CN112226728B - Tungsten product with oxidation-resistant coating and preparation method thereof - Google Patents
Tungsten product with oxidation-resistant coating and preparation method thereof Download PDFInfo
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- CN112226728B CN112226728B CN202011102664.0A CN202011102664A CN112226728B CN 112226728 B CN112226728 B CN 112226728B CN 202011102664 A CN202011102664 A CN 202011102664A CN 112226728 B CN112226728 B CN 112226728B
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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
- C23C12/00—Solid state diffusion of at least one non-metal element other than silicon and at least one metal element or silicon into metallic material surfaces
- C23C12/02—Diffusion in one step
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
Abstract
The invention belongs to the field of tungsten product preparation, and relates to a tungsten product with an oxidation-resistant coating and a preparation method thereof. The method comprises the following steps: immersing a tungsten product substrate into an acid electrolyte, electrolyzing for 2-3 minutes under the protection of argon at the electrolytic pressure of 15-20V, ultrasonically cleaning and drying the tungsten product substrate, embedding the tungsten product substrate into a coating seepage material, and sequentially preserving heat at 700-750 ℃ for 5-10 hours and 900-1000 ℃ for 3-8 hours, wherein the coating seepage material contains 15-20 wt% of aluminum powder, 5-10 wt% of boron powder, 2-5 wt% of ammonium chloride, 2-5 wt% of sodium fluoride and the balance of aluminum oxide powder, and introducing argon for protection in the whole process. The method provided by the invention can obviously improve the oxidation resistance of the tungsten product, simultaneously can keep the strength and hardness of the tungsten product, can prevent the deformation of the metal tungsten product and keep the precision of the metal tungsten product.
Description
Technical Field
The invention belongs to the field of tungsten product preparation, and particularly relates to a tungsten product with an oxidation-resistant coating and a preparation method thereof.
Background
The metal tungsten belongs to refractory metal materials, has the advantages of high melting point, high strength, high hardness and the like, and is widely applied to the fields of modern industry and national defense and military industry. The metal tungsten and the alloy thereof have good high-temperature mechanical properties, but have poor high-temperature oxidation resistance, and under the condition of no protective measures, namely non-vacuum or non-protective atmosphere environment, the metal tungsten and the alloy thereof have serious oxidation phenomena at 650-700 ℃, and faint yellow oxides such as tungsten trioxide, tungsten dioxide and the like are formed on the surface of the metal tungsten and the alloy thereof, so that the performance of the metal tungsten and the alloy thereof is reduced, and the application range of the metal tungsten and the alloy thereof under the high-temperature condition is greatly limited.
The oxidation-resistant coating tungsten product, namely the oxidation-resistant coating is prepared on the surface of the metal tungsten, so that the oxidation resistance of the metal tungsten can be obviously improved, the use of the metal tungsten in an aerobic high-temperature environment is realized, and the high-temperature strength of the metal tungsten is maintained. At present, the preparation methods of the oxidation-resistant coating on the surface of the metal tungsten comprise a slurry method, an embedding infiltration method, a thermal spraying method, a plasma spraying method, physical/chemical vapor deposition and the like, and different coating preparation methods have advantages and are suitable for different working condition application environments. However, the above coating preparation methods all need to be carried out at a relatively high temperature, for example, the temperature required for preparing the coating by a slurry method is usually over 1200 ℃, and the temperature generated by thermal spraying and plasma spraying even reaches thousands of degrees. The preparation of the oxidation-resistant coating on the surface of the metal tungsten at an excessively high temperature can have adverse effects on the metal tungsten product, on one hand, the increase of the grain size of the tungsten and the obvious reduction of the hardness and the strength can be caused when the preparation temperature of the coating exceeds the recrystallization temperature (1150-1350 ℃) of the metal tungsten, on the other hand, the deformation and the reduction of the precision of the metal tungsten can be caused, and particularly, the influences on tungsten sheets, tungsten bars and the like are serious. In addition, coating preparation techniques such as slurry and embedding require the use of reactive activators, which can corrode the tungsten metal and deform at high temperatures.
