CN106637353B - A kind of stainless steel watch surface passivation treatment fluid and deactivating process for the treatment of - Google Patents

A kind of stainless steel watch surface passivation treatment fluid and deactivating process for the treatment of Download PDF

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CN106637353B
CN106637353B CN201611012977.0A CN201611012977A CN106637353B CN 106637353 B CN106637353 B CN 106637353B CN 201611012977 A CN201611012977 A CN 201611012977A CN 106637353 B CN106637353 B CN 106637353B
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stainless steel
electrode
treatment
treatment liquid
working electrode
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CN106637353A (en
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林志峰
李相波
许立坤
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725th Research Institute of CSIC
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725th Research Institute of CSIC
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/34Anodisation of metals or alloys not provided for in groups C25D11/04 - C25D11/32

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  • Chemical Kinetics & Catalysis (AREA)
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  • Chemical Treatment Of Metals (AREA)
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Abstract

The present invention provides a kind of stainless steel watch surface passivation treatment fluid and deactivating process for the treatment of, belongs to field of metal material surface treatment.The inactivating treatment liquid includes rare earth metal salt, silicate and oxidant, and rare earth metal salt is cerous sulfate, and silicate is sodium metasilicate, and oxidant is potassium permanganate, and above-mentioned substance is added in a certain amount of distilled water, is stirred well to solid matter and all dissolves.The present invention places it in inactivating treatment liquid using stainless steel as working electrode, forms three-electrode system with reference electrode and to electrode, carries out anodic oxidation to working electrode, forms passivation film in stainless steel surface, realizes the Passivation Treatment to stainless steel surface.Inactivating treatment liquid of the invention is without the strong corrosives such as Cr VI and sulfuric acid, nitric acid or hydrochloric acid acid, preparation process is simple, it is low in cost, favorable reproducibility and be not necessarily to Large expensive equipment, prepared passivation film can apply to the fields such as surface of stainless steel product processing, the corrosion resistance for significantly improving stainless steel, prolongs its service life.

