CN111945102A - Method for preparing oxide film on surface of metal tantalum and application thereof - Google Patents

Method for preparing oxide film on surface of metal tantalum and application thereof Download PDF

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Publication number
CN111945102A
CN111945102A CN201910398933.3A CN201910398933A CN111945102A CN 111945102 A CN111945102 A CN 111945102A CN 201910398933 A CN201910398933 A CN 201910398933A CN 111945102 A CN111945102 A CN 111945102A
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China
Prior art keywords
temperature
oxidation
furnace
metal
atmosphere furnace
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CN201910398933.3A
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Chinese (zh)
Inventor
王丁丁
王筠
马贤
刘庆凯
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Research Institute of Physical and Chemical Engineering of Nuclear Industry
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Research Institute of Physical and Chemical Engineering of Nuclear Industry
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Priority to CN201910398933.3A priority Critical patent/CN111945102A/en
Publication of CN111945102A publication Critical patent/CN111945102A/en
Pending legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • 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
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
    • C23C8/10—Oxidising
    • C23C8/12—Oxidising using elemental oxygen or ozone

Abstract

The invention discloses a method for preparing an oxide film on the surface of metal tantalum and application thereof, wherein the method comprises the following steps: step 1, polishing pretreatment is carried out on a metal tantalum substrate; step 2, raising the temperature of the atmosphere furnace 1 to a first oxidation temperature T1, introducing oxygen, keeping the oxygen pressure at positive pressure, placing the metal tantalum substrate in the atmosphere furnace, closing a furnace door of the atmosphere furnace, starting timing when the temperature in the atmosphere furnace is constant, and finishing the first-step oxidation when the time reaches a first oxidation time T1; and 3, raising the temperature in the atmosphere furnace to a second oxidation temperature T2, starting timing when the temperature reaches a preset temperature, closing the furnace body for heating when the time reaches a second oxidation time T2, closing oxygen after the furnace body is cooled to 100 ℃, taking out a sample, and naturally cooling to room temperature to finish oxidation treatment. The method can effectively improve the corrosion resistance of the metal tantalum in the liquid metal smelting process.

