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 PDF

Info

Publication number
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
Authority
CN
China
Prior art keywords
molybdenum
base alloy
vapor deposition
chemical vapor
coating
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201610452635.4A
Other languages
Chinese (zh)
Inventor
范佳晨
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Zhangjiagang Si Jie Hardware Tools Co Ltd
Original Assignee
Zhangjiagang Si Jie Hardware Tools Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Zhangjiagang Si Jie Hardware Tools Co Ltd filed Critical Zhangjiagang Si Jie Hardware Tools Co Ltd
Priority to CN201610452635.4A priority Critical patent/CN107523801A/en
Publication of CN107523801A publication Critical patent/CN107523801A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22Chemical 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
    • C23C16/30Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/42Silicides

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

The method that in-situ chemical vapor deposition method prepares silicified molybdenum coating on molybdenum-base alloy surface
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.
CN201610452635.4A 2016-06-21 2016-06-21 The method that in-situ chemical vapor deposition method prepares silicified molybdenum coating on molybdenum-base alloy surface Pending CN107523801A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610452635.4A CN107523801A (en) 2016-06-21 2016-06-21 The method that in-situ chemical vapor deposition method prepares silicified molybdenum coating on molybdenum-base alloy surface

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610452635.4A CN107523801A (en) 2016-06-21 2016-06-21 The method that in-situ chemical vapor deposition method prepares silicified molybdenum coating on molybdenum-base alloy surface

Publications (1)

Publication Number Publication Date
CN107523801A true CN107523801A (en) 2017-12-29

Family

ID=60735290

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610452635.4A Pending CN107523801A (en) 2016-06-21 2016-06-21 The method that in-situ chemical vapor deposition method prepares silicified molybdenum coating on molybdenum-base alloy surface

Country Status (1)

Country Link
CN (1) CN107523801A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
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

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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)

* Cited by examiner, † Cited by third party
Title
汪异: "钼基合金高温抗氧化涂层的制备及其性能研究", 《中国博士学位论文全文数据库 工程科技Ⅰ辑》 *

Cited By (3)

* Cited by examiner, † Cited by third party
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

Similar Documents

Publication Publication Date Title
CN107523785A (en) Molybdenum-base alloy surface oxidation-resistant coating and preparation method thereof
CN110117765B (en) TiO 2 2 Base electrothermal coating and preparation method thereof
CN108067407B (en) Antibacterial non-stick material, preparation method thereof and antibacterial non-stick cookware
CN104532229B (en) Ceramic coating for pot and preparation method thereof
CN106587629B (en) Boride modified glass ceramic base combined high temperature antioxidant coating and preparation method thereof
CN104694863B (en) A kind of heat treatment method of titanium alloy
CN107523801A (en) The method that in-situ chemical vapor deposition method prepares silicified molybdenum coating on molybdenum-base alloy surface
CN102503176A (en) Method for increasing strength of transparent electropane
CN103420622A (en) Preparation method of metal-glass composite material and processing system using the same
CN104846307A (en) High-temperature resistant ceramic coating for metal based hot spraying and spraying method of coating
CN108359932A (en) A kind of die surface TD processing methods
CN105349738A (en) Corrosion resistance thermal treatment method for steel
CN108239771B (en) Spraying process of metal protective coating of impeller and sealing ring
CN106793232B (en) Forming method of microwave oven or oven cavity
CN106584033A (en) Forming method of cavity of microwave oven or toaster
CN107523784A (en) The method that antioxidant coating and molybdenum-base alloy surface prepare boronation molybdenum coating
CN103253872B (en) Method for preparing glass surface ceramic coating layer
CN107523782A (en) Molybdenum-base alloy surface oxidation-resistant coating and preparation method thereof
CN105801141A (en) Macro-hole corundum-spinel brick for bottom of Ausmelt furnace and preparation method of macro-hole corundum-spinel brick
CN109097717B (en) Electromagnetic induction heating cooker and preparation method thereof
CN103658670B (en) Purification ultrafine titanium powder and preparation method thereof
RU2387716C2 (en) Blast furnace tuyere preparation method
CN104744973B (en) A kind of effective high radiation ceramic coating of heating-furnace and its preparation, application method
CN105821400A (en) Method for preparing ceramic coating through laser pyrolysis of polysilazane precursor
CN107841705A (en) A kind of method for preparing anti-oxidant refractory metal coating

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WD01 Invention patent application deemed withdrawn after publication
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20171229