Description

A kind of stainless steel watch surface passivation treatment fluid and deactivating process for the treatment of
Technical field
It can be somebody's turn to do in the inactivating treatment liquid and processing method of stainless steel surface preparation Corrosion Resistant Film the invention discloses a kind of Treatment fluid and method are suitable for stainless steel watch surface treatment, belong to technical field of metal material surface treatment.
Background technique
Metal erosion brings massive losses to national economy every year.Common metal erosion means of defence includes that corrosion resistant is made Lose alloy and coating etc..The common element to prepare alloy includes nickel (Ni), chromium (Cr), silicon (Si), molybdenum (Mo) etc..It is stainless Steel is the stronger steel material of common corrosion resistance, is made of the elements such as iron and nickel, chromium.Stainless steel have unique intensity, Higher wearability, superior antiseptic property and being not easy such as gets rusty at the excellent characteristic.Thus it is widely used in chemical industry, foods machine The fields such as tool, electromechanics.
Stainless steel has good corrosion resisting property in normal atmospheric conditions, this is because its surface have one layer it is fine and close Passivating film.When stainless steel is applied in the stronger environment of the corrosivity such as marine environment, the stronger ion of corrosivity such as chlorine from Son etc. can destroy the passivating film on its surface, so as to cause the corrosion of stainless steel.Surface treatment is that raising stainless steel is corrosion proof Main method, while being also removal surface contaminants, improve the main method of aesthetic measure, mainly includes chemical method and electrochemistry Method.Chemical method is to be dipped into stainless steel sample in the solution containing chemical reagent to carry out the processing regular hour, passing through reagent In substance and steel react and generate passivating film.Mostly containing the strong pollution object of the strong acid and chromic acid etc. such as nitric acid, hydrochloric acid in reagent Matter causes certain threat to environment if dealt with improperly.Treatment fluid used in electrochemical process equally has certain pollution Property, as contained in a kind for the treatment of fluid reported in the literature: 5 g/L of chromic anhydride, 20 g/L of ammonium molybdate, 30 g/L of ammonium sulfate, boric acid 15 g/L, 0.3~0.4 A/dm of anodic current density2, 15~20 DEG C of temperature, 15~20 min of time.This traditional nitre Acid and chromic acid passivation, acid solution are harmful to the human body and pollute environment.Therefore, the small stainless steel treatment fluid of exploitation green, pollution It is imperative.
Researcher has been developed for the treatment process of some environment-friendly types at present, such as uses 130~150 g/ of sodium metavanadate L, the treatment fluid of 1100~1200 g/L of sulfuric acid, 24 % of vanadate, treatment fluid of 42 % of sulfuric acid etc..These treatment fluids contain more The strong acid such as the sulfuric acid of high concentration still have no small pressure to subsequent wastewater treatment.
Summary of the invention
The present invention provides a kind of environmental type not on the basis of fully understanding domestic and international method for treating stainless steel surfaces Become rusty steel surface inactivating treatment liquid and deactivating process for the treatment of, and the processing method is based on inactivating treatment liquid of the invention, in anode current Under the action of, the metallic element of stainless steel surface loses electronics, and the rare earth ion and silicate ion in solution exist It is reacted in Jacquet diffusion layer with metal ion, generates the silicate compound containing the metallic elements such as rare earth element and iron, and sink Product arrives stainless steel surface, one layer of strong film of corrosion resistance is formed, to improve the corrosion resisting property of stainless steel.
The technical solution adopted by the present invention to solve the technical problems is:
1, the present invention provides a kind of stainless steel watch surface passivation treatment fluid, including rare earth metal salt, silicate and oxidant, In, rare earth metal salt is cerous sulfate, and silicate is sodium metasilicate, and oxidant is potassium permanganate, above-mentioned substance is added to a certain amount of Distilled water in, be stirred well to solid matter all dissolve.
Specifically, including: cerous sulfate 0.05-0.1 mol, sodium metasilicate 0.002-0.005 in every liter of inactivating treatment liquid Mol, potassium permanganate 5-15 g.
2, the present invention separately provides a kind of stainless steel surface deactivating process for the treatment of, and this method is using stainless steel as three-electrode system In working electrode, working electrode is placed in above-mentioned inactivating treatment liquid, with reference electrode and to electrode composition be conducted three Electrode system carries out anodic oxidation to working electrode under constant current density, forms passivation film in stainless steel surface.
Specifically, this method comprises the following steps:
1) it the configuration of inactivating treatment liquid: according to the composition of inactivating treatment liquid, is configured according to the proportion;
2) preparation of working electrode: using stainless steel substrates as basis material, basis material being encapsulated, and is reserved suitably Work area;
3) the anodic passivity processing of working electrode: working electrode is placed in the configured inactivating treatment liquid of step 1), with Reference electrode and the three-electrode system being conducted to electrode composition, control current density are 50-100 mAcm-2, sedimentation time For 5-15 min, inactivating treatment liquid temperature is 70-80oC;
The content, current density of each component, sedimentation time and temperature parameter are according to required passivation film in inactivating treatment liquid Thickness, hardness, corrosion resistance select in given range.
Specifically, this method further include: before working electrode is placed in the configured inactivating treatment liquid of step 1), to work Electrode is pre-processed.
Specifically, to working electrode carry out pretreatment refer to SiC sand paper polish, then successively with acetone, ethyl alcohol, go from It is spare after sub- water ultrasonic cleaning is clean.
Specifically, the inactivating treatment liquid carries out temperature control using water bath with thermostatic control.
Specifically, described is platinum niobium silk electrode to electrode.
Specifically, the reference electrode is saturated calomel electrode.
Of the invention a kind of stainless steel watch surface passivation treatment fluid and deactivating process for the treatment of, compared with prior art caused by Beneficial effect is:
