CN109321874A - A kind of preparation method of pure tungsten surface sial permeation anti-oxidation composite coating - Google Patents
A kind of preparation method of pure tungsten surface sial permeation anti-oxidation composite coating Download PDFInfo
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- CN109321874A CN109321874A CN201811464673.7A CN201811464673A CN109321874A CN 109321874 A CN109321874 A CN 109321874A CN 201811464673 A CN201811464673 A CN 201811464673A CN 109321874 A CN109321874 A CN 109321874A
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- powder
- pure tungsten
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- coating
- sial
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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
- C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
- C23C10/28—Solid state diffusion of only metal elements or silicon into metallic material surfaces using solids, e.g. powders, pastes
- C23C10/34—Embedding in a powder mixture, i.e. pack cementation
- C23C10/52—Embedding in a powder mixture, i.e. pack cementation more than one element being diffused in one step
-
- 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
- C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
- C23C10/02—Pretreatment of the material to be coated
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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
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Abstract
The invention discloses a kind of preparation methods of pure tungsten surface sial permeation anti-oxidation composite coating, can effectively extend the service life of pure tungsten in the high temperature environment using pack cementation technology.The coating of different-thickness is obtained by control penetration enhancer ingredient, permeation temperature and time etc., coating surface richness Al, Si generates continuous fine and close Al in the high temperature environment2O3Phase, SiO2It is equal, to delay the degeneration of coating, show good high temperature oxidation resistance.
Description
Technical field
The invention belongs to refractory metal surfaces method of modifying technical fields, and in particular to a kind of pure tungsten surface sial permeation is anti-
Aoxidize the preparation method of composite coating.
Background technique
Refractory metals tungsten has fusing point high, is with a wide range of applications in controlled thermonuclear fusion energy field.However pure tungsten
It is easily oxidized in 400 DEG C or more of hot environment, seriously constrains its use as high-temperature material.Currently, common
Anti-oxidant means have alloying and surface treatment.In comparison, alloyage process improvement high-temperature oxidation resistance has certain
Limitation, usually to lose intensity and processing performance as cost, and surface protection coating to the Effect on Mechanical Properties of metal very
It is small, and the antioxygenic property of matrix can be significantly improved.Therefore, on pure tungsten surface, preparation antioxidant coating is that raising pure tungsten is anti-oxidant
The feasible way of performance.
Sial compound coating has fusing point height, thermal stability good, the excellent feature of antioxygenic property, the height suitable for alloy
Warm antioxidant defense.Embedding cementation process is a kind of chemical heat treatment technology, is basis material to be embedded in inert filler, metal
The packet of coating element and halide activators composition seeps in case, is heat-treated in an inert atmosphere, by neatly migrating and
Diffusion is to form coating.It is metallurgical bonding between coating and parent metal, thus very securely, not easily to fall off, this is other coatings
Less than method.
Currently, the technology of preparing and its application of sial compound infiltration layer resistant to high temperatures are prepared on pure tungsten surface by pack cementation method
Still belong to blank.Therefore, study and realize the technology of preparing of the sial compound coating of pure tungsten surface oxidation-resistant to pure tungsten high-temperature material
It is of great significance on engineer application.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of pure tungsten surface sial permeation anti-oxidation composite coating, can
Significantly improve the antioxygenic property of composite coating.
The preparation method of sial permeation anti-oxidation composite coating in pure tungsten surface of the present invention, specifically comprises the following steps:
Step 1: the pre-treatment of matrix
Pure tungsten matrix is passed through 120#、240#、400#、600#With 1000#Carborundum paper is polished step by step, is cleaned by ultrasonic and is dried
The smooth pure tungsten sample of surface cleaning is obtained after dry；
Step 2: preparing embedding penetration enhancer
It is put into planetary ball mill after aluminium powder, silicon powder, fluorination sodium powder, alumina powder are mixed uniformly mixed and thin
Change, obtains embedding penetration enhancer；
In step 2, aluminium powder, silicon powder, fluorination sodium powder and the purity of alumina powder are not less than 99.0%；
In step 2, aluminium powder, silicon powder, fluorination sodium powder and the proportion of alumina powder are constituted according to mass percent are as follows: aluminium powder
0-30%, silicon powder 0-30% are fluorinated sodium powder 1-5%, alumina powder 65-80%.
In step 2, drum's speed of rotation is 200-500 revs/min, ratio of grinding media to material 10:1, Ball-milling Time 2-6h, ball grinder
It is tungsten carbide with Material quality of grinding balls.
Step 3: sial permeation
Pure tungsten sample is embedded in the Noah's ark equipped with embedding penetration enhancer and seals Noah's ark, is first evacuated to high temperature process furnances
Interior air pressure is to 0.02MPa hereinafter, being filled with argon gas into high temperature process furnances again to atmospheric pressure, control high-temperature tubular furnace temperature is 800-
It 1200 DEG C, soaking time 3-10h, cools to the furnace after room temperature and obtains Al-Si coating in pure tungsten specimen surface.
