CN112048726B - Process method for improving surface quality of beta-type titanium alloy during acid pickling - Google Patents
Process method for improving surface quality of beta-type titanium alloy during acid pickling Download PDFInfo
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
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Abstract
The invention belongs to the technical field of titanium alloy surface treatment, and relates to a process method for improving surface quality of beta-type titanium alloy during acid washing; according to the invention, the titanium alloy is subjected to short-time acid cleaning by introducing the nitric acid aqueous solution with a certain concentration, and the proportioning components of the pickling solution are correspondingly adjusted, so that the nitric acid aqueous solution with stronger acidity and higher concentration is subjected to a micro-passivation reaction preferentially with the titanium alloy matrix, the reaction of residual hydrofluoric acid and the titanium alloy matrix is fully inhibited, the risk of hydrogen absorption of the titanium alloy matrix is avoided, the surface of the part subjected to acid cleaning has no defects of acid spots, pits, corrosion pits and the like, the surface is silvery white, and the technical problem of low surface quality during acid cleaning of the beta-type titanium alloy is fundamentally solved; the method has simple and convenient process operation, is suitable for pickling and cleaning the near-beta type, metastable-beta type and fully-stable beta type titanium alloys, not only reduces the labor intensity of operators and improves the pickling efficiency, but also enhances the stability of the pickling surface quality of the beta type titanium alloys, and is particularly suitable for industrial large-scale production.
Description
Technical Field
The invention belongs to the technical field of titanium alloy surface treatment, and relates to a process method for improving surface quality of beta-type titanium alloy during acid washing.
Background
The titanium alloy acid cleaning process is a well developed surface treatment technology. The principle of pickling titanium alloy with hydrofluoric acid-nitric acid-water solution system is that hydrofluoric acid solution can destroy and dissolve passive film on the surface of titanium alloy, remove part of matrix to obtain better surface quality, and add nitric acid solution with certain concentration to inhibit hydrogen generation and avoid the risk of hydrogen absorption of matrix. The pickling process is applied to semi-finished products of titanium alloy, including plates, strips, sections, pipes, wire rods, bars, forgings, die forgings, castings, sheet metal parts and machined parts, and aims to remove oxide skins and hard alpha layers on the surfaces of the titanium alloy. In addition, in the process of anodizing, passivating, electroplating, welding and the like of the titanium alloy, pickling is an essential pretreatment step. In the current industrial field, different pickling processes are generally implemented according to different purposes when the titanium alloy is pickled, and after pickling is finished, the titanium alloy is cleaned by water and dried by compressed air. The ideal surface of the titanium alloy after acid pickling should be silvery white metallic luster, the hydrogen content does not exceed the standard, and production technicians can generally judge whether the acid pickling process is reasonable according to the surface appearance characteristics.
The beta titanium alloy has the characteristics of excellent heat treatment strengthening effect, high hardenability, good processing performance and the like, and is most suitable for developing and developing high-strength and high-toughness or ultrahigh-strength and high-toughness titanium alloys. With the urgent need of a new generation of advanced airplanes for weight reduction, key structural components made of the titanium alloy are gradually applied. However, when the titanium alloy is pickled by using the traditional pickling method, the surface of the part after pickling is rapidly blackened and acid spots are locally formed when the part is put into a water tank for cleaning, the popular description is that the part blackens when meeting water, and the defects of pits, corrosion pits and the like are formed in serious conditions, so that the pickled surface quality of the part is influenced. Although the surface of the part is rapidly and one by one washed by experienced operators by using rapidly flowing water to be improved, the problems of blackening the surface of the titanium alloy, and locally forming acid spots, pockmarks and pits can not be completely solved due to the existence of a plurality of complex characteristics of variable cross sections, grooves, holes and the like of the part. Therefore, the labor intensity of operators is increased, the production progress is influenced, the stability of the part acid washing process is influenced, and the method is not suitable for large-scale high-efficiency acid washing of industry. In addition, engineering technicians can relieve the phenomenon by properly changing the component ratio of the hydrofluoric acid-nitric acid-aqueous solution, but the problem cannot be completely solved. Therefore, in order to solve the technical problems that the acid-washed surface of the beta-type titanium alloy is blackened and acid spots, pits and corrosion pits are easily formed locally and improve the acid-washed surface quality of the beta-type titanium alloy, a new process method suitable for industrial large-scale production needs to be designed.
