CN107523801A - The method that in-situ chemical vapor deposition method prepares silicified molybdenum coating on molybdenum-base alloy surface - Google Patents
The method that in-situ chemical vapor deposition method prepares silicified molybdenum coating on molybdenum-base alloy surface Download PDFInfo
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- CN107523801A CN107523801A CN201610452635.4A CN201610452635A CN107523801A CN 107523801 A CN107523801 A CN 107523801A CN 201610452635 A CN201610452635 A CN 201610452635A CN 107523801 A CN107523801 A CN 107523801A
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- molybdenum
- base alloy
- vapor deposition
- chemical vapor
- coating
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/42—Silicides
Abstract
This application discloses a kind of method that in-situ chemical vapor deposition method prepares silicified molybdenum coating on molybdenum-base alloy surface, including step:(1), silica flour, sodium fluoride and aluminum oxide are mixed, are placed in batch mixing 20~24 hours in ball mill, obtains powder feed;(2), molybdenum-base alloy is surface-treated, successively including sandblasting, ultrasonic wave cleaning, oil removing;(3), powder feed and molybdenum-base alloy are placed in tube furnace, is pre-processed 10~12 hours at 900~1000 DEG C, is cooled to room temperature, then ultrasonic wave is cleaned and dried, and molybdenum disilicide layer is prepared on Mo substrate surface.The molybdenum disilicide layer that the present invention obtains on molybdenum-base alloy surface, there is good antioxygenic property, service life length, the diffusion between coating and matrix can be delayed.
Description
Technical field
The application is related to a kind of in-situ chemical vapor deposition method and prepares silicified molybdenum coating on molybdenum-base alloy surface
Method.
Background technology
Metal molybdenum and its alloy have the advantages that high intensity, high-melting-point, corrosion-resistant and wear-resistant, by with
In the alloy components and parts that manufacture warship, tank, firearms, rocket, satellite.In addition metal molybdenum and
Its alloy is also often used to manufacture the heater and structural material of high temperature furnace, such as in glass and refractory fibre work
Industry is used as the electrode and glass melting high-temperature structural material of smelting furnace, and electrode and smelting are used as in rare-earth industry
With stirring rod etc..
Although metal molybdenum and its alloy are the materials for preparing high-temperature furnace heating body and structural member well,
In air at more than 600 DEG C will vigorous oxidation, with the rise of temperature, the intensity of its product declines, damage
Consumption aggravation, performance are affected, and this seriously constrains the application of molybdenum and its alloy.At present both at home and abroad
Substantial amounts of research is carried out to the antioxidant defense method of metal and alloy, the results showed that improve metal and conjunction
The main path of the high-temperature oxidation resistance of gold has alloying protection and face coat protection.Alloying is typically
To lose intensity and processing characteristics as cost, and add Effect on Mechanical Properties very little of the coating to alloy, and energy
Inoxidizability is significantly improved, experiment is proved to be practicable approach.
In actual use, in order to ensure molybdenum and its alloy use at high temperature, and increase the service life,
Economize on resources, reduce cost, reduce the purpose of pollution, it is necessary to which high-temperature oxidation resistant protection is carried out to it.Cause
This, it is most important to develop the high-temperature oxidation resistant coating to match therewith.
Embedding cementation process has been widely used in metal and alloy surface prepares protective coating to adapt to height
The requirement of warm environment.This technique preparation is simple, cost is cheap, and is that viable commercial diffusion applies
Layer preparation technology.
The content of the invention
It is an object of the invention to provide a kind of in-situ chemical vapor deposition method two are prepared on molybdenum-base alloy surface
The method of silication molybdenum coating, to overcome deficiency of the prior art.
To achieve the above object, the present invention provides following technical scheme:
The embodiment of the present application discloses a kind of in-situ chemical vapor deposition method and prepares two silication on molybdenum-base alloy surface
The method of molybdenum coating, including step:
(1), silica flour, sodium fluoride and aluminum oxide are mixed, are placed in batch mixing 20~24 hours in ball mill,
Obtain powder feed;
(2), molybdenum-base alloy is surface-treated, successively including sandblasting, ultrasonic wave cleaning, oil removing;
(3), powder feed and molybdenum-base alloy are placed in tube furnace, 10~12 are pre-processed at 900~1000 DEG C
Hour, room temperature is cooled to, then ultrasonic wave is cleaned and dried, and two silication are prepared on Mo substrate surface
Molybdenum layer.