The beneficial effects of the present invention are:
1, high-temperature oxidation resistant coating stable preparation process prepared by the present invention is reliable, layer surface even tissue, densification.
2, the present invention can effectively extend the service life of pure tungsten in the high temperature environment using pack cementation technology.Coating surface is rich
Al, Si generate continuous fine and close Al in the high temperature environment2O3Phase, SiO2It is equal, to delay the degeneration of coating, show good
High temperature oxidation resistance.
3, the coating of different-thickness, simple process and repetition be can get by control penetration enhancer ingredient, permeation temperature and time
Property it is good, can be used for the preparation of industrial large area.
Detailed description of the invention
Fig. 1 is the surface topography map of the high-temperature oxidation resistant coating prepared using preparation method of the invention.As shown in Figure 1,
The Al-Si high-temperature oxidation resistant coating surface that the present invention prepares is in cell structure, surface compact, flawless, hole phenomenon.
Fig. 2 is the Cross Section Morphology figure of the high-temperature oxidation resistant coating prepared using preparation method of the invention.As shown in Figure 2,
Coating cross sections mainly contain infiltration layer and matrix, are tightly combined between infiltration layer and substrate.
Fig. 3 is that the high-temperature oxidation resistant coating prepared using preparation method of the invention aoxidizes the section shape of 10h at 1000 DEG C
Looks.From the figure 3, it may be seen that after 1000 DEG C of oxidation 10h, the fine and close continuous SiO of the Surface Creation of composite coating2Film, and SiO2Film with
There is obvious line of demarcation between composite coating, without obscission between coating and matrix, is well combined.
Fig. 4 is the oxidation weight gain curve for aoxidizing 15h at 1000 DEG C using substrate of the present invention and the sample of prepares coating.By scheming
4 it is found that the 45.96mg/cm that increases weight after 1 sample of embodiment, 1000 DEG C of oxidation 15h2, increase after 2 sample of embodiment, 1000 DEG C of oxidation 15h
Weight is 41.50mg/cm2, and pure tungsten substrate is 282.81mg/cm by 1000 DEG C of oxidation 15h weight gains2, illustrate the sample containing coating
High-temperature oxidation resistance is good, and oxidation weight gain is only 1/5 or so of pure tungsten substrate.
Specific embodiment
Embodiment 1:
In the present embodiment pure tungsten surface A l-Si permeation high-temperature oxidation resistant coating the preparation method is as follows:
Step 1: the pre-treatment of matrix
Pure tungsten matrix is passed through 120#、240#、400#、600#With 800#Carborundum paper is polished step by step, and ultrasonic cleaning is dried
The smooth pure tungsten sample of surface cleaning is obtained after dry；
Step 2: configuration embedding penetration enhancer
It is silicon powder 30% by the mass fraction of each component, is fluorinated sodium powder 3%, alumina powder 67%, by above-mentioned each component
The ball milling 4h in 300 revs/min of planetary ball mill obtains embedding penetration enhancer；Wherein, aluminium powder, silicon powder, fluorination sodium powder, oxidation
The purity of aluminium powder is not less than 99.0%；
Step 3: sial permeation
Pure tungsten sample is embedded in the Noah's ark equipped with embedding penetration enhancer and seals Noah's ark, is first evacuated to high temperature process furnances
To 0.1MPa hereinafter, being filled with argon gas into high temperature process furnances to atmospheric pressure, control high-temperature tubular furnace temperature is 800 DEG C for interior air pressure,
Soaking time is 10h, cools to the furnace after room temperature and obtains Al-Si coating in pure tungsten specimen surface.
Embodiment 2:
In the present embodiment pure tungsten surface A l-Si permeation high-temperature oxidation resistant coating the preparation method is as follows:
Step 1: the pre-treatment of matrix
Pure tungsten matrix is passed through 120#、240#、400#、600#With 800#Carborundum paper is polished step by step, and ultrasonic cleaning is dried
The smooth pure tungsten sample of surface cleaning is obtained after dry；
Step 2: configuration embedding penetration enhancer
It is aluminium powder 30% by the mass fraction of each component, is fluorinated sodium powder 3%, alumina powder 67%, by above-mentioned each component
The ball milling 4h in 300 revs/min of planetary ball mill obtains embedding penetration enhancer；Wherein, aluminium powder, silicon powder, fluorination sodium powder, oxidation
The purity of aluminium powder is not less than 99.0%；
Step 3: sial permeation
Pure tungsten sample is embedded in the Noah's ark equipped with embedding penetration enhancer and seals Noah's ark, is first evacuated to high temperature process furnances
To 0.1MPa hereinafter, being filled with argon gas into high temperature process furnances to atmospheric pressure, control high-temperature tubular furnace temperature is 1000 DEG C for interior air pressure,
Soaking time is 5h, cools to the furnace after room temperature and obtains Al-Si coating in pure tungsten specimen surface.
