CN103233260A - Preparation of antifouling ceramic membrane electrolyte for titanium alloy surface and micro-arc oxidation method - Google Patents
Preparation of antifouling ceramic membrane electrolyte for titanium alloy surface and micro-arc oxidation method Download PDFInfo
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Abstract
The invention relates to preparation of antifouling ceramic membrane electrolyte for a titanium alloy surface and a micro-arc oxidation method and belongs to the field of metal material surface modification. The electrolyte contains sodium aluminate, sodium fluoride, potassium hydroxide, copper sulfate and a complexing agent. The preparation comprises the following operation steps of: (1) polishing the surface of a titanium alloy sample by polishing and carrying out oil removing; (2) preparing electrolyte, setting micro-arc oxidation technological parameters, connecting the sample with an anode and dipping the sample and the anode into the electrolyte together, and adopting a stainless steel electrolytic tank containing the electrolyte as a cathode; (3) switching on an alternating current pulse power supply to perform micro-arc oxidation treatment; and (4) washing the sample subjected to micro-arc oxidation treatment by deionized water, and then naturally drying. A titanium alloy surface ceramic membrane prepared by the method has the advantages that the microhardness is up to 900HV at most, the abrasive resistance of the titanium alloy surface ceramic membrane is about 3 times that of a titanium alloy substrate, the resistance to electrochemical corrosion of the titanium alloy surface ceramic membrane is superior to that of the titanium alloy substrate, and no marine organism is attached after six months immersion test in natural seawater in Qingdao.
Description
Technical field
The invention belongs to the metal surface properties modification technical field, be specifically related to the titanium alloy surface differential arc oxidation and handle, particularly relate to a kind of differential arc oxidation legal system and be equipped with the electrolytic solution of the anti-biological stained ceramic membrane of titanium alloy surface wear-and corrosion-resistant and concrete differential arc oxidation working method.
Background technology
For the most of equipment and the material that in ocean environment, use, owing to various microorganisms and marine organisms adhere to and breed and cause biodeterioration and microbiological corrosion, cause their use properties and life-span significantly to be reduced.Biodeterioration can increase the dynamic drag of tube wall and naval vessel shell, increases thermal resistance and the hydraulic pressure of heat exchanger, causes the obstruction of multihole devices such as strainer.Data shows that the microbial film that 0.1mm is thick will increase friction resistance more than 10%; The microorganism mucous membrane that 1mm is thick, its friction resistance increases by 80%, makes ship's speed reduce by 10%.In addition, microbial-induced corrosion phenomenon is also very serious, and only the corrosive nature of the hydrogen sulfide that produces because of sulphate reducing bacteria just makes production, transportation and the bunkerage of petroleum industry suffer the loss of multi-billion dollar every year.Up to now, unique effective measure of control biodeterioration and microbiological corrosion are to use sterilant, but because environmental issue, the use of chemical bactericide more and more is restricted.Therefore, anti-biological stained and measure microbiological corrosion of the effective compliance with environmental protection requirements of development of new is imperative.
Along with the fast development of marine oil probing with exploitation, the application of titanium alloy member such as titanium pump, valve, joint, fastening piece, anchor clamps and spare and accessory parts etc. is more and more, make oil drilling can enter darker waters and oil well, and adapt to higher temperature and the more serious production environment of corrosion.Also used titanium alloy in a large number on the external offshore oil exploration logging instrumentation shell.Although titanium alloy has excellent corrosion resistance nature, as marine oil equipment material, long service under ocean environment, titanium alloy and dissimilar metal surface come in contact the burn into wearing and tearing and biodeterioration is difficult to avoid.Therefore take measures titanium alloy surface is protected, improve its wear-and corrosion-resistant in the marine oil environment and prevent that the biodeterioration performance is very necessary.