Disclosure of Invention
In order to overcome the defects of pickling beta-type titanium alloy in the prior pickling technology, the invention provides a process method for improving the surface quality of the beta-type titanium alloy during pickling.
The technical scheme adopted by the invention is as follows:
a process method for improving surface quality of beta-type titanium alloy during acid washing is characterized by comprising the following steps:
(1) pretreatment before pickling: removing oxide skin and impurities on the surface of the titanium alloy, cleaning and drying;
(2) acid washing: soaking the titanium alloy treated in the step (1) into a mixed solution containing 560-700 ml/l of industrial nitric acid, 40-80 ml/l of industrial hydrofluoric acid and the balance of water at room temperature for pickling, wherein the pickling time is 5-15 minutes;
(3) acid cleaning: after the titanium alloy treated in the step (2) is subjected to acid pickling, quickly immersing the titanium alloy into a mixed solution containing (100-200) ml/l of industrial grade nitric acid and the balance of water at room temperature for cleaning for 5-30 seconds;
(4) water cleaning: and (4) cleaning the titanium alloy treated in the step (3) with water at room temperature, and finally drying the titanium alloy by blowing with clean compressed air or in an oven.
The pretreatment before acid washing in the step (1) is one or more of composite pretreatment of sand blowing, organic solvent cleaning, chemical oil removal and alkali washing.
The concentration of the industrial nitric acid in the step (2) is 60-65%.
The concentration of the industrial hydrofluoric acid in the step (2) is 45%.
The concentration of the industrial nitric acid in the step (3) is 60-65%.
And (3) after the titanium alloy in the step (2) is subjected to acid cleaning, the transfer time is not more than 20 seconds.
Compared with the prior art, the invention has the following advantages:
1. the invention provides a process method for improving surface quality of beta-type titanium alloy during acid pickling, and aims to solve the technical problems that the surface of the beta-type titanium alloy is blackened during acid pickling, and acid spots, pits and pits are easily formed locally. In the traditional process, the titanium alloy is generally washed by water directly after being washed by acid, but when the beta-type titanium alloy is washed by acid, because the reaction rate of the beta-type titanium alloy and hydrofluoric acid is obviously higher than that of the alpha-type and (alpha + beta) -type titanium alloys, the hydrofluoric acid remained on the surface of a part is instantly contacted with water to react with a titanium alloy matrix quickly, but the reaction product cannot be dissolved by the aqueous solution at the moment, and macroscopically, the phenomenon that the surface of the titanium alloy is blackened to form acid spots, pits and pits is shown. By introducing a short-time acid cleaning process and correspondingly adjusting the proportion of proper pickling solution, the invention can effectively prevent the residual hydrofluoric acid aqueous solution on the surface of the part from reacting with the titanium alloy matrix, thereby solving the production problem of low surface quality of the beta-type titanium alloy part (especially the part with complex characteristics). In addition, the process is simple and convenient to operate, is suitable for pickling and cleaning near-beta type, metastable-beta type and fully-stable beta type titanium alloys, not only reduces the labor intensity of operators and improves the pickling efficiency, but also enhances the stability of the pickling surface quality of the titanium alloys, and is particularly suitable for industrial large-scale production.
2. The key technology of the invention is as follows: the titanium alloy is subjected to short-time acid cleaning for 5-30 seconds by introducing the nitric acid aqueous solution with a certain concentration, the nitric acid aqueous solution with stronger acidity and higher concentration is subjected to micro-passivation reaction preferentially with the titanium alloy matrix, the reaction of residual hydrofluoric acid and the titanium alloy matrix is fully inhibited, the risk of hydrogen absorption of the titanium alloy matrix is completely eradicated, the technical problems of surface blackening, acid spots, pits and pits formed during acid cleaning of the beta-type titanium alloy are fundamentally solved, and the acid cleaning surface quality is remarkably improved.
The present invention will be described in further detail with reference to examples.
