CN101634043B - Aqueous solution of electrolyte and surface treatment method for zirconium and zirconium alloy - Google Patents
Aqueous solution of electrolyte and surface treatment method for zirconium and zirconium alloy Download PDFInfo
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Abstract
The invention provides aqueous solution of electrolyte, which contains hydroxide, silicate and borate. The invention also provides a surface treatment method for zirconium and a zirconium alloy. By the method, an oxidation film is formed on the surface of the zirconium or the zirconium alloy, so the corrosion resistance and abrasive resistance of the zirconium or the zirconium alloy can be greatly improved. Besides, after a loose layer on the surface layer of the oxidation film is removed, the hardness and scratch resistance of the oxidation film can be further improved.
Description
Technical field
The present invention relates to the surface treatment method of a kind of aqueous electrolyte liquid and zirconium and zirconium alloy.
Background technology
The content of zirconium in the earth's crust is quite big, and is all bigger than general metallic zinc commonly used, copper, tin etc., is light grey.Density is 6.49g/cm
3, fusing point is 1852 ± 2 ℃, boiling point is 4377 ℃, valency is+2 ,+3 and+4.Be that matrix adds other element and can constitute zirconium alloy with the zirconium, described other element for example can be tin, niobium, iron etc.Zirconium alloy has moderate mechanical property, lower atonic heat capacity neutron-absorption cross-section, and nuclear fuel is had good consistency, how as the core structural material of water cooled nuclear reactor.And zirconium alloy plasticity is good, can make tubing, sheet material, bar and silk material by plastic working; Its weldability can be in order to carry out welding processing.
In addition, zirconium and zirconium alloy have enough obdurabilities and biocompatibility, and elasticity volume is lower than alloys such as titanium alloy, cobalt chrome molybdenum.Therefore zirconium alloy also has been widely used at tooth implant and bone implant field.But zirconium and zirconium alloy are perishable at normal temperatures, wear resistance and scratch resistance are relatively poor, therefore, have limitation in the application in some field.
For performances such as corrosion-resistant, the wear resistance that improves zirconium and zirconium alloy and scratch resistance, be well known that at present by zirconium or zirconium alloy are carried out the method that anodic oxidation forms oxide film in sodium hydroxide solution, sodium silicate solution or sodium radio-phosphate,P-32 solution.But it is still relatively poor that aforesaid method is handled corrosion-resistant, the wear resistance and the scratch resistance of the zirconium obtain and zirconium alloy.Therefore, erosion resistance, wear resistance and the scratch resistance of raising zirconium and zirconium alloy are significant for zirconium and the further widespread use of zirconium alloy in industry.
Summary of the invention
The objective of the invention is in order to overcome the shortcoming of the corrosion-resistant of zirconium and zirconium alloy in the prior art, a kind of electrolyte solution of the erosion resistance that can improve zirconium and zirconium alloy and the surface treatment method of zirconium and zirconium alloy are provided.
The invention provides a kind of aqueous electrolyte liquid, wherein, this aqueous electrolyte liquid contains oxyhydroxide, silicate and borate.
The present invention also provides the surface treatment method of a kind of zirconium and zirconium alloy, wherein, it is anode that this method is included in the electrolytic solution with zirconium or zirconium alloy, being not negative electrode with the electro-conductive material of electrolytic solution reaction, anode and negative electrode are electrically connected with the negative pole and the positive pole of power supply respectively, described zirconium or zirconium alloy are carried out anodic oxidation, and described electrolytic solution is aqueous electrolyte liquid of the present invention.
By method of the present invention, form oxide film on the surface of zirconium or zirconium alloy, thereby can increase substantially the erosion resistance of zirconium or zirconium alloy.In addition, after the tectorium on the top layer of removing this oxide film, can also further improve wear resistance, hardness and the scratch resistance on zirconium or zirconium alloy surface.
Embodiment
Aqueous electrolyte liquid of the present invention contains oxyhydroxide, silicate and borate.Described oxyhydroxide, silicate and borate are water-soluble salt, thereby can form aqueous electrolyte liquid.