The Chinese patent publication number is CN102409353A, open day is on April 11st, 2012, the applying date is on November 15th, 2011, invention and created name is " a kind of distributed titanium alloy pipeline electrolysis anti-soil apparatus ", the applicant is No.China Shipbuilding Industry Group Co.ltd. 725 Institute, a kind of distributed titanium alloy pipeline electrolysis anti-soil apparatus is disclosed in this application case, comprise direct supply, electrolytic anode, flange form negative electrode, cable, switching element and titanium alloy pipeline, produce chlorine and hypochlorite stain control agent by electrolytic seawater, reach antifouling purpose.Weak point is the device complexity, influences the production operation of marine oil equipment, does not also have the wear-and corrosion-resistant effect." developing material and application " magazine 2012 the 27th volume the 6th phase 48-53 page or leaf has been published the paper of " titanium alloy surface differential arc oxidation nano antifouling coating and performance study " that No.China Shipbuilding Industry Group Co.ltd. 725 Institute writes, mainly introduced a kind of differential arc oxidization technique that adopts and prepared the method for nano antifouling ceramic coating at the Ti-6Al-3Nb-2Zr alloy surface, its electrolytic solution is by phosphoric acid salt, stain control agent and deionized water mixed preparing.But do not mention concrete composition and the proportioning of electrolytic solution in the literary composition, do not provide the concrete processing parameter that differential arc oxidation is handled yet.
Differential arc oxidation is a kind of new technology at valve metals such as Mg, Al, Ti and alloy surface growth in situ membrane of oxide ceramics thereof.Adopt differential arc oxidization technique to generate one deck ceramic insulating layer in the titanium alloy surface original position, significantly improve solidity to corrosion, wear resistance and the insulativity of titanium alloy.If contain anti-biological stained element in the electrolytic solution, anti-biological stained element also can be participated in reaction in the differential arc oxidation process, and the ceramic membrane of generation also can have anti-biological stained function.Red copper oxide is to use one of anti-biological stained dose with the longest history.Red copper oxide can take place to decompose in seawater to produce cupric ion, lose activity or directly make biological cell protein be transformed into the metalloprotein throw out and be dissolved in apoenzyme that the cupric ion in the seawater can make biology depend on for existence, biological tissue is changed and dead.Red copper oxide has advantages such as safe, inexpensive as anti-biological stained dose, is bringing into play important effect in the development process of whole anti-biological stained coating.
The present invention develops a kind of employing differential arc oxidation legal system and is equipped with the anti-biological stained ceramic membrane electrolytic solution of titanium alloy surface wear-and corrosion-resistant, and by a series of simple operation processes the antifouling effect of Red copper oxide and the wear resistance and corrosion resistance of titanium alloy ceramic coating formed by micro-arc oxidation are combined, preparation has the multifunction surface ceramic membrane of wear-and corrosion-resistant and anti-marine biofouling simultaneously.Its technological process is simple, and cost is low, and is practical, is fit to suitability for industrialized production.
Summary of the invention
The technical problem to be solved in the present invention is to overcome titanium alloy easily to come in contact the easy to wear and easy problems such as generation marine biofouling and biological corrosion of burn into dissimilar metal in the abominable Service Environment in ocean, provides a kind of differential arc oxidation legal system that adopts to be equipped with the electrolytic solution of the anti-biological stained ceramic membrane of titanium alloy surface wear-and corrosion-resistant and concrete differential arc oxidation working method.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
The differential arc oxidation legal system is equipped with in the anti-biological stained ceramic membrane electrolytic solution of titanium alloy surface wear-and corrosion-resistant and comprises: sodium aluminate, Sodium Fluoride, potassium hydroxide, copper sulfate and complexing agent.By quality and cumulative volume ratio, the concentration of sodium aluminate, Sodium Fluoride and potassium hydroxide is 1-10g/L in the electrolytic solution, and the concentration of cupric sulfate pentahydrate is 0.5-5g/L.Complexing agent is one or both of sodium ethylene diamine tetracetate, ammoniacal liquor in the electrolytic solution, and by quality and cumulative volume ratio, two water sodium ethylene diamine tetracetate concentration are 0.5-5g/L, and ammonia concn is 0-60mL/L.