Disclosure of Invention
The invention aims to overcome the defects that the strength and hardness of a tungsten product are reduced and the tungsten product is deformed due to the fact that an oxidation-resistant coating is prepared on the surface of the tungsten product by the existing method, and provides a tungsten product with the oxidation-resistant coating and a preparation method thereof.
Specifically, the invention provides a tungsten product with an oxidation-resistant coating, which comprises a tungsten product substrate and the oxidation-resistant coating attached to the surface of the tungsten product substrate, wherein the oxidation-resistant coating comprises a composite oxide of Al, B and W (hereinafter referred to as Al-B-W), the formation temperature of the oxidation-resistant coating is lower than the recrystallization temperature of metal tungsten, and the difference between the strength and the hardness of the tungsten product with the oxidation-resistant coating and the tungsten product substrate is not more than +/-3%.
Preferably, the thickness of the oxidation-resistant coating is 40-80 μm.
Preferably, the material of the tungsten product substrate is metal tungsten or tungsten alloy.
Preferably, the metal element other than tungsten in the tungsten alloy is selected from at least one of molybdenum, rhenium, tantalum, lanthanum and thorium.
Preferably, the tungsten product substrate is in the shape of a tungsten block, a tungsten sheet, a tungsten bar, a tungsten rod or other irregular shapes.
The invention also provides a preparation method of the tungsten product with the oxidation-resistant coating, which comprises the following steps:
s1, immersing the tungsten product substrate into an acid electrolyte, adding argon hydrofluoric acid, 15-20 vt% nitric acid and the balance of water, taking out the tungsten product substrate after the electrolysis is finished, and drying after ultrasonic cleaning to obtain a pretreated tungsten product substrate;
s2, embedding the pretreated tungsten product substrate into coating seeping materials, wherein the coating seeping materials contain 15-20 wt% of aluminum powder, 5-10 wt% of boron powder, 2-5 wt% of ammonium chloride, 2-5 wt% of sodium fluoride and the balance of alumina powder, then adding the coating seeping materials embedded with the pretreated tungsten product substrate into a heating furnace, heating to 700-750 ℃, preserving heat for 5-10 hours, then heating to 900-1000 ℃, preserving heat for 3-8 hours, introducing argon for protection in the whole process, and cooling to room temperature along with the furnace after the heat preservation is finished, thereby obtaining the tungsten product with the oxidation-resistant coating.
In the invention, the purpose of heating and heat preservation is divided into two stages: the first stage can achieve the effect of forming aluminum atoms and boron atoms through preferential reaction between the seeping materials, and avoid the corrosion of ammonium chloride and sodium fluoride on tungsten products; the second stage ensures that sufficient diffusion activation energy is provided to cause the aluminum atoms and boron atoms to diffuse toward the surface of the tungsten article to form an oxidation-resistant coating, thereby improving the oxidation resistance of the tungsten article without substantially affecting the strength and hardness and dimensional accuracy of the tungsten article.
Preferably, the temperature rise rate is 4-6 ℃/min.
Preferably, the material of the tungsten product substrate is metal tungsten or tungsten alloy.
Preferably, the metal element other than tungsten in the tungsten alloy is selected from at least one of molybdenum, rhenium, tantalum, lanthanum and thorium.
Preferably, the tungsten product substrate is in the shape of a tungsten block, a tungsten sheet, a tungsten bar, a tungsten rod or other irregular shapes.
In addition, the invention also provides a tungsten product with the oxidation-resistant coating prepared by the method.
The invention takes the composite oxide of Al, B and W as the oxidation resistant coating, and has good oxidation resistance at 700-900 ℃. The treatment temperature adopted by the invention is lower than the recrystallization temperature of the metal tungsten, the treatment temperature is low, the high-temperature deformation can be prevented, the recrystallization phenomenon can be avoided, and the strength, the hardness and the dimensional accuracy of the tungsten product can be kept.