Under the preferable case, described oxyhydroxide is sodium hydroxide and/or potassium hydroxide, described silicate and borate respectively do for oneself sodium salt and/or sylvite.
Can realize purpose of the present invention as long as contain each above-mentioned composition of the present invention in the described aqueous electrolyte liquid, the content of each composition can change in the larger context.Under the preferable case, in this aqueous electrolyte liquid, the concentration of described oxyhydroxide is the 1-30 grams per liter, and the concentration of described silicate is the 1-40 grams per liter, and described boratory concentration is the 1-15 grams per liter.Further under the preferable case, in this aqueous electrolyte liquid, the concentration of described oxyhydroxide is the 5-20 grams per liter, and the concentration of described silicate is the 10-25 grams per liter, and described boratory concentration is the 2-8 grams per liter.Under above-mentioned preferable case, can further improve erosion resistance, wear resistance, hardness and the scratch resistance on zirconium or zirconium alloy surface.
Aqueous electrolyte liquid of the present invention preferably also contains tungstate, and described tungstate is a water-soluble salt, is preferably sodium salt and/or sylvite, and the concentration of described tungstate can change in the larger context, is preferably the 0.1-10 grams per liter, more preferably the 1-5 grams per liter.Under above-mentioned preferable case, can further improve erosion resistance, wear resistance, hardness and the scratch resistance on zirconium or zirconium alloy surface.
Aqueous electrolyte liquid of the present invention preferably also contains anion surfactant, described anion surfactant can be a various anion surfactant known in those skilled in the art, is preferably Sodium dodecylbenzene sulfonate and/or sodium lauryl sulphate.The amount of described anion surfactant can change in the larger context, and under the preferable case, in described aqueous electrolyte liquid, the concentration of described anion surfactant is the 0.01-2 grams per liter, more preferably the 0.1-0.8 grams per liter.Under above-mentioned preferable case, can further improve erosion resistance, wear resistance, hardness and the scratch resistance on zirconium or zirconium alloy surface.
It is anode that the surface treatment method of zirconium of the present invention and zirconium alloy is included in the electrolytic solution with zirconium or zirconium alloy, being not negative electrode with the electro-conductive material of electrolytic solution reaction, anode and negative electrode are electrically connected with the negative pole and the positive pole of power supply respectively, described zirconium or zirconium alloy are carried out anodic oxidation, and described electrolytic solution is aqueous electrolyte liquid of the present invention.The present invention forms oxide film and can reach purpose of the present invention as long as described zirconium or zirconium alloy are carried out anodic oxidation in described aqueous electrolyte liquid.Described for example can not be stainless steel or graphite with the electro-conductive material of electrolytic solution reaction.
In order further to improve erosion resistance, wear resistance, hardness and the scratch resistance on zirconium or zirconium alloy surface, under the preferable case, described anodised condition comprises: described power supply is the direct impulse power supply, voltage is 150-400V, dutycycle is 10-40%, pulse width is 200-450Hz, and current density is 6-25A/dm
2, the temperature of electrolytic solution is 20-40 ℃, the time is 5-40 minute.
Method of the present invention all is suitable for zirconium and various zirconium alloy, is particularly useful for following preferred zirconium alloy.Total amount with described zirconium alloy is a benchmark, and described zirconium alloy preferably contains the zirconium of 35-45 weight %, the titanium of 10-15 weight %, the copper of 10-15 weight %, the nickel of 5-15 weight %, the beryllium of 20-25 weight %.
In addition, need to prove, generally speaking, outwards comprise transition layer, tight zone and tectorium at the oxide film that substrate surface forms successively by substrate surface by anodised method.The general hardness of described tight zone, wear resistance, scratch resistance and erosion resistance are all better.Though described tectorium also can play good provide protection to the surface of zirconium or zirconium alloy, more crisp usually with respect to tight zone, hardness, wear resistance, scratch resistance are relatively poor.Therefore, for obtain to have high rigidity, the zirconium or the zirconium alloy of high-wearing feature and high scratch resistance, under the preferable case, the surface treatment method of zirconium of the present invention and zirconium alloy also is included in described zirconium or zirconium alloy is carried out after the anodic oxidation, remove the top layer part of the oxide film that forms by anodic oxidation, make that the surface hardness of this zirconium or zirconium alloy is more than the 600HV, more preferably 1000-2000HV.Promptly, improve hardness, scratch resistance and the wear resistance on zirconium or zirconium alloy surface by removing the part or all of tectorium part of oxide film.