The technical process of adopting this electrolytic solution to handle the titanium alloy specimen surface is:
(1) adopt the 100-1500# carborundum paper that Ti6Al4V titanium alloy specimen surface is carried out grinding process, make titanium alloy surface smooth, clean titanium alloy sample after the polishing with acetone soln then, with deionized water the titanium alloy specimen surface is rinsed well at last and dried up standby with blower.
(2) by the concentration of electrolyte requirement, with pharmaceutical chemicals and deionized water preparation differential arc oxidation electrolytic solution.
(3) will immerse in the electrolytic solution of step (2) configuration through the titanium alloy sample after step (1) processing, the titanium alloy sample is linked to each other with power anode, the stainless steel electrolytic groove is linked to each other with power cathode.Adopt current constant mode, the micro-arc oxidation process parameter area is: current density 1-10A/dm
2, frequency 100-800Hz, dutycycle 10%-50%, reaction times 0.5-2 hour.After differential arc oxidation was handled, powered-down took out the titanium alloy sample from electrolytic solution, rinse well with deionized water, dries naturally in air.
Through above processing, can obtain the ceramic membrane that one deck has the anti-biological stained function of wear-and corrosion-resistant at the titanium alloy specimen surface.
Compared with prior art the invention has the beneficial effects as follows:
1. adopt electrolytic solution provided by the invention and differential arc oxidation method to generate the anti-biological stained ceramic membrane of one deck wear-and corrosion-resistant in the titanium alloy surface original position, need not add the coating that other device or outer planting contain toxin and just can reach the purpose of preventing marine biofouling;
2. owing to contain cupric ion in electrolytic solution, after the differential arc oxidation reaction, also contain copper in the ceramic membrane that titanium alloy surface generates, its existence form is Cu
2O.Because cupric ion is inhibited to adhering to of microorganism, can not cause again ocean environment and marine organisms simultaneously and seriously influence, therefore the inexpensive practicality of this ceramic membrane, good antifouling effect, the lacing film experiment did not have marine organisms to adhere to after 6 months in the natural sea-water of Qingdao;
3. adopt electrolytic solution provided by the invention and differential arc oxidation method at the ceramic membrane of titanium alloy surface preparation, microhardness reaches as high as more than the 900HV, is about 3 times of titanium alloy substrate; Wear resistance is about 3 times of titanium alloy substrate; The electrochemical corrosion resistant performance obviously is better than the titanium alloy sample without the differential arc oxidation processing.
4. the cupric ceramic membrane that obtains of the present invention has the characteristic that continues slow copper ion releasing, can be used for the bottom of titanium alloy surface such as boats and ships or offshore oil production platform, prevents that marine organisms from adhering to and breed, reduces seawater resistance and friction, the reduction energy consumption.Also can be used for simultaneously other offshore engineering structure or equipment surface, prevent that marine organisms from adhering to the material corrosion that causes and destroying or line clogging, assurance equipment normally moves, and improves the safe reliability of structure.At marine oil equipment and the field of making, naval vessel good prospects for application is arranged.
5. the used pharmaceutical chemicals of electrolytic solution of the present invention is cheap and easy to get, and described differential arc oxidation method is simple to operate, is not subjected to the restriction of titanium alloy-based shape, is suitable for suitability for industrialized production;
6. the method for the invention not only can be used for the Ti6Al4V alloy, also extends to valve metal materials such as other titanium alloys, aluminium alloy, magnesium alloy.
Description of drawings
Fig. 1 is the anti-fouling ceramic coating formed by micro-arc oxidation of titanium alloy surface lacing film experiment sample photo after 6 months in the natural sea-water of Qingdao.
Fig. 2 is the polarization curve contrast before and after the titanium alloy surface differential arc oxidation is handled.
Fig. 3 is the SEM photo of titanium alloy surface differential arc oxidation brown ceramic membrane.
Fig. 4 is the SEM photo of titanium alloy surface differential arc oxidation black ceramic membrane.