Description

Method for preparing oxide film on surface of metal tantalum and application thereof
Technical Field
The invention relates to the technical field of metal surface treatment, in particular to a method for preparing an oxide film on the surface of metal tantalum, which can effectively improve the corrosion resistance of the metal tantalum in the process of smelting liquid metal, prolong the service life of materials and reduce the secondary pollution of the materials to the smelted metal.
Background
When a vacuum furnace is adopted for smelting metal, the metal has very active chemical properties in a melting evaporation state and can almost react with most materials, so that the smelted container material is required to have good high-temperature chemical stability, high-temperature resistance, thermal shock resistance and the like.
The oxide film is prepared on the surface of the metal tantalum in order to improve the corrosion resistance of the metal tantalum to liquid metal, so that the formed oxide film is required to be uniform, compact and free from obvious peeling, and needs to reach a certain thickness. The currently common anodic oxidation method is easy to form a film on the surface of some simple shapes, and the film is not uniform on a large-scale complex member. The direct oxidation method has a main problem that the formed film is not dense, and the oxide film is very easy to crack and peel.
Disclosure of Invention
The invention aims to solve the problems of uneven film formation, non-density and easy cracking of an oxide film on the surface of metal tantalum by using an anodic oxidation method in the prior art, and provides a method for preparing the oxide film on the surface of the metal tantalum, which can effectively protect a metal tantalum substrate, further improve the corrosion resistance of the metal tantalum in the liquid metal smelting process, prolong the service life of materials and reduce the secondary pollution of the materials to the molten metal.
Another object of the present invention is to provide the use of the method for improving the corrosion resistance of a tantalum metal substrate, wherein the thickness of the oxide film can reach 10-20 microns.
The technical scheme adopted for realizing the purpose of the invention is as follows:
a method for preparing an oxide film on the surface of metallic tantalum comprises the following steps:
step 1, polishing pretreatment is carried out on a metal tantalum substrate;
step 2, raising the temperature of the atmosphere furnace 1 from the temperature rise speed of 5-10 ℃/min to a first oxidation temperature T1, introducing oxygen, keeping the oxygen pressure at positive pressure (0.2-0.4MPa, preferably 0.3MPa), placing the metal tantalum substrate in the atmosphere furnace, and finishing the first-step oxidation when the time reaches a first oxidation time T1;
and 3, increasing the temperature in the atmosphere furnace from the heating speed of 5-10 ℃/min to a second oxidation temperature T2, starting timing when the temperature reaches a preset temperature, closing the furnace body for heating when the time reaches a second oxidation time T2, closing oxygen after the furnace body is cooled to 100 ℃, taking out a sample, and naturally cooling to the room temperature to finish the oxidation treatment.
In the technical scheme, the polishing pretreatment in the step 1 is to use No. 60-240 sand paper for polishing, polishing and grinding.
In the above technical solution, the metal tantalum substrate is an irregular substrate.
In the above technical scheme, the metal tantalum substrate is a tantalum crucible.
In the above technical solution, in the step 2, the metal tantalum substrate is placed on a pedestal support in the atmosphere furnace.
In the technical scheme, the first oxidation temperature T1 in the step 2 is 200-400 ℃, and the first oxidation time T1 is 30 min-1 h.
In the technical scheme, the second oxidation temperature T2 in the step 3 is 400-600 ℃, and the second oxidation time T2 is 30 min-1 h.
In the above technical solution, the second oxidation temperature T2 in the step 3 is 200 to 400 ℃ higher than the first oxidation temperature T1 in the step 2.
In the technical scheme, the oxygen pressure in the step 2 is 0.2-0.4 MPa.
In another aspect of the invention, the use of the method for improving the corrosion resistance of the tantalum metal substrate is also included.
In the above technical solution, the thickness of the oxide film is 10-20 μm.
Compared with the prior art, the invention has the beneficial effects that:
1. by using the two-step oxidation technology, the metal tantalum is oxidized, the problems of pulverization and stripping in the oxidation process are solved, and the thickness of an oxide film is increased. Meanwhile, the film forming is relatively uniform for some components with complex shapes.
2. The treatment process is simple and convenient for commercial production and application.
Drawings
FIG. 1 is a flow chart of a metallic tantalum oxidation process;
FIG. 2 is a schematic view of an oxidation process.
In the figure: 1-atmosphere furnace, 2-metal tantalum substrate (tantalum crucible to be treated), and 3-support.
Detailed Description
The present invention will be described in further detail with reference to specific examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
A method for preparing an oxide film on the surface of metallic tantalum comprises the following steps:
step 1, performing pretreatment on a metal tantalum substrate 2 (tantalum crucible), specifically, performing polishing (coarse grinding and fine grinding) and polishing and grinding treatment by using No. 60-240 abrasive paper, so as to reduce processing marks on the surface of the metal tantalum substrate and facilitate the uniformity of film formation.
And 2, raising the temperature of the atmosphere furnace 1 to 400 ℃ of the first oxidation temperature at the temperature rise speed of 5 ℃/min, introducing oxygen, keeping the pressure of the oxygen at the micro positive pressure of 0.3MPa, placing the metal tantalum substrate in the atmosphere furnace and on a base support 3 of the atmosphere furnace to ensure that the oxygen can smoothly circulate, and finally closing a furnace door of the atmosphere furnace. And when the temperature in the furnace is constant, timing is started, and when the time reaches 30min, the first-step oxidation is finished.
And 3, increasing the temperature of the atmosphere furnace to 600 ℃ of the second oxidation temperature at the temperature increase speed of 5 ℃/min, starting timing when the temperature reaches the preset temperature, and closing the furnace body for heating when the temperature reaches 30 min. And (4) cooling to 100 ℃ along with the furnace, simultaneously closing oxygen, taking out the sample, and naturally cooling to room temperature to finish the oxidation treatment.
In order to obtain a dense, uniform oxide film, the rate of oxidation must be controlled, the primary factor being the temperature of oxidation. When the temperature is low, the oxidation has no obvious effect, and when the temperature is too high, the oxidation is violent, the tantalum matrix is rapidly oxidized, and the phenomena of pulverization, stripping and the like occur on the surface. By adopting the first low-temperature oxidation treatment, the phenomena of pulverization and stripping of the oxide film are obviously solved, and the uniform and compact oxide film is obtained.
In order to make the oxide film corrosion resistant, the thickness of the formed film must be constant, and therefore, when the temperature is constant, the thickness of the oxide film must be increased by increasing the oxidation time. The technology enables the thickness of the oxide film to reach dozens of microns in a short time through two-step high-temperature oxidation, and the corrosion resistance is improved.
Example 2
Step 1, performing pretreatment on a metal tantalum substrate 2 (tantalum crucible), specifically, performing polishing (coarse grinding and fine grinding) and polishing and grinding treatment by using No. 60-240 abrasive paper, so as to reduce processing marks on the surface of the metal tantalum substrate and facilitate the uniformity of film formation.
And 2, raising the temperature of the atmosphere furnace 1 to 200 ℃ of the first oxidation temperature at the temperature rise speed of 10 ℃/min, introducing oxygen, keeping the pressure of the oxygen at the micro positive pressure of 0.2MPa, placing the metal tantalum substrate in the atmosphere furnace and on a base support 3 of the atmosphere furnace to ensure that the oxygen can smoothly circulate, and finally closing a furnace door of the atmosphere furnace. When the temperature in the furnace is constant, timing is started, and when the time reaches 1h, the first-step oxidation is completed.
And 3, increasing the temperature of the atmosphere furnace to a second oxidation temperature of 400 ℃ at a temperature increase speed of 10 ℃/min, starting timing when the temperature reaches a preset temperature, and stopping heating of the furnace body when 1h is reached. Cooling the sample to 100 ℃ along with the furnace, closing the oxygen, taking out the sample, and naturally cooling the sample to room temperature to finish the oxidation treatment.
The process for oxidizing the metal tantalum solves the problems of pulverization and stripping in the oxidation process, improves the thickness of an oxide film, and simultaneously forms a film on some components with complex shapes more uniformly.
Example 3
Step 1, performing pretreatment on a metal tantalum substrate 2 (tantalum crucible), specifically, performing polishing (coarse grinding and fine grinding) and polishing and grinding treatment by using No. 60-240 abrasive paper, so as to reduce processing marks on the surface of the metal tantalum substrate and facilitate the uniformity of film formation.
And 2, raising the temperature of the atmosphere furnace 1 to 200 ℃ of the first oxidation temperature at the temperature rise speed of 8 ℃/min, introducing oxygen, keeping the pressure of the oxygen at the micro positive pressure of 0.4MPa, placing the metal tantalum substrate in the atmosphere furnace, placing the metal tantalum substrate on a base support of the atmosphere furnace 3, ensuring that the oxygen can smoothly circulate, and finally closing a furnace door of the atmosphere furnace. When the temperature in the furnace is constant, timing is started, and when the time reaches 1h, the first-step oxidation is completed.
And 3, increasing the temperature of the atmosphere furnace to 600 ℃ of the second oxidation temperature at the temperature increase speed of 8 ℃/min, starting timing when the temperature reaches the preset temperature, and closing the furnace body for heating when the temperature reaches 30 min. And when the temperature is reduced to 100 ℃, closing the oxygen, taking out the sample, and naturally cooling to the room temperature to finish the oxidation treatment.
The process for oxidizing the metal tantalum solves the problems of pulverization and stripping in the oxidation process, improves the thickness of an oxide film, and simultaneously forms a film on some components with complex shapes more uniformly.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (11)

