CN110102751A - Metallic particles anti oxidation layer plasma technology of preparing - Google Patents
Metallic particles anti oxidation layer plasma technology of preparing Download PDFInfo
- Publication number
- CN110102751A CN110102751A CN201910313155.3A CN201910313155A CN110102751A CN 110102751 A CN110102751 A CN 110102751A CN 201910313155 A CN201910313155 A CN 201910313155A CN 110102751 A CN110102751 A CN 110102751A
- Authority
- CN
- China
- Prior art keywords
- fsa
- metallic particles
- temperature
- plasma
- layer
- 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.)
- Granted
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oxygen, Ozone, And Oxides In General (AREA)
Abstract
The present invention relates to metallic particles anti oxidation layer plasma technology of preparing, detailed processes are as follows: high-temperature oxydation obtains persursor material in air by metallic particles；Persursor material is plasma-treated, form the high-temperature oxidation resistant graded ceramics structure that surface of metal particles is attached to a thickness of the stabilization of 200~600nm；Wherein, the air pressure of corona treatment is 50~150Pa, and temperature is 500~900 DEG C, and power is 300~500W, and the single reaction time is 20s~60s, and interval time is 20~40s, and reaction times are 20~40 times.The graded ceramics layer that the present invention is formed can effectively reduce the transmission channel between FSA and oxidizing atmosphere, improve the anti-oxidant and corrosion resistance of FSA；Compared with traditional antioxidant coating, the graded ceramics and metallic particles bond strength with higher of growth in situ, so that fire-resistant oxidation resistant layer is greatly promoted with matrix matched coefficients of thermal expansion.
Description
Technical field
The present invention relates to metallic particles anti oxidation layer plasma technologies of preparing, particularly relate in surface of metal particles
A kind of plasma technique of one layer of graded ceramics structure with good antioxidation of preparation.
Background technique
Zero-valent metal granular materials is widely used in defence and military, mechanical microelectronics, optical device, biologic medical, change
The fields such as the work energy.However, not surface treated zero-valent metal granular materials there are inoxidizability it is poor, perishable the defects of.
CN105385987A discloses a kind of preparation method of tungsten surface high-temp anti oxidation layer, and this method will mainly have cleaning
In the tungsten embedment molybdenum penetration enhancer on surface, tungsten surface is obtained after inert atmosphere is heat-treated with tungsten solid solution layer
The semi-finished product are then embedded in silication penetration enhancer by semi-finished product after nitrogen is heat-treated, and hot-working obtains in an inert atmosphere
Tungsten surface is the finished product of W-Mo-N-Si system high-temperature oxidation resistant layer.However, the preparation process is complex, production cost compared with
Height, and the structure and phase of poor, the uncontrollable coating of thermal matching between coating and matrix, directly affect the height of tungsten
Warm service life.The patent application of Publication No. CN1452453 proposes and a kind of irradiates to form anti oxidation layer by ultraviolet light
Method first imposes the covering of elargol in the cladding epithelial surfaces of former conductive bodies first, and then on the surface layer of elargol, coating is included
The PU (polyurethane) of UV initiator, finally again through ultraviolet irradiation, enabling PU generate with initiator, friendship is poly- to react, and formation consolidates attached
In anti-oxidant PU layers of elargol surface layer.The preparation process equally exists the thermal expansion coefficient between coating and matrix and is difficult to match
The problem of.
Summary of the invention
It is an object of the present invention to for metal particle material is perishable, antioxygenic property is poor, anti-existing for background technique
Oxide layer and matrix thermal expansion coefficient are difficult to matched defect, propose metallic particles anti oxidation layer plasma technology of preparing.
The present invention surface of metal particles obtain a layer thickness be 200~600nm stabilization be attached to surface of metal particles it is anticorrosive,
The graded ceramics structure of high-temperature oxidation resistant.