Specific embodiment
Below in conjunction with accompanying drawing the present invention is elaborated:
The objective of the invention is to overcome titanium alloy and in the abominable Service Environment in ocean, easily come in contact the easy to wear and easy problems such as generation marine biofouling and biological corrosion of burn into dissimilar metal, provide a kind of differential arc oxidation legal system that adopts to be equipped with the electrolytic solution of the anti-biological stained ceramic membrane of titanium alloy surface wear-and corrosion-resistant and concrete differential arc oxidation working method.
For achieving the above object, the present invention is research object with the titanium alloy ti6al4v, with electrolytic solution of the present invention titanium alloy surface is carried out differential arc oxidation and handles, and generates the anti-biological stained ceramic membrane of wear-and corrosion-resistant.
Specific embodiment one: (1) adopts carborundum paper to be polished in Ti6Al4V alloy sample surface, and sand paper is followed successively by 320#, 600#, 800#, 1200# and 1500# from coarse to fine.In ultrasonic washing instrument, specimen surface was cleaned oil removing 15 minutes with acetone soln then, rinse well with deionized water, dry up with blower.(2) take by weighing certain amount of medicine and put into electrolyzer, add small amount of deionized water and stir and make the medicine dissolving, and then add deionized water until electrolyte dilution to prescribed concentration.By quality and cumulative volume ratio, chemical concentration is respectively: sodium aluminate 10g/L, Sodium Fluoride 5g/L, potassium hydroxide 5g/L, cupric sulfate pentahydrate 0.5-2.5g/L, two water sodium ethylene diamine tetracetate 0-3g/L, ammoniacal liquor 0-50ml/L.(3) the titanium alloy sample is linked to each other with power anode immerse in the electrolytic solution, the stainless steel electrolytic groove is linked to each other with power cathode.Adopt constant current mode, it is 8.2A/dm that the differential arc oxidation current density is set
2, frequency is that 600Hz, dutycycle are 40%, oxidization time is 2 hours.Power-on is carried out the differential arc oxidation processing then.Reaction finishes the back and takes out sample, rinses well with deionized water, dries naturally.Through above processing, specimen surface just generates the ceramic membrane that one deck contains copper, thereby has had the function that prevents marine biofouling, and the lacing film experiment did not have marine organisms to adhere to (Fig. 1) after 6 months in the natural sea-water of Qingdao.The ceramic membrane microhardness is up to 900HV, is about 3 times of titanium alloy substrate.The ceramic membrane wear resistance is about 3 times of titanium alloy substrate.Ceramic membrane electrochemical corrosion resistant performance obviously is better than the titanium alloy sample (Fig. 2) without the differential arc oxidation processing.
Specific embodiment two: what present embodiment and specific embodiment one were different is that the concentration of cupric sulfate pentahydrate is 0.75-1.75g/L in the step (2), and the concentration of two water sodium ethylene diamine tetracetates is 1-2.33g/L, and the concentration of ammoniacal liquor is 0.Other is identical with specific embodiment one.
Specific embodiment three: what present embodiment and specific embodiment one were different is that the concentration of cupric sulfate pentahydrate is 0.5g/L in the step (2), and the concentration of two water sodium ethylene diamine tetracetates is 0.67g/L, and the concentration of ammoniacal liquor is 0.Other is identical with specific embodiment one.
Specific embodiment four: what present embodiment and specific embodiment one were different is that the concentration of cupric sulfate pentahydrate is 2g/L in the step (2), and the concentration of two water sodium ethylene diamine tetracetates is 2.67g/L, and the concentration of ammoniacal liquor is 0.Other is identical with specific embodiment one.
Specific embodiment five: what present embodiment and specific embodiment one were different is that the concentration of cupric sulfate pentahydrate is 0.75g/L in the step (2), and the concentration of two water sodium ethylene diamine tetracetates is 1g/L, and the concentration of ammoniacal liquor is 0.Other is identical with specific embodiment one.
Specific embodiment six: what present embodiment and specific embodiment one were different is that the concentration of cupric sulfate pentahydrate is 1g/L in the step (2), and the concentration of two water sodium ethylene diamine tetracetates is 1.33g/L, and the concentration of ammoniacal liquor is 0.Other is identical with specific embodiment one.
