CN102234835B - Stripping solution and method for stripping titanium carbide film layer by electrolysis - Google Patents
Stripping solution and method for stripping titanium carbide film layer by electrolysis Download PDFInfo
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- CN102234835B CN102234835B CN201010151339.3A CN201010151339A CN102234835B CN 102234835 B CN102234835 B CN 102234835B CN 201010151339 A CN201010151339 A CN 201010151339A CN 102234835 B CN102234835 B CN 102234835B
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- decoating liquid
- titanium carbide
- complexing agent
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- alkali metal
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/02—Etching
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- Chemical Kinetics & Catalysis (AREA)
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- Electrodes For Compound Or Non-Metal Manufacture (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
Abstract
The invention provides a stripping solution which is used for stripping a titanium carbide film layer by a two-step electrolytic method, and the stripping solution comprises a first stripping solution and a second stripping solution; the first stripping solution comprises 2-80 g/L of soluble alkali metal hydroxides and 5-100 g/L of aqueous solutions of complexing agents which have complexation effect with titanium ions; the second stripping solution comprises 50-300 g/L of soluble alkali metal hydroxides, 5-100 g/L of complexing agents which have complexation effect with titanium ions, and 10-60 g/L of aqueous solutions of alcohol amine compounds which have complexation with the titanium ion. The compexing agents in the first stripping solution and the second stripping solution do not contain the alcohol amine compounds. The invention also provides a method for stripping a titanium carbide film layer by electrolysis by using the stripping solution.
Description
Technical field
The present invention relates to a kind of decoating liquid of electrolytic removal substrate surface titanium carbide rete and utilize the method for this decoating liquid electrolytic removal titanium carbide rete.
Background technology
Coating process has a wide range of applications at industrial circle.Yet needing plated film is stripped under following two kinds of situations usually: through behind the life-time service, the plated film of workpiece surface has been damaged or serious aging (1), needs to remove coating, plating again; (2) aborning, the coating of institute's plating does not meet quality requirements, for reducing the loss, saves cost, need return coating, allows the workpiece plated film again of doing over again.Therefore, how under the situation of not damaging base material, it is a major issue the industrial production that coating is removed fully from substrate surface.
Titanium carbide (TiC) film is a kind of coating of excellent property, has very strong anti-oxidant, erosion resistance and wear resistance, has broad application prospects at industrial circle.During vacuum moulding machine titanium carbide rete, usually adjust the color of titanium carbide rete by the content of constantly adjusting carbon, so the carbon content difference at different thickness place in the titanium carbide rete, the carbon content at general outermost layer place is the highest.Titanium carbonitride film for this carbon content increases gradually if the one-step electrolysis method of employing strips, need apply greater than 12A/dm usually
2Above current density, and the time of electrolysis is longer.This method is owing to the big electric current that applies of long period, and the possibility that makes base material be corroded improves greatly, and energy consumption is bigger, and required time is longer.
Summary of the invention
In view of this, be necessary to provide a kind of not easy damaged base material, energy consumption is less, and can strip the electrolytic stripping solution of titanium carbide rete effectively.
In addition, be necessary to provide a kind of method of using above-mentioned electrolytic stripping solution stripping titanium carbide rete.
A kind of decoating liquid of electrolytic removal titanium carbide rete, this decoating liquid has the complexing agent of complexing action and 10 ~ 60g/L and titanium ion that the aqueous solution of the alcamine compound of complexing action is arranged for containing 50 ~ 300g/L soluble alkali metal oxyhydroxide, 5 ~ 100g/L and titanium ion, and described complexing agent does not comprise alcamine compound.
A kind of decoating liquid, be used for two one-step electrolysis methods stripping titanium carbide rete, this decoating liquid comprises first decoating liquid and second decoating liquid, and this first decoating liquid is for containing the aqueous solution that 2 ~ 80g/L soluble alkali metal oxyhydroxide and 5 ~ 100g/L and titanium ion have the complexing agent of complexing action; This second decoating liquid has the complexing agent of complexing action and 10 ~ 60g/L and titanium ion that the aqueous solution of the alcamine compound of complexing action is arranged for containing 50 ~ 300g/L soluble alkali metal oxyhydroxide, 5 ~ 100g/L and titanium ion, and the complexing agent in described first decoating liquid, second decoating liquid does not comprise alcamine compound.