In the preparation process of the tungsten product with the oxidation-resistant coating, on one hand, the tungsten product matrix is electrolyzed in an acid electrolyte containing 10-15 vt% of hydrofluoric acid, 15-20 vt% of nitric acid and the balance of water, so that the surface of the tungsten product matrix can be passivated, the corrosion effect of subsequent coating seeping materials on the surface of the tungsten product matrix is avoided, and the problem of corrosion deformation of the surface of the tungsten product matrix is solved; on the other hand, the purpose of embedding the tungsten product substrate after the electrolytic pretreatment into a coating material containing 15 to 20 wt% of aluminum powder, 5 to 10 wt% of boron powder, 2 to 5 wt% of ammonium chloride, 2 to 5 wt% of sodium fluoride and the balance being alumina powder, and performing a two-stage heat preservation treatment is to form an Al-B-W oxidation-resistant coating at a temperature lower than the recrystallization temperature of metallic tungsten, thereby improving the oxidation resistance of the tungsten product substrate without affecting the strength, hardness and dimensional accuracy of the tungsten product substrate.
The method has the advantages of simple process and low cost, can realize large-scale production, has no special requirements on the shape of the product, is particularly suitable for the production of tungsten products with complex shapes and the production of easily deformed tungsten products such as tungsten sheets, tungsten bars, tungsten rods and the like, and has wide industrial application prospect.
Drawings
FIG. 1 is a cross-sectional SEM image of a tungsten article having an oxidation-resistant coating made in example 1.
Fig. 2 is a surface SEM image of a tungsten article having an oxidation resistant coating prepared in example 1.
Detailed Description
The present invention will be described in detail below by way of examples. The examples of embodiments are intended to be illustrative of the invention and are not to be construed as limiting the invention. Those skilled in the art will recognize that the specific techniques or conditions, not specified in the examples, are according to the techniques or conditions described in the literature of the art or according to the product specification. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
Example 1
S1, placing the tungsten product matrix (tungsten bar, the material is metal tungsten) into an electrolyte composed of 10% hydrofluoric acid by volume, 20% nitric acid and the balance of distilled water, electrolyzing for 3 minutes under the electrolytic voltage of 15V, leading flowing argon gas to protect the whole process, taking out after the electrolysis, performing ultrasonic cleaning, and drying to obtain the pretreated tungsten product matrix.
S2, embedding the matrix of the tungsten product to be pretreated into coating seeping material consisting of 15% aluminum powder, 10% boron powder, 5% ammonium chloride, 2% sodium fluoride and the balance of aluminum oxide powder, putting the coating seeping material embedded with the matrix of the tungsten product to be pretreated into a heating furnace, heating the coating seeping material to 700 ℃ at the speed of 5 ℃/min, preserving the heat for 10 hours, heating the coating seeping material to 1000 ℃ at the speed of 5 ℃/min after the heat preservation is finished, preserving the heat for 3 hours, cooling the coating seeping material along with the furnace after the heat preservation is finished, leading to flowing argon gas for protection in the whole process, taking out the coating to carry out ultrasonic cleaning after the coating is cooled to room temperature, and obtaining the tungsten product with the oxidation-resistant coating.
Fig. 1 is a cross-sectional SEM image of a tungsten article having an oxidation-resistant coating. Fig. 2 is a surface SEM image of a tungsten article having an oxidation resistant coating. As can be seen from fig. 1, the tungsten product with the oxidation-resistant coating comprises a tungsten product substrate (tungsten substrate for short) and an oxidation-resistant coating attached to the surface of the tungsten product substrate, wherein the average thickness of the oxidation-resistant coating is 60 μm. The component of the oxidation-resistant coating is a composite oxide of Al, B and W. As can be seen from fig. 2, the oxidation-resistant coating surface was dense and no large through-cracks occurred. Compared with the tungsten product substrate, the tungsten product with the oxidation-resistant coating basically has no deformation, and the deformation rate is less than or equal to 0.5 percent.
Example 2
S1, placing a tungsten product matrix (tungsten sheet, tungsten alloy with the components of tungsten and molybdenum in a mass ratio of 90: 10) into an electrolyte composed of 15% by volume of hydrofluoric acid, 15% by volume of nitric acid and the balance of distilled water, electrolyzing for 3 minutes under an electrolytic voltage of 15V, introducing flowing argon gas for protection in the whole process, taking out after the electrolysis is finished, and performing ultrasonic cleaning and drying to obtain the pretreated tungsten product matrix.