Specific embodiment seven: what present embodiment and specific embodiment one were different is that the concentration of cupric sulfate pentahydrate is 1.25g/L in the step (2), and the concentration of two water sodium ethylene diamine tetracetates is 1.67g/L, and the concentration of ammoniacal liquor is 0.Other is identical with specific embodiment one.
Specific embodiment eight: what present embodiment and specific embodiment one were different is that the concentration of cupric sulfate pentahydrate is 1.5g/L in the step (2), and the concentration of two water sodium ethylene diamine tetracetates is 2g/L, and the concentration of ammoniacal liquor is 0.Other is identical with specific embodiment one.
Specific embodiment nine: what present embodiment and specific embodiment one were different is that the concentration of cupric sulfate pentahydrate is 1.75g/L in the step (2), and the concentration of two water sodium ethylene diamine tetracetates is 2.33g/L, and the concentration of ammoniacal liquor is 0.Other is identical with specific embodiment one.
The ceramic coating formed by micro-arc oxidation surface that specific embodiment two to specific embodiment nine is prepared is brown, and by scanning electron microscopic observation, ceramic membrane surface is the vesicular structure (Fig. 3) that the micropore by a large amount of craters pattern constitutes.
Specific embodiment ten: what present embodiment and specific embodiment one were different is that the concentration of cupric sulfate pentahydrate is 0.5g/L in the step (2), and the concentration of two water sodium ethylene diamine tetracetates is 0g/L, and the concentration of ammoniacal liquor is 10mL/L.Other is identical with specific embodiment one.
Specific embodiment 11: what present embodiment and specific embodiment one were different is that the concentration of cupric sulfate pentahydrate is 2.5g/L in the step (2), and the concentration of two water sodium ethylene diamine tetracetates is 0g/L, and the concentration of ammoniacal liquor is 50mL/L.Other is identical with specific embodiment one.
Specific embodiment 12: what present embodiment and specific embodiment one were different is that the concentration of cupric sulfate pentahydrate is 1g/L in the step (2), and the concentration of two water sodium ethylene diamine tetracetates is 0g/L, and the concentration of ammoniacal liquor is 20mL/L.Other is identical with specific embodiment one.
Specific embodiment 13: what present embodiment and specific embodiment one were different is that the concentration of cupric sulfate pentahydrate is 1.5g/L in the step (2), and the concentration of two water sodium ethylene diamine tetracetates is 0g/L, and the concentration of ammoniacal liquor is 30mL/L.Other is identical with specific embodiment one.
Specific embodiment 14: what present embodiment and specific embodiment one were different is that the concentration of cupric sulfate pentahydrate is 2g/L in the step (2), and the concentration of two water sodium ethylene diamine tetracetates is 0g/L, and the concentration of ammoniacal liquor is 40mL/L.Other is identical with specific embodiment one.
The ceramic coating formed by micro-arc oxidation surface that specific embodiment ten to specific embodiment 14 is prepared is black, pass through scanning electron microscopic observation, ceramic membrane surface is similar to the surface topography of the ceramic membrane of specific embodiment nine preparations to specific embodiment two, also be the vesicular structure that the micropore by a large amount of craters pattern constitutes, but pore size obviously reduce (Fig. 4).
Claims (5)
1. a differential arc oxidation legal system is equipped with the anti-biological stained ceramic membrane electrolytic solution of titanium alloy surface, it is characterized in that comprising sodium aluminate, Sodium Fluoride, potassium hydroxide, copper sulfate and complexing agent.
2. according to the described electrolytic solution of claim 1, it is characterized in that chemical concentration is: the concentration of sodium aluminate, Sodium Fluoride and potassium hydroxide is 1-10g/L by quality and cumulative volume ratio, the concentration of cupric sulfate pentahydrate is 0.5-5g/L.