A kind of method of electrolytic removal titanium carbide rete may further comprise the steps:
The surface is formed with the base material of titanium carbide rete as anode, in first decoating liquid, carry out the first step electrolysis, strip this titanium carbide rete with part, this first decoating liquid has the aqueous solution of the complexing agent of complexing action for what contain 2 ~ 80g/L soluble alkali metal oxyhydroxide and 5 ~ 100g/L with titanium ion, complexing agent in this first decoating liquid does not comprise alcamine compound, and described base material is ferrous alloy;
Clean the base material after this first step electrolysis;
Base material after this is cleaned is as anode, in second decoating liquid, carry out second one-step electrolysis, to strip the remaining titanium carbide rete of this substrate surface, this second decoating liquid has the complexing agent of complexing action and 10 ~ 60g/L and titanium ion that the aqueous solution of the alcamine compound of complexing action is arranged for containing 50 ~ 300g/L soluble alkali metal oxyhydroxide, 5 ~ 100g/L and titanium ion, and the complexing agent in this second decoating liquid does not comprise alcamine compound.
Compared to prior art, compared to prior art, the decoating liquid of described electrolytic removal titanium carbide rete and electrolytic removal titanium carbonitride film layer method be the easy damaged base material not, and energy consumption is less, and can strip the titanium carbide rete that is formed at substrate surface effectively.
Embodiment
Decoating liquid of the present invention is applicable to the titanium carbide rete that is formed at substrate surface by electrolytic removal.Described base material is ferrous alloy, as stainless steel.
Decoating liquid of the present invention comprises first decoating liquid and second decoating liquid.
This first decoating liquid is the aqueous solution that contains alkali and promotor.The alkali of this first decoating liquid is soluble alkali metal oxyhydroxide, for example, can be a kind of or its combination in sodium hydroxide and the potassium hydroxide.The concentration of this alkali can be 2 ~ 80g/L, is preferably 5 ~ 50g/L.Described alkali plays electric action in first decoating liquid, alkaline environment is provided simultaneously, and the titanium carbide rete can be partially dissolved in first decoating liquid.
The promotor of this first decoating liquid be for can there being the complexing agent of complexing action with titanium ion, as being one or more the mixture in Seignette salt, Sunmorl N 60S, Trisodium Citrate and the ethylenediamine tetraacetic acid (EDTA) compounds such as (EDTA).The concentration of promotor is 5 ~ 100g/L, is preferably 5 ~ 40g/L.After chromium in this titanium carbide rete is dissolved in first decoating liquid, with promotor complexing action takes place and form complex compound, therefore is conducive to the lasting dissolving in the titanium carbide rete.
This first decoating liquid can be by with above-mentioned alkali with promotor is water-soluble makes.
This second decoating liquid is the aqueous solution that contains alkali, promotor and auxiliary.
The alkali of this second decoating liquid is similarly soluble alkali metal oxyhydroxide, for example, can be a kind of or its combination in sodium hydroxide and the potassium hydroxide.The concentration of alkali can be 50 ~ 300g/L in this second decoating liquid, is preferably 120 ~ 180g/L.Alkali plays a part similar in alkali in described second decoating liquid and first decoating liquid.
Promotor being similarly of this second decoating liquid can have the complexing agent of complexing action with titanium ion, as being one or more the mixture in Seignette salt, Sunmorl N 60S, Trisodium Citrate and the ethylenediamine tetraacetic acid (EDTA) compounds such as (EDTA).The promoter concentration of second decoating liquid is 5 ~ 100g/L, is preferably 5 ~ 40g/L.The promotor of the promotor of this second decoating liquid and first decoating liquid is played similar effect.
This auxiliary is the compound that complexing action can be arranged with titanium in the alcamines organism, and as trolamine, thanomin and diethanolamine etc., it can be preferably trolamine for one or more the mixture in the above compound.The concentration of this auxiliary is 10 ~ 60g/L, is preferably 18 ~ 40g/L.What produce in the adsorbable electrolytic deplating process process of this auxiliary is dirty, after being conducive to strengthen electrolysis and finishing to the washing effect of base material.
This second decoating liquid can be by making above-mentioned alkali, promotor and auxiliary are water-soluble.
First decoating liquid of above-mentioned decoating liquid and second decoating liquid can be used for the electrolytic solution of one-step electrolysis method stripping titanium carbide rete separately, also can be used separately as the electrolytic solution of two one-step electrolysis methods stripping titanium carbide rete.
Utilize the method for above-mentioned decoating liquid electrolytic removal titanium carbide rete, may further comprise the steps:
At first, the base material that the surface is formed with the titanium carbide rete carries out the first step electrolysis in above-mentioned first decoating liquid.This first decoating liquid is heated to 50 ~ 95 ℃, is preferably 60 ~ 80 ℃.Described base material soaked place first decoating liquid, and with this base material as anode, with stainless steel plate or carbon plate as negative electrode, with 1 ~ 10A/dm
2Current density electrolysis 3 ~ 8 minutes, make the stripping of titanium carbonitride film layer segment.Preferred 4 ~ the 7A/dm of described current density
2This first step electrolysis makes in this titanium carbide rete the higher part of carbon content at first dissolve.
