dirt or the part of stria shape, oil removing relief titanium alloy component seasoning or dry up with pressurized air; 2), dress is hung; 3), electrochemical deoiling: titanium alloy component is put into chemical solvents when temperature is 70 ℃, soaked 3 minutes; 4), washing: with the flushing of mobile water; 5), pickling (sandblast); 6), washing: with the flushing of mobile water; 7) anodic oxidation, titanium alloy component hangs with titanium material system hanger, hanger is used for the titanium alloy component contact position and will contacts well, put into the anode oxidation treatment liquid that configures then, keep 5 ℃ of treatment solution temperature, negative electrode adopts stainless steel plate, and anodic current density is controlled at 0.1A/dm2, give electricity, anodizing time 45 minutes in the staged mode.
Under this kind prescription and the condition, titanium alloy component is after anodic oxidation treatment, and its oxide thickness is 3 μ m, and light/dark balance is evenly fine and closely woven, covers complete; Again through 8) washing: with the flushing of mobile water; 9) drying: dry or dry up with pressurized air; 10) deliver for a check: titanium alloy component surface forms the light/dark balance oxidation film layer and firmly wipes repeatedly with clean fine cloth and try, without any coming off or the phenomenon of peeling.
Embodiment 3
1, the configuration of anode oxidation treatment liquid: get distillation 1000kg, add chemical pure potassium bichromate K earlier
2Cr
2O
7After the 60 kg dissolving, again by adding chemical pure manganous sulfate MnSO successively in proper order
420 kg, technical pure blackening agent for surface 4kg, technical pure ammonium sulfate (NH
4)
2SO
455 kg, and stir; Wherein contain 0.6kg Potassium Persulphate K among the blackening agent for surface 4kg
2S
2O
8, 0.08kg Sodium Fluoride NaF, 3.32kg distilled water.
2, the configuration of chemical solvents: get distilled water 1000 kg, after the adding technical pure sodium hydroxide NaOH 40kg dissolving earlier, again by adding technical pure yellow soda ash Na successively in proper order
2CO
330 kg, technical pure sodium phosphate Na
3PO
470 kg, technical pure water glass 15 kg, and stir.
3, anodic oxidation treatment
With titanium alloy component in turn through 1), use Solvent degreasing: it is with clean gasoline 35 ℃ of temperature, also can be that other organic solvent soaks titanium alloy component 5 minutes, can brush away greasy dirt with fine, soft fur for the bigger screw thread of other greasy dirt or the part of stria shape, oil removing relief titanium alloy component seasoning or dry up with pressurized air; 2), dress is hung; 3), electrochemical deoiling: titanium alloy component is put into chemical solvents when temperature is 85 ℃, soaked 10 minutes; 4), washing: with the flushing of mobile water; 5), pickling (sandblast); 6), washing: with the flushing of mobile water; 7) anodic oxidation, titanium alloy component hangs with the titanium alloys hanger, hanger is used for the titanium alloy component contact position and will contacts well, put into the anode oxidation treatment liquid that configures then, keep 30 ℃ of treatment solution temperature, negative electrode adopts stainless steel plate, and anodic current density is controlled at 0.3A/dm2, give electricity, anodizing time 55 minutes in the staged mode.
Under this kind prescription and the condition, titanium alloy component is after anodic oxidation treatment, and its oxide thickness is 8 μ m, and aterrimus is evenly fine and closely woven, covers complete; Again through 8) washing: with the flushing of mobile water; 9) drying: dry or dry up with pressurized air; 10) deliver for a check: titanium alloy component surface forms the aterrimus oxidation film layer and firmly wipes repeatedly with clean fine cloth and try, without any coming off or the phenomenon of peeling.
Adopted titanium alloy black anode oxidation process of the present invention, make the titanium alloy component surface form firm oxidation film layer black, even, sticking power is good, difficult drop-off, firmly wipe examination repeatedly with clean fine cloth, without any coming off or the phenomenon of peeling, better satisfied the particular requirement of the titanium alloy surface needs delustring that is applied in the optical system.