Removing the method for the top layer part of oxide film can select arbitrarily, for example can be to realize that by the method for polishing described polishing can be a mechanical grinding, and also can be manual grinding.The preferred sand paper that adopts carries out manual grinding, and described sand paper preferably uses 1200 purpose sand paper.The method of manual grinding can fully be removed loose top layer for erose zirconium or zirconium alloy workpiece particularly suitable.
Under the preferable case, method of the present invention also comprises polishes zirconium or zirconium alloy after the polishing, and the method for described polishing can be the method for the various polishings of routine.
In addition, method of the present invention can also be included in and clean carrying out oil removing before described zirconium or zirconium alloy are in being impregnated into electrolytic solution earlier.
The present invention will be described in more detail below by embodiment.
Embodiment 1
Present embodiment illustrates the surface treatment method of aqueous electrolyte liquid of the present invention and zirconium and zirconium alloy.
Preparation aqueous electrolyte liquid: 50 gram sodium hydroxide, 75 gram water glass, 20 gram Sodium Tetraboratees and 10 gram sodium wolframates are dissolved in 5 premium on currency, obtain aqueous electrolyte liquid provided by the invention, this aqueous electrolyte liquid contains 10 grams per liter sodium hydroxide, 15 grams per liter water glass, 4 grams per liter Sodium Tetraboratees, 2 grams per liter sodium wolframates.
Zirconium alloy (U.S. Liquidmetal Technologies company with 5cm * 5cm * 2mm, this zirconium alloy contains the zirconium of 50 weight %, the titanium of 10 weight %, the copper of 5 weight %, the nickel of 15 weight %, the beryllium of 15 weight %, the tin of 5 weight %) clean washing then with acetone.
With this zirconium alloy is anode, is negative electrode with the stainless steel plate, and anode and negative electrode are electrically connected with the negative pole and the positive pole of direct impulse power supply respectively, places the above-mentioned aqueous electrolyte liquid of oxidation trough to carry out anodic oxidation on this anode, negative electrode.The condition of oxidation is: the temperature of aqueous electrolyte liquid is 30 ℃, and pulse width is 300Hz, and dutycycle is 20%, and voltage is 300V, and current density is 15A/dm
2, the time of oxidation is 25 minutes.
Finally obtain surface treated zirconium alloy A1.
Embodiment 2
According to method preparation aqueous electrolyte liquid and the processing zirconium alloy of embodiment 1, different is that described aqueous electrolyte liquid contains 5 grams per liter sodium hydroxide, 10 grams per liter water glass, 2 grams per liter Sodium Tetraboratees, 1 grams per liter sodium wolframate.Finally obtain surface treated zirconium alloy A2.
Embodiment 3
According to method preparation aqueous electrolyte liquid and the processing zirconium alloy of embodiment 1, different is that described aqueous electrolyte liquid contains 20 grams per liter sodium hydroxide, 25 grams per liter water glass, 8 grams per liter Sodium Tetraboratees, 5 grams per liter sodium wolframates.Finally obtain surface treated zirconium alloy A3.
Embodiment 4
According to method preparation aqueous electrolyte liquid and the processing zirconium alloy of embodiment 1, different is that described aqueous electrolyte liquid contains 1 grams per liter sodium hydroxide, 1 grams per liter water glass, 1 grams per liter Sodium Tetraborate, 0.5 grams per liter sodium wolframate.Finally obtain surface treated zirconium alloy A4.
Embodiment 5
According to method preparation aqueous electrolyte liquid and the processing zirconium alloy of embodiment 1, different is that described aqueous electrolyte liquid contains 30 grams per liter sodium hydroxide, 40 grams per liter water glass, 15 grams per liter Sodium Tetraboratees, 10 grams per liter sodium wolframates.Finally obtain surface treated zirconium alloy A5.