After finishing the first step electrolysis this base material water is cleaned, in above-mentioned second decoating liquid, carry out second one-step electrolysis then.Above-mentioned second decoating liquid is heated to 50 ~ 95 ℃, is preferably 60 ~ 80 ℃.The base material that the surface is formed with the titanium carbide rete soaks and places this second decoating liquid, and with this base material that is formed with the titanium carbide rete as anode, with stainless steel plate or carbon plate as negative electrode, with 1 ~ 10A/dm
2Current density electrolysis 3 ~ 8 minutes, with the remaining titanium carbide rete of stripping substrate surface.Preferred 4 ~ the 7A/dm of described current density
2
After finishing second one-step electrolysis, base material being carried out water clean, is cleanings that neutralize of 5% sulphuric acid soln with weight content then, and washing afterwards again, drying gets final product.
The present invention is described in more detail below by embodiment.
Embodiment 1
Prepare first decoating liquid and second decoating liquid of decoating liquid respectively.This first decoating liquid is made up of the sodium hydroxide of 5g/L, the ethylenediamine tetraacetic acid (EDTA) of 10g/L (ED TA) and the water of surplus.This second decoating liquid is made up of the sodium hydroxide of 150g/L, the sodium tartrate of 20g/L, the trolamine of 33g/L and the water of surplus.
Carry out the first step electrolysis.This first decoating liquid is heated to 60 ℃, it is that the sample of the titanium carbide rete of about 2 μ m soaks and places first decoating liquid that the stainless steel substrate surface is formed with thickness, and with this stainless steel substrate that is formed with the titanium carbide rete as anode, make negative electrode with carbon plate, use 4A/dm
2Current density electrolysis 4 minutes, make this titanium carbonitride film layer segment dissolving.
Water cleans this sample after the first step electrolysis, carries out second one-step electrolysis then.Second decoating liquid is heated to 80 ℃, this sample is soaked places second decoating liquid, and with this sample as anode, make negative electrode with carbon plate, use 5A/dm
2Current density electrolysis 4 minutes, the remaining titanium carbide rete in stainless steel substrate surface is stripped fully.
Then to stainless steel substrate clean, neutralization and drying treatment.
Embodiment 2
Embodiment 2 and embodiment 1 are except decoating liquid is different, and other Step By Conditions are all identical.First decoating liquid of the decoating liquid of embodiment 2 is made up of the sodium hydroxide of 20g/L, the ethylenediamine tetraacetic acid (EDTA) of 20g/L (ED TA) and the water of surplus; Second decoating liquid is made up of the sodium hydroxide of 75g/L, the Trisodium Citrate of 20g/L, the trolamine of 28.6g/L and the water of surplus.
Embodiment 3
Prepare first decoating liquid and second decoating liquid of decoating liquid respectively.This first decoating liquid is made up of the potassium hydroxide of 10g/L, the Sunmorl N 60S of 10g/L and the water of surplus.This second decoating liquid is made up of the potassium hydroxide of 100g/L, the sodium tartrate of 10g/L, the Sunmorl N 60S of 5g/L, the trolamine of 16.3g/L and the water of surplus.
Carry out the first step electrolysis.This first decoating liquid is heated to 65 ℃, it is that the sample of the titanium carbide rete of about 2 μ m soaks and places first decoating liquid that the stainless steel substrate surface is formed with thickness, and with this stainless steel substrate that is formed with the titanium carbide rete as anode, make negative electrode with carbon plate, use 3A/dm
2Current density electrolysis 5 minutes, make this titanium carbonitride film layer segment dissolving.
Water cleans this sample after the first step electrolysis, carries out second one-step electrolysis then.Second decoating liquid is heated to 80 ℃, this sample is soaked places second decoating liquid, and with this sample as anode, make negative electrode with carbon plate, use 6A/dm
2Current density electrolysis 5 minutes, this remaining titanium carbide rete in stainless steel substrate surface is stripped fully.
Then to stainless steel substrate clean, neutralization and drying treatment.
Sample behind the stripping rete in above-described embodiment 1 to embodiment 3 is done X-ray diffraction (X-RD) analysis, do not find that all the Cr element exists, and proves that rete strips fully; Sample behind the stripping rete is carried out scanning electron microscope (SEM) test, find that base material is not all corroded.