S2, embedding the pretreated tungsten product substrate into a coating seeping material consisting of 20% of aluminum powder, 5% of boron powder, 3% of ammonium chloride, 5% of sodium fluoride and the balance of aluminum oxide powder, putting the coating seeping material embedded with the pretreated tungsten product substrate into a heating furnace, raising the temperature to 750 ℃ at the speed of 5 ℃/min, preserving the temperature for 5 hours, raising the temperature to 900 ℃ at the speed of 5 ℃/min after preserving the temperature, preserving the temperature for 8 hours, cooling along with the furnace after preserving the temperature, leading to flowing argon gas for protection in the whole process, taking out the coating after cooling to room temperature, and carrying out ultrasonic cleaning to obtain the tungsten product with the oxidation-resistant coating. The thickness of the oxidation-resistant coating was 50 μm as determined by SEM. Compared with the tungsten product, the tungsten product with the oxidation-resistant coating basically does not deform, and the deformation rate is less than or equal to 0.5 percent.
Example 3
S1, placing a tungsten product matrix (tungsten rod, tungsten alloy with the components of tungsten and rhenium in a mass ratio of 95: 5) into an electrolyte composed of 12% hydrofluoric acid by volume, 18% nitric acid by volume and the balance of distilled water, electrolyzing for 3 minutes under an electrolytic voltage of 15V, leading flowing argon gas to protect the whole process, taking out after the electrolysis is finished, and carrying out ultrasonic cleaning and drying to obtain the pretreated tungsten product matrix.
S2, embedding the matrix of the tungsten product to be pretreated into coating seeping material consisting of 16% aluminum powder, 8% boron powder, 5% ammonium chloride, 5% sodium fluoride and the balance of aluminum oxide powder, putting the coating seeping material embedded with the matrix of the tungsten product to be pretreated into a heating furnace, raising the temperature to 750 ℃ at the speed of 5 ℃/min, preserving the temperature for 5 hours, raising the temperature to 950 ℃ at the speed of 5 ℃/min after preserving the temperature, preserving the temperature for 5 hours, cooling along with the furnace after preserving the temperature, leading to flowing argon gas for protection in the whole process, taking out the coating after cooling to room temperature, and carrying out ultrasonic cleaning to obtain the tungsten product with the oxidation-resistant coating. The thickness of the oxidation-resistant coating was 75 μm as determined by SEM. Compared with the tungsten product substrate, the tungsten product with the oxidation-resistant coating basically has no deformation, and the deformation rate is less than or equal to 0.5 percent.
Comparative example 1
A tungsten article having an oxidation-resistant coating was produced by following the procedure of example 1 except that step S1 was not included, and the tungsten article substrate was directly embedded in the coating material to be subjected to a protective treatment, and the other conditions were the same as in example 1, to obtain a reference tungsten article having an oxidation-resistant coating comprising a tungsten article substrate and an oxidation-resistant coating having a composition of a composite oxide of Al, B and W adhered to the surface of the tungsten article substrate. According to SEM detection, the thickness of the oxidation-resistant coating is 120 microns, the tungsten product is obviously deformed, and the deformation rate is more than or equal to 5%.
Comparative example 2
A tungsten article having an oxidation-resistant coating was produced by following the method of example 1 except that, in step S2, the heat-retaining treatment was carried out in two stages, but the heat-retaining treatment was carried out directly at 1200 ℃ for 13 hours, and the other conditions were the same as in example 1, to obtain a reference tungsten article having an oxidation-resistant coating comprising a tungsten article substrate and an oxidation-resistant coating having a composition of a composite oxide of Al, B and W adhered to the surface of the tungsten article substrate. According to SEM detection, the thickness of the oxidation-resistant coating is 210 microns, the surface of the coating is loose and porous, large cracks exist, the deformation of the tungsten product is serious, and the deformation rate is more than or equal to 8%.
Test example
(1) Strength:
the tungsten products with oxidation-resistant coatings obtained in examples 1 to 3 and the reference tungsten products with oxidation-resistant coatings obtained in comparative examples 1 to 2 were tested for strength according to the method of GB/T228.2-2015, the results of which are given in Table 1;
(2) hardness:
the hardness of the tungsten products with oxidation-resistant coatings obtained in examples 1 to 3 and the reference tungsten products with oxidation-resistant coatings obtained in comparative examples 1 to 2 were measured using an FM-ARS9000 microhardness tester, the results of which are shown in table 1;
(3) oxidation resistance:
the oxidation resistance of the tungsten products with oxidation-resistant coatings obtained in examples 1 to 3 and the reference tungsten products with oxidation-resistant coatings obtained in comparative examples 1 to 2 were tested according to the method of GB/T13303-91, and the results are shown in Table 1.