The specific implementation mode is as follows:
example 1
Taking a method for removing oxide scale by pickling a TB8 titanium alloy plate with the thickness of 20mm as an example, the method comprises the following steps:
(1) pretreatment before pickling: primarily removing oxide skin on the surface of the TB8 titanium alloy plate by dry sand blasting, then removing sand attached to the surface by water at room temperature, and drying the water stain of the plate by compressed air;
(2) acid washing: soaking the TB8 titanium alloy plate treated in the step (1) into a mixed solution of 560ml/l industrial nitric acid, 45ml/l industrial hydrofluoric acid and the balance of water at room temperature for pickling for 10 minutes;
(3) acid cleaning: rapidly immersing the TB8 titanium alloy plate treated in the step (2) into a mixed solution of 120ml/l industrial grade nitric acid and the balance of water within 20 seconds to clean, wherein the cleaning time is 10 seconds;
(4) water cleaning: and (4) cleaning the TB8 titanium alloy plate treated in the step (3) with water at room temperature, and finally drying the TB8 titanium alloy plate by blowing with clean compressed air or in an oven.
After acid cleaning, the oxide skin on the surface of the plate is thoroughly removed, the surface color is uniform, the defects of acid spots, pockmarks, corrosion pits and the like are avoided, the plate is silvery white metallic luster, the content of the plate H is 0.004%, and the standard requirement is met.
Example 2
Taking the pickling process involved in the process of passivating the TB17 titanium alloy part as an example, the method comprises the following steps:
(1) pretreatment before pickling: after chemical degreasing and alkali washing, the TB17 titanium alloy part is washed by water at room temperature, and then the water stain on the surface of the TB17 titanium alloy part is dried by compressed air;
(2) acid washing: soaking the TB17 titanium alloy part treated in the step (1) into a mixed solution containing 600ml/l of industrial nitric acid, 50ml/l of industrial hydrofluoric acid and the balance of water at room temperature for pickling for 5 minutes;
(3) acid cleaning: rapidly immersing the TB17 titanium alloy part treated in the step (2) into a mixed solution containing 150ml/l of industrial grade nitric acid and the balance of water within 20 seconds to clean, wherein the cleaning time is 8 seconds;
(4) water cleaning: and (4) cleaning the TB17 titanium alloy part treated in the step (3) with water at room temperature, and finally drying the TB17 titanium alloy part with clean compressed air or drying the titanium alloy part in an oven.
After acid pickling, the surface of the TB17 titanium alloy part has uniform color, no defects such as acid spots, pits, corrosion pits and the like, the surface has silvery white metallic luster, the content of the part H is 0.005 percent, and the standard requirement is met.
Example 3
Taking the pickling process involved in the process of passivating the TC18 titanium alloy part as an example, the method comprises the following steps:
(1) pretreatment before pickling: after chemical degreasing and alkali washing, the TC18 titanium alloy part is washed by water at room temperature, and then the water stain on the surface of the TC18 titanium alloy part is dried by compressed air;
(2) acid washing: soaking the TC18 titanium alloy part treated in the step (1) into a mixed solution containing 650ml/l of industrial nitric acid, 60ml/l of industrial hydrofluoric acid and the balance of water at room temperature for pickling for 8 minutes;
(3) acid cleaning: rapidly immersing the TC18 titanium alloy part treated in the step (2) into a mixed solution containing 180ml/l of industrial grade nitric acid and the balance of water within 20 seconds for cleaning, wherein the cleaning time is 10 seconds;
(4) water cleaning: and (4) cleaning the TC18 titanium alloy part treated in the step (3) by using water at room temperature, and finally drying the TC18 titanium alloy part by using clean compressed air or drying the TC18 titanium alloy part in an oven.
After acid pickling, the TC18 titanium alloy part has uniform surface color, no defects such as acid spots, pits, corrosion pits and the like, silver-white metallic luster on the surface, and 0.0031 percent of H content, and meets the standard requirement.