Preferably, molybdenum disilicide is prepared on molybdenum-base alloy surface in above-mentioned in-situ chemical vapor deposition method to apply
In the method for layer, in step (1), 20~25wt.% of silicone content, 5~7wt.% of fluorination sodium content.
Preferably, molybdenum disilicide is prepared on molybdenum-base alloy surface in above-mentioned in-situ chemical vapor deposition method to apply
In the method for layer, in step (1), silicone content 25wt.%, sodium content 5wt.%, alumina content are fluorinated
70wt.%.
Preferably, molybdenum disilicide is prepared on molybdenum-base alloy surface in above-mentioned in-situ chemical vapor deposition method to apply
In the method for layer, in step (3), 900~1000 DEG C are warming up to 7~10 DEG C/min heating rate.
Preferably, molybdenum disilicide is prepared on molybdenum-base alloy surface in above-mentioned in-situ chemical vapor deposition method to apply
In the method for layer, in step (2), blasting method includes:With the corundum sand that granularity is 0.7~1.0mm
Blasting treatment is carried out in the case where pressure is 0.6~0.8MPa compressed air, to remove the oxygen on molybdenum-base alloy surface
Change skin and cause matrix surface to reach roughening.
Compared with prior art, the advantage of the invention is that:The present invention molybdenum-base alloy surface obtain two
Molybdenum silicide layer, there is good antioxygenic property, service life length, can delay between coating and matrix
Diffusion.
Embodiment
The present invention is described further by the following example:, can be more preferably geographical according to following embodiments
The solution present invention.However, as it will be easily appreciated by one skilled in the art that specific material described by embodiment
The present invention is merely to illustrate than, process conditions and its result, without should be also without limitation on claims
In the described in detail present invention.
Embodiment 1
The method that in-situ chemical vapor deposition method prepares silicified molybdenum coating on molybdenum-base alloy surface
(1), silica flour, sodium fluoride and aluminum oxide are mixed, are placed in batch mixing 24 hours in ball mill, is obtained
Powder feed, wherein silicone content 25wt.%, it is fluorinated sodium content 5wt.%, alumina content 70wt.%;
(2), molybdenum-base alloy is surface-treated, successively including sandblasting, ultrasonic wave cleaning, oil removing;
(3), powder feed and molybdenum-base alloy are placed in tube furnace, with 10 DEG C/min heating rate liter
Warm to 900~1000 DEG C pre-process 12 hours, are cooled to room temperature, then ultrasonic wave is cleaned and dried, in molybdenum
Molybdenum disilicide layer is prepared in matrix surface.
In step (2), blasting method includes:The corundum sand for being 0.7~1.0mm with granularity is in pressure
Blasting treatment is carried out under 0.6~0.8MPa compressed air, to remove the oxide skin on molybdenum-base alloy surface and make
Obtain matrix surface and reach roughening.
Embodiment 2
The method that in-situ chemical vapor deposition method prepares silicified molybdenum coating on molybdenum-base alloy surface
(1), silica flour, sodium fluoride and aluminum oxide are mixed, are placed in batch mixing 24 hours in ball mill, is obtained
Powder feed, wherein silicone content 20wt.%, it is fluorinated sodium content 5wt.%, alumina content 75wt.%;
(2), molybdenum-base alloy is surface-treated, successively including sandblasting, ultrasonic wave cleaning, oil removing;
(3), powder feed and molybdenum-base alloy are placed in tube furnace, with 10 DEG C/min heating rate liter
Warm to 900~1000 DEG C pre-process 12 hours, are cooled to room temperature, then ultrasonic wave is cleaned and dried, in molybdenum
Molybdenum disilicide layer is prepared in matrix surface.
In step (2), blasting method includes:The corundum sand for being 0.7~1.0mm with granularity is in pressure
Blasting treatment is carried out under 0.6~0.8MPa compressed air, to remove the oxide skin on molybdenum-base alloy surface and make
Obtain matrix surface and reach roughening.
Embodiment 3
The method that in-situ chemical vapor deposition method prepares silicified molybdenum coating on molybdenum-base alloy surface
(1), silica flour, sodium fluoride and aluminum oxide are mixed, are placed in batch mixing 24 hours in ball mill, is obtained
Powder feed, wherein silicone content 25wt.%, it is fluorinated sodium content 5wt.%, alumina content 70wt.%;
(2), molybdenum-base alloy is surface-treated, successively including sandblasting, ultrasonic wave cleaning, oil removing;
(3), powder feed and molybdenum-base alloy are placed in tube furnace, heated up with 7 DEG C/min heating rate
Pre-processed 10 hours to 900~1000 DEG C, be cooled to room temperature, then ultrasonic wave is cleaned and dried, in molybdenum base
Molybdenum disilicide layer is prepared in body surface face.