1. A method for preparing an oxide film on the surface of metal tantalum is characterized by comprising the following steps:
step 1, polishing pretreatment is carried out on a metal tantalum substrate;
step 2, raising the temperature of the atmosphere furnace 1 from the temperature rise speed of 5-10 ℃/min to a first oxidation temperature T1, introducing oxygen, keeping the oxygen pressure at positive pressure, placing the metal tantalum substrate in the atmosphere furnace, and finishing the first-step oxidation when the time reaches a first oxidation time T1;
and 3, increasing the temperature in the atmosphere furnace from the heating speed of 5-10 ℃/min to a second oxidation temperature T2, starting timing when the temperature reaches a preset temperature, closing the furnace body for heating when the time reaches a second oxidation time T2, closing oxygen after the furnace body is cooled to 100 ℃, taking out a sample, and naturally cooling to the room temperature to finish the oxidation treatment.
2. The method according to claim 1, wherein the pre-polishing treatment in step 1 is a grinding, polishing and lapping treatment with 60 to 240 grit sandpaper.
3. The method of claim 1, wherein the metallic tantalum substrate is an irregularly shaped substrate.
4. The method of claim 3, wherein the metallic tantalum substrate is a tantalum crucible.
5. The method of claim 1, wherein said tantalum metal substrate is placed on a pedestal support in said atmospheric furnace in step 2.
6. The method of claim 1, wherein the first oxidation temperature T1 in the step 2 is 200-400 ℃ and the first oxidation time T1 is 30 min-1 h.
7. The method of claim 1, wherein the second oxidation temperature T2 in the step 3 is 400-600 ℃, and the second oxidation time T2 is 30 min-1 h.
8. The method of claim 1, wherein the second oxidation temperature T2 in step 3 is 200-400 ℃ higher than the first oxidation temperature T1 in step 2.
9. The method of claim 1, wherein the oxygen pressure in step 2 is 0.2 to 0.4 MPa.
10. Use of the method of any one of claims 1-9 to improve the corrosion resistance of the metallic tantalum substrate.
11. The use according to claim 10, wherein the oxide film has a thickness of 10-20 microns.
CN201910398933.3A 2019-05-14 2019-05-14 Method for preparing oxide film on surface of metal tantalum and application thereof Pending CN111945102A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113930712A (en) * 2021-09-29 2022-01-14 西安理工大学 Corrosion protection method for supercritical generator set

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2012021218A (en) * 2010-07-16 2012-02-02 Dowa Eco-System Co Ltd Method for recovering tantalum

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2012021218A (en) * 2010-07-16 2012-02-02 Dowa Eco-System Co Ltd Method for recovering tantalum

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113930712A (en) * 2021-09-29 2022-01-14 西安理工大学 Corrosion protection method for supercritical generator set
CN113930712B (en) * 2021-09-29 2024-03-22 西安理工大学 Supercritical generator set corrosion protection method

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