Embodiment 6
According to method preparation aqueous electrolyte liquid and the processing zirconium alloy of embodiment 1, different is that described aqueous electrolyte liquid contains 35 grams per liter sodium hydroxide, 45 grams per liter water glass, 20 grams per liter Sodium Tetraboratees, 10 grams per liter sodium wolframates.Finally obtain surface treated zirconium alloy A6.
Embodiment 7
According to method preparation aqueous electrolyte liquid and the processing zirconium alloy of embodiment 1, different is that the condition of described oxidation is: the temperature of aqueous electrolyte liquid is 20 ℃, and pulse width is 200HZ, and dutycycle is 10%, and voltage is 150V, and current density is 6A/dm
2, the time of oxidation is 40 minutes.Finally obtain surface treated zirconium alloy A7.
Embodiment 8
According to method preparation aqueous electrolyte liquid and the processing zirconium alloy of embodiment 1, different is that the condition of described oxidation is: the temperature of aqueous electrolyte liquid is 40 ℃, and pulse width is 450HZ, and dutycycle is 40%, and voltage is 400V, and current density is 25A/dm
2, the time of oxidation is 5 minutes.Finally obtain surface treated zirconium alloy A8.
Embodiment 9
According to method preparation aqueous electrolyte liquid and the processing zirconium alloy of embodiment 1, different is that the condition of described oxidation is: the temperature of aqueous electrolyte liquid is 40 ℃, and pulse width is 450HZ, and dutycycle is 45%, and voltage is 420V, and current density is 30A/dm
2, the time of oxidation is 50 minutes.Finally obtain surface treated zirconium alloy A9.
Embodiment 10
Carry out surface treatment according to the method preparation aqueous electrolyte liquid of embodiment 1 with to zirconium alloy, different is that this zirconium alloy contains the zirconium of 41.2 weight %, the titanium of 13.8 weight %, the copper of 12.5 weight %, the nickel of 10 weight %, the beryllium of 22.5 weight %.Finally obtain surface treated zirconium alloy A10.
Embodiment 11
Carry out surface treatment according to the method preparation aqueous electrolyte liquid of embodiment 1 with to the metal zirconium (the safe zirconium metal of Shenzhen roc company limited, zirconium content 94.7 weight %) of 5cm * 5cm * 2mm.Finally obtain surface treated zirconium alloy A11.
Embodiment 12
According to method preparation aqueous electrolyte liquid and the processing zirconium alloy of embodiment 1, different is that described aqueous electrolyte liquid also contains the Sodium dodecylbenzene sulfonate of 0.1 grams per liter.Finally obtain surface treated zirconium alloy A12.
Embodiment 13
According to method preparation aqueous electrolyte liquid and the processing zirconium alloy of embodiment 1, different is that described aqueous electrolyte liquid also contains the Sodium dodecylbenzene sulfonate of 0.8 grams per liter.Finally obtain surface treated zirconium alloy A13.
Embodiment 14
According to method preparation aqueous electrolyte liquid and the processing zirconium alloy of embodiment 1, different is that described aqueous electrolyte liquid also contains the sodium lauryl sulphate of 0.5 grams per liter.Finally obtain surface treated zirconium alloy A14.
Embodiment 15
According to method preparation aqueous electrolyte liquid and the processing zirconium alloy of embodiment 1, different is not add sodium wolframate in the aqueous electrolyte liquid.Finally obtain surface treated zirconium alloy A15.
Embodiment 16
According to method preparation aqueous electrolyte liquid and the processing zirconium alloy of embodiment 2, different is not add sodium wolframate in the aqueous electrolyte liquid.Finally obtain surface treated zirconium alloy A16.
Embodiment 17
According to method preparation aqueous electrolyte liquid and the processing zirconium alloy of embodiment 3, different is not add sodium wolframate in the aqueous electrolyte liquid.Finally obtain surface treated zirconium alloy A17.
Embodiment 18
According to method preparation aqueous electrolyte liquid and the processing zirconium alloy of embodiment 4, different is not add sodium wolframate in the aqueous electrolyte liquid.Finally obtain surface treated zirconium alloy A18.