3. according to the described electrolytic solution of claim 1, it is characterized in that complexing agent is one or both of sodium ethylene diamine tetracetate, ammoniacal liquor.Wherein, by quality and cumulative volume ratio, two water sodium ethylene diamine tetracetate concentration are 0.5-5g/L, and ammonia concn is 0-60mL/L.
4. differential arc oxidation method for preparing the anti-biological stained ceramic membrane of titanium alloy surface is characterized in that operating according to the following steps: (1) with the titanium alloy specimen surface polish, oil removal treatment; (2) preparation electrolytic solution is set the micro-arc oxidation process parameter, sample is linked to each other with anode and immerses in the electrolytic solution, and the stainless steel electrolytic groove that holds electrolytic solution is done negative electrode; (3) open the alternating-current pulse power supply and carry out the differential arc oxidation processing; (4) sample after the differential arc oxidation processing is also dried naturally with deionized water rinsing.
5. method according to claim 4 is characterized in that the microarc oxidation treatment process parameter is: adopt the constant current mode differential arc oxidization technique, current density 1-10A/dm
2, frequency 100-800Hz, dutycycle 10%-50%, oxidization time 0.5-2 hour.
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| CN107099712A (en) * | 2017-05-26 | 2017-08-29 | 中国石油大学(华东) | A kind of solvable composite material of magnesium alloy pressure break ball and preparation method thereof |
| CN109183110A (en) * | 2018-11-27 | 2019-01-11 | 中国科学院海洋研究所 | A kind of micro-arc oxidation preparation antifouling Integrative Coating of aluminium alloy surface anti-corrosion and preparation method thereof |
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| CN109537022A (en) * | 2019-01-15 | 2019-03-29 | 中国特种飞行器研究所 | Large-scale titanium alloy structure differential arc oxidation and verification method based on scanning cathode |
| CN110952124A (en) * | 2018-09-27 | 2020-04-03 | 中国科学院宁波材料技术与工程研究所 | Antifouling titanium alloy material based on bionic super-smooth surface, and preparation method and application thereof |
| CN113235145A (en) * | 2021-04-29 | 2021-08-10 | 上海交通大学 | Method for preparing 'amorphous outer-polycrystalline inner' double-film antibacterial coating on surface of titanium alloy |
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| CN106676606A (en) * | 2016-11-21 | 2017-05-17 | 广西大学 | Method for preparing ceramic oxidation films in different colors on surface of titanium alloy |
| CN106676606B (en) * | 2016-11-21 | 2019-03-01 | 广西大学 | The method that titanium alloy surface prepares different colours ceramic coating |
| CN107099712A (en) * | 2017-05-26 | 2017-08-29 | 中国石油大学(华东) | A kind of solvable composite material of magnesium alloy pressure break ball and preparation method thereof |
| CN107099712B (en) * | 2017-05-26 | 2019-01-04 | 中国石油大学(华东) | A kind of solvable composite material of magnesium alloy pressure break ball and preparation method thereof |
| CN110952124A (en) * | 2018-09-27 | 2020-04-03 | 中国科学院宁波材料技术与工程研究所 | Antifouling titanium alloy material based on bionic super-smooth surface, and preparation method and application thereof |
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| CN109183110A (en) * | 2018-11-27 | 2019-01-11 | 中国科学院海洋研究所 | A kind of micro-arc oxidation preparation antifouling Integrative Coating of aluminium alloy surface anti-corrosion and preparation method thereof |
| CN109537022A (en) * | 2019-01-15 | 2019-03-29 | 中国特种飞行器研究所 | Large-scale titanium alloy structure differential arc oxidation and verification method based on scanning cathode |
| CN113235145A (en) * | 2021-04-29 | 2021-08-10 | 上海交通大学 | Method for preparing 'amorphous outer-polycrystalline inner' double-film antibacterial coating on surface of titanium alloy |
| CN116288347A (en) * | 2023-03-01 | 2023-06-23 | 纳狮新材料有限公司杭州分公司 | Method for reducing corrosive wear and marine environment surface corrosion wear resistant fluorocarbon base film |
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