Claims (13)
1. the decoating liquid of an electrolytic removal titanium carbide rete, it is characterized in that: this decoating liquid has the complexing agent of complexing action and 10 ~ 60g/L and titanium ion that the aqueous solution of the alcamine compound of complexing action is arranged for containing 50 ~ 300g/L soluble alkali metal oxyhydroxide, 5 ~ 100g/L and titanium ion, and described complexing agent does not comprise alcamine compound.
2. the decoating liquid of electrolytic removal titanium carbide rete as claimed in claim 1 is characterized in that: this soluble alkali metal oxyhydroxide is a kind of or its combination in sodium hydroxide and the potassium hydroxide, and the concentration of this soluble alkali metal oxyhydroxide is 120 ~ 180g/L.
3. the decoating liquid of electrolytic removal titanium carbide rete as claimed in claim 1, it is characterized in that: this complexing agent is one or more the mixture in Seignette salt, Sunmorl N 60S, Trisodium Citrate and the ethylenediamine tetraacetic acid (EDTA), and the concentration of this complexing agent is 5 ~ 40g/L.
4. the decoating liquid of electrolytic removal titanium carbide rete as claimed in claim 1 is characterized in that: this alcamine compound is selected from one or more the combination in trolamine, thanomin and the diethanolamine, and the concentration of this alcamine compound is 18 ~ 40g/L.
5. decoating liquid, be used for two one-step electrolysis methods stripping titanium carbide rete, this decoating liquid comprises first decoating liquid and second decoating liquid, it is characterized in that: this first decoating liquid is for containing the aqueous solution that 2 ~ 80g/L soluble alkali metal oxyhydroxide and 5 ~ 100g/L and titanium ion have the complexing agent of complexing action; This second decoating liquid has the complexing agent of complexing action and 10 ~ 60g/L and titanium ion that the aqueous solution of the alcamine compound of complexing action is arranged for containing 50 ~ 300g/L soluble alkali metal oxyhydroxide, 5 ~ 100g/L and titanium ion, and the complexing agent in described first decoating liquid, second decoating liquid does not comprise alcamine compound.
6. decoating liquid as claimed in claim 5, it is characterized in that: the soluble alkali metal oxyhydroxide in this first decoating liquid and second decoating liquid is a kind of or its combination in sodium hydroxide and the potassium hydroxide, the concentration of soluble alkali metal oxyhydroxide is 5 ~ 50g/L in this first decoating liquid, and the concentration of soluble alkali metal oxyhydroxide is 120 ~ 180g/L in this second decoating liquid.
7. decoating liquid as claimed in claim 5, it is characterized in that: the complexing agent in this first decoating liquid and second decoating liquid is one or more the mixture in Seignette salt, Sunmorl N 60S, Trisodium Citrate and the ethylenediamine tetraacetic acid (EDTA), and the concentration of the complexing agent in this first decoating liquid and second decoating liquid is 5 ~ 40g/L.
8. decoating liquid as claimed in claim 5 is characterized in that: this alcamine compound is selected from one or more the combination in trolamine, thanomin and the diethanolamine, and the concentration of this alcamine compound is 18 ~ 40g/L.
9. the method for an electrolytic removal titanium carbide rete may further comprise the steps:
The surface is formed with the base material of titanium carbide rete as anode, in first decoating liquid, carry out the first step electrolysis, strip this titanium carbide rete with part, this first decoating liquid has the aqueous solution of the complexing agent of complexing action for what contain 2 ~ 80g/L soluble alkali metal oxyhydroxide and 5 ~ 100g/L with titanium ion, complexing agent in this first decoating liquid does not comprise alcamine compound, and described base material is ferrous alloy;
Clean the base material after this first step electrolysis;
Base material after this is cleaned is as anode, in second decoating liquid, carry out second one-step electrolysis, to strip the remaining titanium carbide rete of this substrate surface, this second decoating liquid has the complexing agent of complexing action and 10 ~ 60g/L and titanium ion that the aqueous solution of the alcamine compound of complexing action is arranged for containing 50 ~ 300g/L soluble alkali metal oxyhydroxide, 5 ~ 100g/L and titanium ion, and the complexing agent in this second decoating liquid does not comprise alcamine compound.
10. the method for electrolytic removal titanium carbide rete as claimed in claim 9, it is characterized in that: the temperature of this first decoating liquid and second decoating liquid is 50 ~ 95 ℃.
11. the method for electrolytic removal titanium carbide rete as claimed in claim 10 is characterized in that: the temperature of this first decoating liquid and second decoating liquid is 60 ~ 80 ℃.