Embodiment 19
According to method preparation aqueous electrolyte liquid and the processing zirconium alloy of embodiment 5, different is not add sodium wolframate in the aqueous electrolyte liquid.Finally obtain surface treated zirconium alloy A19.
Embodiment 20
According to method preparation aqueous electrolyte liquid and the processing zirconium alloy of embodiment 6, different is not add sodium wolframate in the aqueous electrolyte liquid.Finally obtain surface treated zirconium alloy A20.
Comparative Examples 1
According to the method for embodiment 1 preparation aqueous electrolyte liquid with handle zirconium alloy, different is, not boronic acid containing sodium and sodium wolframate in the aqueous electrolyte liquid.Finally obtain surface treated zirconium alloy D1.
Comparative Examples 2
According to the method for embodiment 6 preparation aqueous electrolyte liquid with handle zirconium alloy, different is, not boronic acid containing sodium and sodium wolframate in the aqueous electrolyte liquid.Finally obtain surface treated zirconium alloy D2.
Embodiment 21
The zirconium alloy A1 that embodiment 1 is made carries out following performance test, and the result is as shown in table 1.
(1) neutral salt spray test
Zirconium alloy A1 is placed in the salt fog cabinet, and the sodium chloride brine with 5 ± 0.5 weight % under 35 ℃ sprays this zirconium alloy A1 continuously, and the oxide film corrosion until this zirconium alloy makes the surface of zirconium alloy expose.The corrosive time appears in record.
(2) remove the oxide film of the top layer part of zirconium alloy A1 with 1200 purpose sand paperings, make that the hardness of oxide film is 1600HV, the hardness of described oxide film is measured according to ASTM D3363 and is obtained.The thickness of the oxide film after the polishing is as shown in table 1.Carry out the test of following wearability test and scratch resistance then.
1) the wear-resisting test of RCA paper tape
Use the RCA paper tape wear resistant instrument of model as F350008, the oxide film on this zirconium alloy of friction A1 surface under 175 gram forces, when exposing obvious polishing scratch on the zirconium alloy surface, the number of turns that the record rubber wheel rotates;
2) scratch resistance test
Carry out scratch resistance test with scratching instrument then, gauge head is the diamond of 0.75 millimeter of diameter, and test angle is 90 °, and with the power of the 3N surface scratch at this zirconium alloy A1, if the surperficial no marking of zirconium alloy A1, then scratch resistance performance is qualified, otherwise is defective.
Embodiment 21-40
According to the method for embodiment 21 embodiment 2-20 is handled the zirconium alloy or the metal zirconium that obtain and carry out performance test.The result is as shown in table 1.
Comparative Examples 3
According to the method for embodiment 21 Comparative Examples 1 is handled the zirconium alloy D1 that obtains and carry out performance test.But this zirconium alloy D1 is after polishing, and the hardness on the surface of zirconium alloy can't reach 1600HV, the highlyest only can reach 900HV.The result is as shown in table 1.
Comparative Examples 4
According to the method for embodiment 21 Comparative Examples 2 is handled the zirconium alloy D2 that obtains and carry out performance test.But this zirconium alloy D2 is after polishing, and the hardness on the surface of zirconium alloy can't reach 1600HV, the highlyest only can reach 600HV.The result is as shown in table 1.
Comparative Examples 5
According to the method for embodiment 21 the not surface treated zirconium alloy of embodiment 10 is carried out performance test, this zirconium alloy note is made D3, the oxide film that this zirconium alloy surface exists natural oxidation to form, the thickness of this oxide film is 0.3 μ m.The result is as shown in table 1.
Comparative Examples 6
Method according to embodiment 21 is carried out performance test to the not surface treated metal zirconium of embodiment 11, and this zirconium alloy note is made D4, the oxide film that this zirconium alloy surface exists natural oxidation to form, and the thickness of this oxide film is 0.2 μ m.The result is as shown in table 1.
Table 1
As can be seen from Table 1, obviously improve through the zirconium of method processing of the present invention or erosion resistance, wear resistance, hardness and the scratch resistance of zirconium alloy.For example, zirconium alloy A15 is compared with zirconium alloy D1 and zirconium alloy A20 is compared with zirconium alloy D2, after aqueous electrolyte liquid of the present invention was handled, the erosion resistance of zirconium alloy and wear resistance all obviously will be got well as can be seen.In addition, under the preferred condition of the present invention, treated zirconium or zirconium alloy have better performance.