Claims (2)
1. the compound method of a titanium alloy black anode oxidation treatment liquid, it is characterized in that: anode oxidation treatment liquid is by potassium bichromate K
2Cr
2O
7, manganous sulfate MnSO
4, blackening agent for surface, ammonium sulfate (NH
4)
2SO
4, distilled water, by following weight part preparation: potassium bichromate K
2Cr
2O
7Be 20-60 part, manganous sulfate MnSO
4Be 10-20 part, blackening agent for surface 2-4 part, ammonium sulfate (NH
4)
2SO
4Be 25-55 part, 1000 parts of distilled water; Described blackening agent for surface 2-4 part specifically is Potassium Persulphate K
2S
2O
8Be 0.2-0.6 part, Sodium Fluoride NaF is 0.02-0.08 part, and distilled water is 1.78-3.32 part.
2. the compound method of a kind of titanium alloy black anode oxidation treatment liquid according to claim 1 is characterized in that: the configuration of described anode oxidation treatment liquid: get distilled water 1000kg, add chemical pure potassium bichromate K earlier
2Cr
2O
7Be after the 33 kg dissolving, again by adding chemical pure manganous sulfate MnSO successively in proper order
4Be 14 kg, technical pure blackening agent for surface 3 kg, technical pure ammonium sulfate (NH
4)
2SO
4Be 40 kg, and stir; Wherein contain 0.36kg Potassium Persulphate K among blackening agent for surface 3 kg
2S
2O
8, 0.045kg Sodium Fluoride NaF, 2.595kg distilled water.
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|---|---|---|---|
| CN2010101314756A CN101805917B (en) | 2010-03-24 | 2010-03-24 | Preparation method of titanium alloy black anode oxidation treatment liquid |
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| CN101805917B true CN101805917B (en) | 2011-12-07 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106149029A (en) * | 2014-12-05 | 2016-11-23 | 财团法人金属工业研究发展中心 | Black titanium-containing oxide layer, preparation method thereof and implant |
Families Citing this family (6)
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|---|---|---|---|---|
| CN102653877A (en) * | 2011-03-04 | 2012-09-05 | 汉达精密电子(昆山)有限公司 | Electrolyte for anodic oxidation treatment of magnesium alloy and treatment method thereof |
| CN104060262B (en) * | 2014-05-26 | 2016-06-15 | 安徽红桥金属制造有限公司 | A kind of cast member surface blackening New Process for Treatment |
| CN104389001A (en) * | 2014-11-26 | 2015-03-04 | 江西洪都航空工业集团有限责任公司 | Anodic oxidation pretreatment method for environment-friendly titanium alloy |
| CN106702461B (en) * | 2016-12-28 | 2018-11-30 | 佛山市铠斯钛科技有限公司 | A kind of titanium magnesium alloy anodizing solution |
| CN109881236B (en) * | 2019-02-28 | 2020-08-04 | 深圳市中科东明表面处理新材料技术有限公司 | Titanium alloy black anodic oxidation liquid and titanium alloy surface treatment method |
| CN110699733B (en) * | 2019-11-20 | 2020-08-11 | 中国计量大学 | Preparation method, product and application of titanium alloy porous oxide film |
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| EP0780495A2 (en) * | 1995-12-22 | 1997-06-25 | KM Europa Metal Aktiengesellschaft | Process for obtaining a brochantit patina on a copper surface |
| CN101457383A (en) * | 2008-12-29 | 2009-06-17 | 长春奥普光电技术股份有限公司 | Titanium alloy black anodic oxidation method capable of reducing oxidation film layer stress |
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|---|---|---|---|---|
| EP0780495A2 (en) * | 1995-12-22 | 1997-06-25 | KM Europa Metal Aktiengesellschaft | Process for obtaining a brochantit patina on a copper surface |
| CN101457383A (en) * | 2008-12-29 | 2009-06-17 | 长春奥普光电技术股份有限公司 | Titanium alloy black anodic oxidation method capable of reducing oxidation film layer stress |
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| CN106149029A (en) * | 2014-12-05 | 2016-11-23 | 财团法人金属工业研究发展中心 | Black titanium-containing oxide layer, preparation method thereof and implant |
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Application publication date: 20100818 Assignee: Xi'an Xiguang Surface Finishing Co., Ltd. Assignor: North Electro-Optics Group Co.,Ltd. Contract record no.: 2013610000015 Denomination of invention: Preparation method of titanium alloy black anode oxidation treatment liquid Granted publication date: 20111207 License type: Exclusive License Record date: 20130412 |
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