CN106637050A - Method for preparing antioxidant film under low oxygen pressure - Google Patents
Method for preparing antioxidant film under low oxygen pressure Download PDFInfo
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- CN106637050A CN106637050A CN201611241612.5A CN201611241612A CN106637050A CN 106637050 A CN106637050 A CN 106637050A CN 201611241612 A CN201611241612 A CN 201611241612A CN 106637050 A CN106637050 A CN 106637050A
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- China
- Prior art keywords
- low oxygen
- oxygen pressure
- quartz ampoule
- under low
- oxidation
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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
- C23C8/16—Oxidising using oxygen-containing compounds, e.g. water, carbon dioxide
- C23C8/18—Oxidising of ferrous surfaces
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
Abstract
The invention belongs to the technical field of surface coating and specifically relates to a method for preparing an antioxidant film with an antioxidant protection property by reacting Fe-base alloy with active gas under a low oxygen pressure. According to the specific scheme, the method comprises the following steps: heating mixed powder of Mn and MnO under an airtight environment; forming a constant low oxygen pressure in the airtight environment; utilizing an oxide to decompose a metallic element under the pressure lower than the low oxygen pressure; and performing external oxidation on Al and Si in the Fe-base alloy and generating a compact antioxidant film on the surface of the Fe-base material. According to a novel technology of preparing the antioxidant film with the antioxidant protection property under the low oxygen pressure provided by the invention, the operation process is simple and the production cost is low.
Description
Technical field
The invention belongs to face coat paint-on technique field, refers in particular to Fe based alloys and gives birth to active gases reaction under low oxygen pressure
Into the preparation method of the oxide film with anti-oxidation protection.
Background technology
At high temperature, the reaction of steel and active gases is a sufficiently complex process, the wherein alloy of surface of steel plate
Element will occur so-called selective oxidation." selective oxidation " refers to that alloying element stronger with oxygen affinity in steel is preferential
In the behavior of matrix Fe Element generation oxides.According to Wagner propose theory, selective oxidation can be divided into external oxidation and
Internal oxidition.External oxidation refers to that the alloying element and oxygen that diffuse to surface react, in Surface Creation oxide；And internal oxidition
It is then that oxygen passes through to be diffused into up to the sub-surface layer below surface, reacts with one or several alloying elements in steel,
Sub-surface layer generates oxide.Steel plate selective oxidation is affected by extraneous several factors, and dew point is to affect high-strength steel to select
Property oxidation a particularly significant factor.Dew point refers to the saturation temperature in annealing atmosphere corresponding to the partial pressure of vapor, dew
The increase of point value means the increase of vapor and oxygen pressure in atmosphere.Perazanovici researchs find that two kinds of elements of Al, Si exist
External oxidation can occur under low dew point conditions, in surface of steel plate Al is generated2O3, SiO2.Generally oxide-film can be divided into two classes：Tool
There are anti-oxidation protection and the not oxide-film with anti-oxidation protection.Wherein most metals can react with active gases
Fine and close oxide-film is generated, this fine and close oxide-film can keep apart oxygen and metal, prevent gas and metal straight
It is reversed to answer, serve anti-oxidation protection effect.
Recent years, sull technology of preparing is developed rapidly.In general, its technology of preparing is segmented into
Two kinds of Physical and chemical method.Physical includes evaporation, sputtering method etc.；Chemical method includes the hydrolysis-precipitation method, sol-gel
Method, liquid phase deposition, atomic layer deposition method, chemical vapour deposition technique etc..Physical and chemical method are compared, comparatively
It is more that Physical prepares energy needed for sull, equipment costly, although and most of chemical methods prepare film needs
Energy is less, can almost prepare all useful sulls, but such as chemical vapour deposition technique needs strict control real
Parameter, such as air pressure, temperature etc. are tested, in addition chemical vapour deposition technique speed is extremely slow, so as to limit its application in some fields.
Therefore, above-mentioned sull paint-on technique is not tedious process, is exactly that deposition velocity is slow or this is more difficult to get uniformity
Film, so developing a kind of sull paint-on technique of novel practical to meet production application be very necessary.