Claims (9)
1. an aqueous electrolyte liquid is characterized in that, this aqueous electrolyte liquid contains oxyhydroxide, silicate, borate, tungstate and anion surfactant.
2. aqueous electrolyte liquid according to claim 1, wherein, in this aqueous electrolyte liquid, the concentration of described oxyhydroxide is the 1-30 grams per liter, and the concentration of described silicate is the 1-40 grams per liter, and described boratory concentration is the 1-15 grams per liter.
3. aqueous electrolyte liquid according to claim 2, wherein, in this aqueous electrolyte liquid, the concentration of described oxyhydroxide is the 5-20 grams per liter, and the concentration of described silicate is the 10-25 grams per liter, and described boratory concentration is the 2-8 grams per liter.
4. according to any described aqueous electrolyte liquid among the claim 1-3, wherein, described oxyhydroxide is sodium hydroxide and/or potassium hydroxide, described silicate and borate respectively do for oneself sodium salt and/or sylvite.
5. aqueous electrolyte liquid according to claim 1, wherein, described tungstate is sodium salt and/or sylvite, the concentration of described tungstate is the 1-5 grams per liter.
6. aqueous electrolyte liquid according to claim 1, wherein, described anion surfactant is Sodium dodecylbenzene sulfonate and/or sodium lauryl sulphate, the concentration of described anion surfactant is the 0.1-0.8 grams per liter.
7. the surface treatment method of zirconium and zirconium alloy, it is characterized in that, it is anode that this method is included in the electrolytic solution with zirconium or zirconium alloy, being not negative electrode with the electro-conductive material of electrolytic solution reaction, anode and negative electrode are electrically connected with the negative pole and the positive pole of power supply respectively, described zirconium or zirconium alloy are carried out anodic oxidation, and described electrolytic solution is any described aqueous electrolyte liquid among the claim 1-6.
8. method according to claim 7 wherein, is a benchmark with the total amount of described zirconium alloy, and described zirconium alloy contains the zirconium of 35-45 weight %, the titanium of 10-15 weight %, the copper of 10-15 weight %, the nickel of 5-15 weight %, the beryllium of 20-25 weight %.
9. method according to claim 7, wherein, this method also is included in carries out described zirconium or zirconium alloy after the anodic oxidation, and the top layer part of removing the oxide film that is formed by anodic oxidation makes that the surface hardness of this zirconium or zirconium alloy is more than the 600HV.
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| CN102851719B (en) * | 2011-06-29 | 2016-01-27 | 比亚迪股份有限公司 | A kind of Zirconium-base non-crystalline alloy compound material and preparation method thereof |
| CN104514027A (en) * | 2014-12-25 | 2015-04-15 | 广东省工业技术研究院(广州有色金属研究院) | Electrolyte solution for preparing aluminum and aluminum alloy ceramic membrane through micro-arc oxidation technology |
| CN108018592B (en) * | 2017-10-10 | 2022-05-10 | 上海核工程研究设计院有限公司 | Zirconium alloy micro-arc oxidation surface modification method |
| CN109825797B (en) * | 2019-03-07 | 2020-06-16 | 苏州微创关节医疗科技有限公司 | Zirconium alloy treatment method and application |
| CN110444814B (en) * | 2019-08-09 | 2021-08-24 | 南京工业大学 | Chargeable and dischargeable aqueous solution energy storage device |
| CN111218707B (en) * | 2020-02-28 | 2021-07-23 | 湖南大学 | Method for improving surface hydrophilicity of zirconium alloy |
| CN111424279A (en) * | 2020-04-26 | 2020-07-17 | 歌尔股份有限公司 | Corrosive and corrosion method for displaying metallographic structure of cobalt-chromium-molybdenum alloy |
| CN113403662A (en) * | 2021-07-27 | 2021-09-17 | 燕山大学 | Micro-arc oxidation treatment method for zirconium and zirconium alloy surfaces |
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