To achieve the above object, The technical solution adopted by the invention is as follows:
Metallic particles anti oxidation layer plasma technology of preparing, which comprises the following steps:
By metallic particles, high-temperature oxydation obtains persursor material in air, and oxidizing temperature is 500~900 DEG C, when oxidation
Between be 1~15h；
Persursor material is plasma-treated, it is formed and is attached to metallic particles table with a thickness of the stabilization of 200~600nm
The high-temperature oxidation resistant graded ceramics structure in face, i.e. anti oxidation layer；Wherein, the air pressure of corona treatment is 50~150Pa, temperature
Be 500~900 DEG C, plasma power be 300~500W, the single reaction time be 20s~60s, interval time be 20~
40s, reaction times are 20~40 times.
Further, the metallic particles includes but is not limited to the zero-valent states particle such as FeCo, FeSiAl.
Further, the high-temperature oxidation resistant graded ceramics structure of the surface of metal particles includes 2~4 layers of graded ceramics
Layer.
The invention has the benefit that
Metallic particles anti oxidation layer plasma technology of preparing provided by the invention, using in the surface FSA (FeSiAl) original
Position oxidation generates unordered oxide layer, and further by plasma technique is converted to unordered oxide layer completely new with excellent
Anti-oxidant, corrosion resistance graded ceramics layer.The graded ceramics layer that the technology of the present invention is formed can effectively reduce FSA and oxidation
Transmission channel between atmosphere improves the anti-oxidant and corrosion resistance of FSA；It is in situ raw compared with traditional antioxidant coating
Long graded ceramics and metallic particles bond strength with higher, so that fire-resistant oxidation resistant layer and matrix thermal expansion coefficient
It is greatly promoted with property.Present invention process is simple, and cost is relatively low, and reaction process is controllable and yield is high, have very big utility value and
Development prospect.
Detailed description of the invention
Fig. 1 is graded ceramics/FSA composite construction (FSA@GCLs) section backscattered electron figure that 1 step 2 of embodiment obtains
Picture；
Fig. 2 is graded ceramics/FSA composite construction SEM figure that Examples 1 to 4 obtains；Wherein, (a) is embodiment 2,
(b) it is embodiment 3, (c) is embodiment 4, (d) is embodiment 1；
Fig. 3 is graded ceramics/FSA composite construction XRD diagram that embodiment 1 obtains；
Fig. 4 is the graded ceramics/FSA composite construction TG curve (a) and second stage starting point temperature that embodiment 1 obtains
(b)。
Specific embodiment
With reference to the accompanying drawings and examples, technical solution of the present invention is described in detail.
A kind of metallic particles anti oxidation layer plasma technology of preparing, comprising the following steps:
FeSiAl (FSA) metallic particles of certain mass is weighed, high-temperature oxydation obtains persursor material in air, oxidation
Temperature is 500~900 DEG C, and oxidization time is 1~15h；
Persursor material is plasma-treated, make persursor material surface experience plasma etching, wash away and from
The processes such as body reconstructed tissue form the high-temperature oxidation resistant that the stabilization that a layer thickness is 200~600nm is attached to surface of metal particles
Graded ceramics structure, i.e. anti oxidation layer；Detailed process are as follows: persursor material is placed in the reacting furnace of inert gas atmosphere, furnace
Interior air pressure is 50~150Pa, and temperature is 500~900 DEG C, and plasma power is 300~500W, and the single reaction time is 20s
~60s, interval time are 20~40s, and reaction times are 20~40 times；After the reaction was completed, cooled to room temperature is taken out, i.e.,
The available high-temperature oxidation resistant graded ceramics structure that surface of metal particles is attached to a thickness of the stabilization of 200~600nm, i.e. antioxygen
Change layer.