The content of the invention
It is an object of the invention to overcome the shortcomings of existing paint-on technique technique, by mixing Mn and MnO powder in proportion,
Constant oxygen pressure is produced in airtight heating space, Al, Si alloying element external oxidation in Fe sills is made then in Fe base materials
Sull needed for material Surface Creation.Described is as follows the step of preparing sull：
(1) after electric arc melting Fe based alloys, homogenizing annealing one week in 1000 DEG C of vacuum atmosphere oven, then be cut into thin
Piece, and polish successively, polish, clean, be dried；
(2) in mass ratio 1：9 ratio weighs Mn and MnO powder, and bulk is pressed into after being well mixed；
(3) first bulk powder put down gently to quartzy bottom of the tube, subsequently quartz ampoule middle part is burnt into recessed, it is to avoid thin slice had been put into
Quartz ampoule bottom is dropped down onto in journey, thin slice is finally putting into, by quartz ampoule vacuum state after, seal；
(4) quartz ampoule is put into the batch-type furnace that temperature is 1000 DEG C and is incubated 1-2h, you can generated and there is anti-oxidation protection
The sull of property.
The principle of the present invention is in the present invention：
Mn and MnO mixed-powders can maintain a low oxygen pressure balance in the environment of airtight heating, and can according to oxygen gesture figure
To read corresponding partial pressure of oxygen when both certain metallic element at a certain temperature and its oxide reach balance.Mn and MnO mixes
Low oxygen pressure produced by powder is more than Al2O3、SiO2Deng the decomposition pressure of oxide, and it is less than the decomposition pressure of the oxide of Fe.Cause
This, the Al in Fe sills, Si can occur external oxidation, and in matrix surface fine and close oxide-film is generated, and Fe then will not be oxidized.
Beneficial effects of the present invention：
Fe based alloys of the present invention are reacted with active gases under low oxygen pressure and generate the oxide film with anti-oxidation protection,
Operating process is simple, low production cost.
Description of the drawings
Fig. 1 is the quartz ampoule schematic diagram after sealing；
Fig. 2 is oxygen gesture figure.
Specific embodiment
Embodiment 1：
(1) after electric arc melting Fe-3wt.%Al alloys, homogenizing annealing one week in 1000 DEG C of vacuum atmosphere oven, then
It is cut into
Thin slice, and polish successively, polish, clean, be dried；
(2) in mass ratio 1：9 ratio weighs Mn and MnO powder, and bulk is pressed into after being well mixed；
(3) first bulk powder put down gently to quartzy bottom of the tube, subsequently quartz ampoule middle part is burnt into recessed, it is to avoid thin slice had been put into
Quartz ampoule bottom is dropped down onto in journey, thin slice is finally putting into, by quartz ampoule vacuum state after, seal；
(4) quartz ampoule is put into the batch-type furnace that temperature is 1000 DEG C and is incubated 1-2h, you can generated and there is anti-oxidation protection
The Al of property2O3Film.
Embodiment 2：
(1) after electric arc melting Fe-3wt.%Si alloys, homogenizing annealing one week in 1000 DEG C of vacuum atmosphere ovens, then cut
Flakiness, and polish successively, polish, clean, be dried；
(2) in mass ratio 1：9 ratio weighs Mn and MnO powder, and bulk is pressed into after being well mixed；
(3) first bulk powder put down gently to quartzy bottom of the tube, subsequently quartz ampoule middle part is burnt into recessed, it is to avoid thin slice had been put into
Quartz ampoule bottom is dropped down onto in journey, thin slice is finally putting into, by quartz ampoule vacuum state after, seal；
(4) quartz ampoule is put into the batch-type furnace that temperature is 1000 DEG C and is incubated 1-2h, you can generated and there is anti-oxidation protection
The SiO of property2Film.
Embodiment 3：
(1) after electric arc melting Fe-3wt.%Al-3wt.%Si alloys, homogenize in 1000 DEG C of vacuum atmosphere oven and move back
Fire one week, then thinly slice, and polish successively, polish, clean, be dried；
(2) in mass ratio 1：9 ratio weighs Mn and MnO powder, and bulk is pressed into after being well mixed；
(3) first bulk powder put down gently to quartzy bottom of the tube, subsequently quartz ampoule middle part is burnt into recessed, it is to avoid thin slice had been put into
Quartz ampoule bottom is dropped down onto in journey, thin slice is finally putting into, by quartz ampoule vacuum state after, seal；
(4) quartz ampoule is put into the batch-type furnace that temperature is 1000 DEG C and is incubated 1-2h, you can generated and there is anti-oxidation protection
The Al of property2O3And SiO2Mixed film.