Embodiment 3:
In the present embodiment pure tungsten surface A l-Si permeation high-temperature oxidation resistant coating the preparation method is as follows:
Step 1: the pre-treatment of matrix
Pure tungsten matrix is passed through 120#、240#、400#、600#With 800#Carborundum paper is polished step by step, and ultrasonic cleaning is dried
The smooth pure tungsten sample of surface cleaning is obtained after dry；
Step 2: configuration embedding penetration enhancer
It is aluminium powder 20% by the mass fraction of each component, silicon powder 10% is fluorinated sodium powder 3%, and alumina powder 67% will be upper
Each component ball milling 4h in 300 revs/min of planetary ball mill is stated, embedding penetration enhancer is obtained；Wherein, aluminium powder, silicon powder, sodium fluoride
Powder, alumina powder purity be not less than 99.0%；
Step 3: sial permeation
Pure tungsten sample is embedded in the Noah's ark equipped with embedding penetration enhancer and seals Noah's ark, is first evacuated to high temperature process furnances
To 0.1MPa hereinafter, being filled with argon gas into high temperature process furnances to atmospheric pressure, control high-temperature tubular furnace temperature is 1200 DEG C for interior air pressure,
Soaking time is 3h, cools to the furnace after room temperature and obtains Al-Si coating in pure tungsten specimen surface.
Claims (5)
1. a kind of preparation method of pure tungsten surface sial permeation anti-oxidation composite coating, it is characterised in that include the following steps:
Step 1: the pre-treatment of matrix
Pure tungsten matrix is polished by carborundum paper, is cleaned by ultrasonic and obtains the smooth pure tungsten sample of surface cleaning after drying；
Step 2: preparing embedding penetration enhancer
It is put into after aluminium powder, silicon powder, fluorination sodium powder, alumina powder are mixed and is uniformly mixed and refines in planetary ball mill, obtained
To embedding penetration enhancer；
Step 3: sial permeation
Pure tungsten sample is embedded in the Noah's ark equipped with embedding penetration enhancer and seals Noah's ark, is first evacuated to gas in high temperature process furnances
0.02MPa is depressed into hereinafter, being filled with argon gas into high temperature process furnances again to atmospheric pressure, control high-temperature tubular furnace temperature is 800-1200
DEG C, soaking time 3-10h is cooled to the furnace after room temperature and is obtained Al-Si coating in pure tungsten specimen surface.
2. preparation method according to claim 1, it is characterised in that:
In step 1, pure tungsten matrix is passed through 120#、240#、400#、600#With 1000#Carborundum paper is polished step by step.
3. preparation method according to claim 1, it is characterised in that:
In step 2, aluminium powder, silicon powder, fluorination sodium powder and the purity of alumina powder are not less than 99.0%.
4. preparation method according to claim 1, it is characterised in that:
In step 2, aluminium powder, silicon powder, fluorination sodium powder and the proportion of alumina powder are constituted according to mass percent are as follows: aluminium powder 0-
30%, silicon powder 0-30% are fluorinated sodium powder 1-5%, alumina powder 65-80%.
5. preparation method according to claim 1, it is characterised in that:
In step 2, drum's speed of rotation is 200-500 revs/min, ratio of grinding media to material 10:1, Ball-milling Time 2-6h, ball grinder and mill
Ball material is tungsten carbide.
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| CN201811464673.7A CN109321874A (en) | 2018-12-03 | 2018-12-03 | A kind of preparation method of pure tungsten surface sial permeation anti-oxidation composite coating |
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| CN201811464673.7A CN109321874A (en) | 2018-12-03 | 2018-12-03 | A kind of preparation method of pure tungsten surface sial permeation anti-oxidation composite coating |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110257764A (en) * | 2019-07-16 | 2019-09-20 | 合肥工业大学 | A kind of preparation method of the compound resistance tritium coating of 316L stainless steel surface Al-Si co-infiltrating oxide |
| CN112226728A (en) * | 2020-10-15 | 2021-01-15 | 厦门理工学院 | Tungsten product with oxidation-resistant coating and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108642439A (en) * | 2018-06-05 | 2018-10-12 | 合肥工业大学 | A method of preparing high-strength coating in tungsten alitizing |
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2018
- 2018-12-03 CN CN201811464673.7A patent/CN109321874A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108642439A (en) * | 2018-06-05 | 2018-10-12 | 合肥工业大学 | A method of preparing high-strength coating in tungsten alitizing |
Non-Patent Citations (2)
| Title |
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| 利亚霍维奇: "《金属和合金的化学热处理手册》", 31 May 1985, 上海科学技术出版社 * |
| 里霍维奇: "《多元共渗》", 31 August 1983, 机械工业出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110257764A (en) * | 2019-07-16 | 2019-09-20 | 合肥工业大学 | A kind of preparation method of the compound resistance tritium coating of 316L stainless steel surface Al-Si co-infiltrating oxide |
| CN112226728A (en) * | 2020-10-15 | 2021-01-15 | 厦门理工学院 | Tungsten product with oxidation-resistant coating and preparation method thereof |
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Application publication date: 20190212 |