TABLE 1
From the above results, it can be seen that the method provided by the present invention can significantly improve the oxidation resistance of the tungsten article, while maintaining the strength and hardness of the tungsten article, and can prevent the deformation of the tungsten article, maintaining the accuracy thereof.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made in the above embodiments by those of ordinary skill in the art without departing from the principle and spirit of the present invention.
Claims (9)
1. A tungsten article having an oxidation-resistant coating comprising a tungsten article substrate and an oxidation-resistant coating adhered to a surface of the tungsten article substrate, wherein the oxidation-resistant coating comprises an Al-B-W composite oxide, wherein the oxidation-resistant coating is formed at a temperature below the recrystallization temperature of metallic tungsten, and wherein the tungsten article having the oxidation-resistant coating does not differ from the tungsten article substrate in strength or hardness by more than + -3%.
2. The tungsten article having an oxidation-resistant coating according to claim 1, wherein the oxidation-resistant coating has a thickness of 40 to 80 μm.
3. The tungsten article having an oxidation-resistant coating according to claim 1, wherein the material of the tungsten article substrate is metallic tungsten or a tungsten alloy; the metal element other than tungsten in the tungsten alloy is at least one selected from molybdenum, rhenium, tantalum, lanthanum and thorium.
4. The tungsten article having an oxidation-resistant coating according to claim 1, wherein the tungsten article substrate is in the shape of a tungsten block, a tungsten sheet, a tungsten bar, a tungsten rod, or other irregular shape.
5. A method of making a tungsten article having an oxidation-resistant coating, the method comprising:
s1, immersing the tungsten product substrate into an acid electrolyte, electrolyzing for 2-3 minutes under the protection of argon at an electrolytic pressure of 15-20V, wherein the electrolyte contains 10-15% of hydrofluoric acid by volume, 15-20% of nitric acid by volume and the balance of water, taking out the tungsten product substrate after the electrolysis is finished, and drying after ultrasonic cleaning to obtain a pretreated tungsten product substrate;
s2, embedding the pretreated tungsten product substrate into coating seeping materials, wherein the coating seeping materials contain 15-20 wt% of aluminum powder, 5-10 wt% of boron powder, 2-5 wt% of ammonium chloride, 2-5 wt% of sodium fluoride and the balance of alumina powder, then adding the coating seeping materials embedded with the pretreated tungsten product substrate into a heating furnace, heating to 700-750 ℃, preserving heat for 5-10 hours, then heating to 900-1000 ℃, preserving heat for 3-8 hours, introducing argon for protection in the whole process, and cooling to room temperature along with the furnace after the heat preservation is finished, thereby obtaining the tungsten product with the oxidation-resistant coating.
6. The method for preparing the tungsten product with the oxidation-resistant coating according to claim 5, wherein the temperature rise rate is 4-6 ℃/min.
7. The method according to claim 5 or 6, wherein the tungsten product substrate is made of metal tungsten or tungsten alloy; the metal element other than tungsten in the tungsten alloy is at least one selected from molybdenum, rhenium, tantalum, lanthanum and thorium.
8. The method of claim 5 or 6, wherein the tungsten article substrate is in the shape of a tungsten block, a tungsten sheet, a tungsten bar, a tungsten rod, or other irregular shape.
9. A tungsten article having an oxidation resistant coating produced by the method of any one of claims 5 to 8.
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| CN105385987B (en) * | 2015-10-15 | 2018-11-13 | 厦门理工学院 | Tungsten surface high-temp anti oxidation layer and preparation method thereof |
| CN107805777B (en) * | 2017-09-19 | 2020-05-15 | 昆明理工大学 | Tungsten-boron layered material with ray and neutron comprehensive shielding effect |
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| CN109881146A (en) * | 2019-04-16 | 2019-06-14 | 合肥工业大学 | A kind of preparation method of the modified pure tungsten pack cementation aluminizing antioxidant coating of rare earth element y |
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