Inactivating treatment liquid of the invention is without the strong corrosives such as Cr VI and sulfuric acid, nitric acid or hydrochloric acid acid, preparation process letter It is single, it is low in cost, facilitate operation, favorable reproducibility and without Large expensive equipment.Prepared passivation film is expected to be applied to not The fields such as rust steel part surface treatment.Stainless steel is surface-treated using inactivating treatment liquid of the invention, can obviously be mentioned The corrosion resistance of high stainless steel, prolongs its service life.
Specific embodiment
With reference to embodiment, to a kind of stainless steel watch surface passivation treatment fluid of the invention and deactivating process for the treatment of It is described in detail below.
Embodiment one
A kind of stainless steel watch surface passivation treatment fluid of the invention, comprising: rare earth metal salt, silicate and oxidant, wherein Rare earth metal salt is cerous sulfate, and silicate is sodium metasilicate, and oxidant is potassium permanganate, and above-mentioned substance is added to a certain amount of steaming In distilled water, it is stirred well to solid matter and all dissolves.
Inactivating treatment liquid concrete composition is as shown in table 1.
1 inactivating treatment liquid of table composition
Cerous sulfate Sodium metasilicate Potassium permanganate
0.05 mol·L-1 0.004 mol·L-1 10 g·L-1
A kind of stainless steel surface deactivating process for the treatment of, this method using stainless steel as three-electrode system in working electrode, Working electrode is placed in above-mentioned inactivating treatment liquid, it is right with reference electrode and the three-electrode system being conducted to electrode composition Working electrode carries out anodic oxidation under constant current density, forms passivation film in stainless steel surface.This method specifically includes Following steps:
1) it the configuration of inactivating treatment liquid: according to the composition of inactivating treatment liquid, is configured according to the proportion;
2) preparation and pretreatment of working electrode: using stainless steel substrates as basis material, by basis material sealant sealing Dress, and the square that work area is 10 mm of side length is reserved, working electrode is polished with 600 mesh SiC sand paper, is then successively used It is spare after acetone, ethyl alcohol, 5 min of deionized water ultrasonic cleaning.
3) the anodic passivity processing of working electrode: working electrode is placed in the configured inactivating treatment liquid of step 1), with Platinum niobium silk electrode is to electrode, and saturated calomel electrode is reference electrode, and control current density is 50 mAcm-2, sedimentation time is 15 min, inactivating treatment liquid temperature are 70oC;Inactivating treatment liquid carries out temperature control using water bath with thermostatic control.
Embodiment two
A kind of stainless steel watch surface passivation treatment fluid of the invention, comprising: rare earth metal salt, silicate and oxidant, wherein Rare earth metal salt is cerous sulfate, and silicate is sodium metasilicate, and oxidant is potassium permanganate, and above-mentioned substance is added to a certain amount of steaming In distilled water, it is stirred well to solid matter and all dissolves.
Inactivating treatment liquid concrete composition is as shown in table 2.
2 inactivating treatment liquid of table composition
Cerous sulfate Sodium metasilicate Potassium permanganate
0.08 mol·L-1 0.002 mol·L-1 15 g·L-1
A kind of stainless steel surface deactivating process for the treatment of, this method using stainless steel as three-electrode system in working electrode, Working electrode is placed in inactivating treatment liquid of any of claims 1 or 2, forms three to be conducted with reference electrode and to electrode Electrode system carries out anodic oxidation to working electrode under constant current density, forms passivation film in stainless steel surface.The party Method specifically comprises the following steps:
1) it the configuration of inactivating treatment liquid: according to the composition of inactivating treatment liquid, is configured according to the proportion;
2) preparation and pretreatment of working electrode: using stainless steel substrates as basis material, by basis material sealant sealing Dress, and reserve the circle that work area is 10 mm of φ, working electrode polishes with 800 mesh SiC sand paper, then successively use acetone, It is spare after ethyl alcohol, 10 min of deionized water ultrasonic cleaning.
3) the anodic passivity processing of working electrode: working electrode is placed in the configured inactivating treatment liquid of step 1), with Platinum niobium silk electrode is to electrode, and saturated calomel electrode is reference electrode, and control current density is 100 mAcm-2, sedimentation time For 5 min, inactivating treatment liquid temperature is 80oC;Inactivating treatment liquid carries out temperature control using water bath with thermostatic control.
Embodiment three
A kind of stainless steel watch surface passivation treatment fluid of the invention, comprising: rare earth metal salt, silicate and oxidant, wherein Rare earth metal salt is cerous sulfate, and silicate is sodium metasilicate, and oxidant is potassium permanganate, and above-mentioned substance is added to a certain amount of steaming In distilled water, it is stirred well to solid matter and all dissolves.
Inactivating treatment liquid concrete composition is as shown in table 3.
3 inactivating treatment liquid of table composition
Cerous sulfate Sodium metasilicate Potassium permanganate
0.1 mol·L-1 0.005 mol·L-1 5 g·L-1
A kind of stainless steel surface deactivating process for the treatment of, this method using stainless steel as three-electrode system in working electrode, Working electrode is placed in inactivating treatment liquid of any of claims 1 or 2, forms three to be conducted with reference electrode and to electrode Electrode system carries out anodic oxidation to working electrode under constant current density, forms passivation film in stainless steel surface.The party Method specifically comprises the following steps:
1) it the configuration of inactivating treatment liquid: according to the composition of inactivating treatment liquid, is configured according to the proportion;
2) preparation and pretreatment of working electrode: using stainless steel substrates as basis material, by basis material sealant sealing Dress, and the square that work area is 10 mm of side length is reserved, working electrode is polished with 1200 mesh SiC sand paper, is then successively used It is spare after acetone, ethyl alcohol, 8 min of deionized water ultrasonic cleaning.
3) the anodic passivity processing of working electrode: working electrode is placed in the configured inactivating treatment liquid of step 1), with Platinum niobium silk electrode is to electrode, and saturated calomel electrode is reference electrode, and control current density is 80 mAcm-2, sedimentation time is 10 min, inactivating treatment liquid temperature are 75oC;Inactivating treatment liquid carries out temperature control using water bath with thermostatic control.
It is noted that the present invention is not limited to the above embodiments, any person skilled in the art is based on this hair Bright technical solution both falls within protection model of the invention to any simple modification, equivalent change and modification made by above-described embodiment In enclosing.