Embodiment 1
Fire-resistant oxidation resistant graded ceramics/FSA composite construction preparation method, comprising the following steps:
Step 1 weighs 50g micron-sized FeSiAl (FSA) metallic particles, and high-temperature oxydation obtains presoma material in air
Material, oxidizing temperature are 700 DEG C, oxidization time 10h；
Step 2, the persursor material (FSA@CLs) obtained by plasma technology of preparing processing step 1；Specifically: it will
The persursor material that step 1 obtains is placed in the CVD furnace of argon atmosphere, air pressure is 95Pa in furnace, temperature is 850 DEG C, etc. from
Daughter power carries out several times of plasma precursor reactant under conditions of being 450W, the single reaction time is 60s, twice the reacting space time
For 20s, reaction times are 20 times；After the reaction was completed, cooled to room temperature takes out product, graded ceramics/FSA can be obtained
Composite construction (FSA@GCLs).
Fig. 1 is graded ceramics/FSA composite construction (FSA@GCLs) section backscattered electron figure that 1 step 2 of embodiment obtains
Picture；As shown in Figure 1, in the composite construction that embodiment 1 obtains, FSA ceramic layer on surface distribution gradient, thickness be about 400nm~
500nm。
Embodiment 2
Compared with Example 1, difference is the present embodiment:
When persursor material (the FSA@CLs) that step 2 is obtained by plasma technology of preparing processing step 1, detailed process
Are as follows: the persursor material for obtaining step 1 is placed in the CVD furnace of argon atmosphere, air pressure is 95Pa in furnace, temperature is 750 DEG C,
Plasma power carries out several times of plasma precursor reactant under conditions of being 450W, the single reaction time is 40s, twice reacting space
Time is 20s, and reaction times are 20 times；After the reaction was completed, cooled to room temperature, take out product, can be obtained graded ceramics/
FSA composite construction (FSA@GCLs).
Embodiment 3
Compared with Example 1, difference is the present embodiment:
When persursor material (the FSA@CLs) that step 2 is obtained by plasma technology of preparing processing step 1, detailed process
Are as follows: the persursor material for obtaining step 1 is placed in the CVD furnace of argon atmosphere, air pressure is 95Pa in furnace, temperature is 800 DEG C,
Plasma power carries out several times of plasma precursor reactant under conditions of being 450W, the single reaction time is 40s, twice reacting space
Time is 20s, and reaction times are 20 times；After the reaction was completed, cooled to room temperature, take out product, can be obtained graded ceramics/
FSA composite construction (FSA@GCLs).
Embodiment 4
Compared with Example 1, difference is the present embodiment:
When persursor material (the FSA@CLs) that step 2 is obtained by plasma technology of preparing processing step 1, detailed process
Are as follows: the persursor material for obtaining step 1 is placed in the CVD furnace of argon atmosphere, air pressure is 95Pa in furnace, temperature is 850 DEG C,
Plasma power carries out several times of plasma precursor reactant under conditions of being 450W, the single reaction time is 40s, twice reacting space
Time is 20s, and reaction times are 20 times；After the reaction was completed, cooled to room temperature, take out product, can be obtained graded ceramics/
FSA composite construction (FSA@GCLs).
Fig. 2 is graded ceramics/FSA composite construction SEM figure that Examples 1 to 4 obtains；Wherein, (a) is embodiment 2,
(b) it is embodiment 3, (c) is embodiment 4, (d) is embodiment 1；As shown in Figure 2, particle surface has a small amount of crackle in embodiment 2,
There are white particles without obvious crackle, 4 particle surface of embodiment in 3 particle surface of embodiment, and particle surface white is micro- in embodiment 1
Grain is significantly increased compared to 4 particle surface white particles size of embodiment.
Fig. 3 is graded ceramics/FSA composite construction XRD diagram that embodiment 1 (FSA@GCLs) is obtained；From the figure 3, it may be seen that
FSA, FSA@CLs and FSA@GCLs main diffraction peak are FSA, while a small amount of Al occur2O3And Fe2O3, this shows FSA through oxygen
Fe is produced after change2O3, FSA@CLs generates Al after plasma-induced technical treatment2O3, while also turn out high-temperature oxydation and
Plasma-induced technology does not have an impact or changes the intrinsic property of FSA.