Claims (3)
1. a kind of method that oxidation barrier film is prepared under low oxygen pressure, is characterized in that, the mixed of Mn and MnO is heated in closed environment
Powder is closed, makes closed environment produce constant low oxygen pressure, so that metallic element of the peroxide breaks down pressure less than this low oxygen pressure, Fe
There is external oxidation in Al, the Si in based alloy, in the oxide-film that Fe sills Surface Creation is fine and close.
2. a kind of method that oxidation barrier film is prepared under low oxygen pressure as claimed in claim 1, it is characterised in that Fe based alloys
The content control of middle Al is controlled in 0～3wt.% in 0～3wt.%, the content of Si, and remaining is Fe.
3. a kind of method that oxidation barrier film is prepared under low oxygen pressure as claimed in claim 1, it is characterised in that specifically include
Following steps：
(1) after electric arc melting Fe based alloys, homogenizing annealing one week in 1000 DEG C of vacuum atmosphere oven, then thinly slice, and
Polish successively, polish, clean, be dried；
(2) in mass ratio 1：9 ratio weighs Mn and MnO powder, and bulk is pressed into after being well mixed；
(3) first bulk powder put down gently to quartzy bottom of the tube, subsequently quartz ampoule middle part is burnt into recessed, it is to avoid thin slice is during being put into
Drop down onto quartzy bottom of the tube, be finally putting into thin slice, by quartz ampoule vacuum state after, seal；
(4) quartz ampoule is put into the batch-type furnace that temperature is 1000 DEG C and is incubated 1-2h, you can generated with anti-oxidation protection
Sull.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611241612.5A CN106637050A (en) | 2016-12-29 | 2016-12-29 | Method for preparing antioxidant film under low oxygen pressure |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611241612.5A CN106637050A (en) | 2016-12-29 | 2016-12-29 | Method for preparing antioxidant film under low oxygen pressure |
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| Publication Number | Publication Date |
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| CN106637050A true CN106637050A (en) | 2017-05-10 |
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| CN201611241612.5A Pending CN106637050A (en) | 2016-12-29 | 2016-12-29 | Method for preparing antioxidant film under low oxygen pressure |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107858636A (en) * | 2017-10-24 | 2018-03-30 | 常州大学 | The standby Al of powder heap control oxygen compacting2O3And Cr2O3The method of film |
| CN110453170A (en) * | 2019-09-10 | 2019-11-15 | 常州大学 | A method of compact oxidation layer is formed in Fe-Cr-Si system alloy surface |
| CN111910148A (en) * | 2020-08-28 | 2020-11-10 | 浙江华达新型材料股份有限公司 | Method for forming compact oxide film on surface of Fe-Mn-Al alloy |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105648398A (en) * | 2016-02-19 | 2016-06-08 | 同济大学 | Method for improving high-temperature oxidation resistance of TiAl-based alloy by pre-oxidation |
-
2016
- 2016-12-29 CN CN201611241612.5A patent/CN106637050A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105648398A (en) * | 2016-02-19 | 2016-06-08 | 同济大学 | Method for improving high-temperature oxidation resistance of TiAl-based alloy by pre-oxidation |
Non-Patent Citations (3)
| Title |
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| 梁成浩: "《现代腐蚀科学与防护技术》", 30 September 2007 * |
| 魏超: "《液体火箭发动机特种制造技术》", 31 October 2014, 中国宇航出版社 * |
| 黄烯祜: "《钢铁冶金原料 (第4版)》", 31 January 2013, 冶金工业出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107858636A (en) * | 2017-10-24 | 2018-03-30 | 常州大学 | The standby Al of powder heap control oxygen compacting2O3And Cr2O3The method of film |
| CN110453170A (en) * | 2019-09-10 | 2019-11-15 | 常州大学 | A method of compact oxidation layer is formed in Fe-Cr-Si system alloy surface |
| CN111910148A (en) * | 2020-08-28 | 2020-11-10 | 浙江华达新型材料股份有限公司 | Method for forming compact oxide film on surface of Fe-Mn-Al alloy |
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Application publication date: 20170510 |