12. the method for electrolytic removal titanium carbide rete as claimed in claim 9 is characterized in that: the current density of this first step electrolysis and second electrolysis is 1 ~ 10A/dm
2, electrolysis time is 3 ~ 8 minutes.
13. the method for electrolytic removal titanium carbide rete as claimed in claim 12 is characterized in that: the current density of this first step electrolysis and second electrolysis is 4 ~ 7A/dm
2
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010151339.3A CN102234835B (en) | 2010-04-20 | 2010-04-20 | Stripping solution and method for stripping titanium carbide film layer by electrolysis |
| US12/974,208 US20110253556A1 (en) | 2010-04-20 | 2010-12-21 | Solution system for electrolytically removing titanium carbide coating and method for same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201010151339.3A CN102234835B (en) | 2010-04-20 | 2010-04-20 | Stripping solution and method for stripping titanium carbide film layer by electrolysis |
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| Publication Number | Publication Date |
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| CN102234835A CN102234835A (en) | 2011-11-09 |
| CN102234835B true CN102234835B (en) | 2013-07-03 |
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| CN201010151339.3A Expired - Fee Related CN102234835B (en) | 2010-04-20 | 2010-04-20 | Stripping solution and method for stripping titanium carbide film layer by electrolysis |
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| CN (1) | CN102234835B (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102628176A (en) * | 2012-04-21 | 2012-08-08 | 广东白云国际科学研究院有限公司 | Electrolyte capable of removing nuclear pollution and movable cathode electrochemical cleaning device |
| CN102644080B (en) * | 2012-04-28 | 2013-06-12 | 杭州广荣科技有限公司 | Stripping liquid for sintering neodymium iron boron magnet chemical nickel plating layers |
| CN104018170A (en) * | 2014-05-29 | 2014-09-03 | 东风汽车紧固件有限公司 | Low-temperature environment-friendly chromium-free phosphating-film-removing agent |
| CN104762621B (en) * | 2015-04-30 | 2017-12-19 | 蓝思科技（长沙）有限公司 | A kind of remover for being used to etch film plating layer on film |
| CN106757089A (en) * | 2017-02-27 | 2017-05-31 | 广东省工业分析检测中心 | The cleaning fluid of stainless steel filter screen in a kind of Infrared Carbon-sulphur absorption apparatus |
| CN108863104B (en) * | 2017-05-10 | 2021-11-23 | 蓝思科技（长沙）有限公司 | Glass stripping agent and glass stripping process |
| CN110714218B (en) * | 2019-10-23 | 2021-07-06 | 湖州师范学院 | A method for preparing MXenes by electrochemical cation intercalation |
| CN111961544A (en) * | 2020-07-23 | 2020-11-20 | 湖北优尼科光电技术股份有限公司 | Film layer removing soaking solution applied to glass coating and application method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4886588A (en) * | 1989-04-10 | 1989-12-12 | Union Carbide Corporation | Electrolytic method of and bath for stripping coating from aluminum bases |
| TW591125B (en) * | 1998-02-13 | 2004-06-11 | Mitsubishi Heavy Ind Ltd | Method and apparatus for removing Ti-derived film |
| CN101358377A (en) * | 2008-09-10 | 2009-02-04 | 苏东艺 | Titanium carbide electrolytic stripping solution and processing technique thereof |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10237699A (en) * | 1997-02-24 | 1998-09-08 | Sumitomo Metal Mining Co Ltd | Method for removing titanium compound coating |
| US7390744B2 (en) * | 2004-01-29 | 2008-06-24 | Applied Materials, Inc. | Method and composition for polishing a substrate |
| US20060163083A1 (en) * | 2005-01-21 | 2006-07-27 | International Business Machines Corporation | Method and composition for electro-chemical-mechanical polishing |
-
2010
- 2010-04-20 CN CN201010151339.3A patent/CN102234835B/en not_active Expired - Fee Related
- 2010-12-21 US US12/974,208 patent/US20110253556A1/en not_active Abandoned
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4886588A (en) * | 1989-04-10 | 1989-12-12 | Union Carbide Corporation | Electrolytic method of and bath for stripping coating from aluminum bases |
| TW591125B (en) * | 1998-02-13 | 2004-06-11 | Mitsubishi Heavy Ind Ltd | Method and apparatus for removing Ti-derived film |
| CN101358377A (en) * | 2008-09-10 | 2009-02-04 | 苏东艺 | Titanium carbide electrolytic stripping solution and processing technique thereof |
Non-Patent Citations (1)
| Title |
|---|
| JP特开平10-237699 1998.09.08 |
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| CN102234835A (en) | 2011-11-09 |
| US20110253556A1 (en) | 2011-10-20 |
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