Example 4
Taking the acid cleaning process involved in the process of anodizing the TB17 titanium alloy part as an example, the method comprises the following steps of:
(1) pretreatment before pickling: after chemical degreasing and alkali washing, the TB17 titanium alloy part is washed by water at room temperature, and then the water stain on the surface of the TB17 titanium alloy part is dried by compressed air;
(2) acid washing: soaking the TB17 titanium alloy part treated in the step (1) into a mixed solution of 680ml/l industrial nitric acid, 70ml/l industrial hydrofluoric acid and the balance of water at room temperature for pickling for 10 minutes;
(3) acid cleaning: rapidly immersing the TB17 titanium alloy part treated in the step (2) into a mixed solution containing 200ml/l of industrial-grade nitric acid and the balance of water within 20 seconds to clean, wherein the cleaning time is 8 seconds;
(4) water cleaning: and (4) cleaning the TB17 titanium alloy part treated in the step (3) with water at room temperature, and finally drying the TB17 titanium alloy part with clean compressed air or drying the titanium alloy part in an oven.
After acid pickling, the surface of the TB17 titanium alloy part is uniform in color, free of defects such as acid spots, pits and corrosion pits and the like, silvery white in metallic luster, and 0.0043% of the H content of the part, and meets the standard requirement.
Claims (6)
1. A process method for improving surface quality of beta-type titanium alloy during acid washing is characterized by comprising the following steps:
(1) pretreatment before pickling: removing oxide skin and impurities on the surface of the titanium alloy, cleaning and drying;
(2) acid washing: soaking the titanium alloy treated in the step (1) into a mixed solution containing 560-700 ml/l of industrial nitric acid, 40-80 ml/l of industrial hydrofluoric acid and the balance of water at room temperature for pickling, wherein the pickling time is 5-15 minutes;
(3) acid cleaning: after the titanium alloy treated in the step (2) is subjected to acid pickling, soaking the titanium alloy into a mixed solution containing 100-200 ml/l of industrial-grade nitric acid and the balance of water for cleaning within 20 seconds at room temperature, wherein the cleaning time is 5-30 seconds;
(4) water cleaning: and (4) cleaning the titanium alloy treated in the step (3) with water at room temperature, and finally blowing the titanium alloy dry with clean compressed air or drying in an oven.
2. The process method for improving the surface quality of the beta titanium alloy during acid washing according to claim 1, wherein the pretreatment before acid washing in the step (1) is one or more of sand blowing, organic solvent cleaning, chemical oil removal and alkaline washing pretreatment.
3. The process method for improving the surface quality of the beta titanium alloy during acid washing according to claim 1, wherein the concentration of the industrial nitric acid in the step (2) is 60-65%.
4. The process method for improving the surface quality of the beta titanium alloy during acid cleaning according to claim 1, wherein the concentration of the industrial-grade hydrofluoric acid in the step (2) is 45%.
5. The process method for improving the surface quality of the beta titanium alloy during acid washing according to claim 1, wherein the concentration of the industrial nitric acid in the step (3) is 60-65%.
6. The process for improving the surface quality of a beta titanium alloy during acid washing according to claim 1, wherein the transfer time of the titanium alloy in the step (2) after acid washing and acid washing in the step (3) is not more than 20 seconds.
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| JPH1158071A (en) * | 1997-08-27 | 1999-03-02 | Nippon Steel Weld Prod & Eng Co Ltd | Pickling method for ti welding wire |
| JP4385157B2 (en) * | 1999-09-22 | 2009-12-16 | 大同特殊鋼株式会社 | Method for producing titanium or titanium alloy product |
| CN104060286A (en) * | 2013-11-28 | 2014-09-24 | 攀钢集团攀枝花钢铁研究院有限公司 | Titanium belt continuous pickling method |
| CN106011889A (en) * | 2016-06-28 | 2016-10-12 | 国营芜湖机械厂 | Technology for removing alpha layer on surface of titanium alloy forge piece |
| CN108118347A (en) * | 2017-12-27 | 2018-06-05 | 西安西工大超晶科技发展有限责任公司 | A kind of method of beta-type titanium alloy plate surface acid-washing |
| CN109136949A (en) * | 2018-09-14 | 2019-01-04 | 昆明理工大学 | A method of removal titanium or titanium alloy sheet are with oxide skin |
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