In step (2), blasting method includes:The corundum sand for being 0.7~1.0mm with granularity is in pressure
Blasting treatment is carried out under 0.6~0.8MPa compressed air, to remove the oxide skin on molybdenum-base alloy surface and make
Obtain matrix surface and reach roughening.
Finally, it is to be noted that, term " comprising ", "comprising" or its any other variant are intended to
Nonexcludability includes, so that process, method, article or equipment including a series of elements are not
Only include those key elements, but also the other element including being not expressly set out, or it is this also to include
Kind of process, method, article or the intrinsic key element of equipment.
Claims (5)
1. a kind of method that in-situ chemical vapor deposition method prepares silicified molybdenum coating on molybdenum-base alloy surface,
It is characterised in that it includes step:
(1), silica flour, sodium fluoride and aluminum oxide are mixed, are placed in batch mixing 20~24 hours in ball mill,
Obtain powder feed;
(2), molybdenum-base alloy is surface-treated, successively including sandblasting, ultrasonic wave cleaning, oil removing;
(3), powder feed and molybdenum-base alloy are placed in tube furnace, 10~12 are pre-processed at 900~1000 DEG C
Hour, room temperature is cooled to, then ultrasonic wave is cleaned and dried, and two silication are prepared on Mo substrate surface
Molybdenum layer.
2. in-situ chemical vapor deposition method according to claim 1 prepares two silicon on molybdenum-base alloy surface
Change the method for molybdenum coating, it is characterised in that:In step (1), 20~25wt.% of silicone content, sodium fluoride contains
Measure 5~7wt.%.
3. in-situ chemical vapor deposition method according to claim 2 prepares two silicon on molybdenum-base alloy surface
Change the method for molybdenum coating, it is characterised in that:In step (1), silicone content 25wt.%, sodium content is fluorinated
5wt.%, alumina content 70wt.%.
4. in-situ chemical vapor deposition method according to claim 1 prepares two silicon on molybdenum-base alloy surface
Change the method for molybdenum coating, it is characterised in that:In step (3), heated up with 7~10 DEG C/min heating rate
To 900~1000 DEG C.
5. in-situ chemical vapor deposition method according to claim 1 prepares two silicon on molybdenum-base alloy surface
Change the method for molybdenum coating, it is characterised in that:In step (2), blasting method includes:It is 0.7~1.0mm with granularity
Corundum sand pressure be 0.6~0.8MPa compressed air under carry out blasting treatment, with remove molybdenum base conjunction
The oxide skin of gold surface simultaneously causes matrix surface to reach roughening.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109666886A (en) * | 2018-12-28 | 2019-04-23 | 河南科技大学 | A kind of preparation method of molybdenum base material surface oxidation-resistant coating |
CN112144011A (en) * | 2020-08-14 | 2020-12-29 | 重庆材料研究院有限公司 | Method for preparing anti-oxidation coating on surface of molybdenum and molybdenum alloy protection tube |
Citations (2)
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CN1843998A (en) * | 2006-04-24 | 2006-10-11 | 浙江大学 | Titanium silicide nano-nail prepared by chemical vapor deposition under normal pressure and preparation method thereof |
CN103132005A (en) * | 2011-12-05 | 2013-06-05 | 湖南科技大学 | Molybdenum disilicide based abrasion-resisting composite coating and manufacture method thereof |
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2016
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Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN1843998A (en) * | 2006-04-24 | 2006-10-11 | 浙江大学 | Titanium silicide nano-nail prepared by chemical vapor deposition under normal pressure and preparation method thereof |
CN103132005A (en) * | 2011-12-05 | 2013-06-05 | 湖南科技大学 | Molybdenum disilicide based abrasion-resisting composite coating and manufacture method thereof |
Non-Patent Citations (1)
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109666886A (en) * | 2018-12-28 | 2019-04-23 | 河南科技大学 | A kind of preparation method of molybdenum base material surface oxidation-resistant coating |
CN112144011A (en) * | 2020-08-14 | 2020-12-29 | 重庆材料研究院有限公司 | Method for preparing anti-oxidation coating on surface of molybdenum and molybdenum alloy protection tube |
CN112144011B (en) * | 2020-08-14 | 2023-06-06 | 重庆材料研究院有限公司 | Method for preparing antioxidation coating on surface of molybdenum and molybdenum alloy protection tube |
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Application publication date: 20171229 |