Claims (8)

1. a kind of stainless steel surface deactivating process for the treatment of, which is characterized in that this method using stainless steel as three-electrode system in Working electrode is placed in inactivating treatment liquid by working electrode, forms the three-electrode system that is conducted with reference electrode and to electrode, Anodic oxidation is carried out under constant current density to working electrode, forms passivation film in stainless steel surface;
Wherein inactivating treatment liquid includes: rare earth metal salt, silicate and oxidant, wherein rare earth metal salt is cerous sulfate, silicic acid Salt is sodium metasilicate, and oxidant is potassium permanganate, and above-mentioned substance is added in a certain amount of distilled water, solids is stirred well to Matter all dissolves.
2. a kind of stainless steel surface deactivating process for the treatment of according to claim 1, which is characterized in that at every liter of passivation Managing in liquid includes: cerous sulfate 0.05-0.1 mol, sodium metasilicate 0.002-0.005 mol, potassium permanganate 5-15 g.
3. a kind of stainless steel surface deactivating process for the treatment of according to claim 1 or 2, which is characterized in that this method includes Following steps:
1) it the configuration of inactivating treatment liquid: according to the composition of inactivating treatment liquid, is configured according to the proportion;
2) preparation of working electrode: using stainless steel substrates as basis material, basis material being encapsulated, and reserves suitable work Area;
3) the anodic passivity processing of working electrode: working electrode is placed in the configured inactivating treatment liquid of step 1), with reference Electrode and the three-electrode system being conducted to electrode composition, control current density are 50-100 mAcm-2, sedimentation time is 5-15 min, inactivating treatment liquid temperature are 70-80oC;
In inactivating treatment liquid the content, current density of each component, sedimentation time and temperature parameter according to required passivation film thickness, Hardness, corrosion resistance select in given range.
4. a kind of stainless steel surface deactivating process for the treatment of according to claim 1 or 2, which is characterized in that this method is also wrapped It includes: before working electrode is placed in the configured inactivating treatment liquid of step 1), working electrode being pre-processed.
5. a kind of stainless steel surface deactivating process for the treatment of according to claim 4, which is characterized in that carried out to working electrode Pretreatment refers to is polished with SiC sand paper, then successively with spare after acetone, ethyl alcohol, deionized water ultrasonic cleaning completely.
6. a kind of stainless steel surface deactivating process for the treatment of described according to claim 1 or 2 or 5, which is characterized in that the passivation Treatment fluid carries out temperature control using water bath with thermostatic control.
7. a kind of stainless steel surface deactivating process for the treatment of described according to claim 1 or 2 or 5, which is characterized in that described to electricity Extremely platinum niobium silk electrode.
8. a kind of stainless steel surface deactivating process for the treatment of described according to claim 1 or 2 or 5, which is characterized in that the reference Electrode is saturated calomel electrode.
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