Fig. 4 is graded ceramics/FSA composite construction the TG curve (a) and second stage that embodiment 1 (FSA@GCLs) is obtained
Starting point temperature (b).By Fig. 4 a it is found that the oxidation of FSA, FSA@CLs and FSA@GCLs can be divided into two stages: solid oxide
And liquid oxidatively.By Fig. 4 b it is found that the second stage initial temperature of FSA@GCLs obviously increases 120 DEG C or more than FSA.
Claims (3)
1. metallic particles anti oxidation layer plasma technology of preparing, which comprises the following steps:
By metallic particles, high-temperature oxydation obtains persursor material in air, and oxidizing temperature is 500~900 DEG C, oxidization time 1
~15h；
Persursor material is plasma-treated, form the high temperature for being attached to surface of metal particles with a thickness of 200~600nm
Anti-oxidant graded ceramics structure, i.e. anti oxidation layer；Wherein, the air pressure of corona treatment be 50~150Pa, temperature be 500~
900 DEG C, plasma power is 300~500W, and the single reaction time is 20s~60s, and interval time is 20~40s, reaction time
Number is 20~40 times.
2. metallic particles anti oxidation layer plasma technology of preparing according to claim 1, which is characterized in that the metal
Particle is FeCo or FeSiAl.
3. metallic particles anti oxidation layer plasma technology of preparing according to claim 1, which is characterized in that the metal
The high-temperature oxidation resistant graded ceramics structure of particle surface includes 2~4 layers of graded ceramics layer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910313155.3A CN110102751B (en) | 2019-04-18 | 2019-04-18 | Plasma preparation technology for metal particle oxidation resistant layer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910313155.3A CN110102751B (en) | 2019-04-18 | 2019-04-18 | Plasma preparation technology for metal particle oxidation resistant layer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110102751A true CN110102751A (en) | 2019-08-09 |
| CN110102751B CN110102751B (en) | 2021-04-30 |
Family
ID=67485797
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910313155.3A Active CN110102751B (en) | 2019-04-18 | 2019-04-18 | Plasma preparation technology for metal particle oxidation resistant layer |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110102751B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114752113A (en) * | 2022-04-25 | 2022-07-15 | 电子科技大学长三角研究院(湖州) | Method for enhancing FeSiAl wave-absorbing material by plasma densification of acrylic polyurethane |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0980916A2 (en) * | 1998-07-30 | 2000-02-23 | Ford Motor Company | Sprayforming bulk deposits of allotropic metal |
| JP2002309323A (en) * | 2001-04-12 | 2002-10-23 | Toyama Prefecture | Functionally gradient material composed of low-melting point metal and oxide ceramics, and its manufacturing method |
| CN1404424A (en) * | 2000-02-18 | 2003-03-19 | 加拿大电子学粉末公司 | Nickel powder for use as electrodes in base metal electrode multilayered ceramic capacitors |
| CN1406693A (en) * | 2001-09-04 | 2003-04-02 | 深圳华科纳米技术开发有限公司 | Preparation for fine-superfines under normal pressure and its apparatus |
| CN101362200A (en) * | 2008-09-20 | 2009-02-11 | 大连理工大学 | Synthesis method of metallic oxide coated dissimilar metal 'core/shell'nano-particles |
| CN101500733A (en) * | 2006-06-19 | 2009-08-05 | 卡伯特公司 | Metal-containing nanoparticles, their synthesis and use |
| CN104674218A (en) * | 2015-03-21 | 2015-06-03 | 西北有色金属研究院 | Preparation method of titanium substrate surface high-temperature antioxidant composite coating |
| CN107904473A (en) * | 2017-10-25 | 2018-04-13 | 广东新秀新材料股份有限公司 | Preparation method of the high tenacity without electromagnetic shielding ceramic composite |
| CN108247072A (en) * | 2016-12-29 | 2018-07-06 | 江民德 | A kind of method that spherical 3D printing powder is prepared using plasma |
-
2019
- 2019-04-18 CN CN201910313155.3A patent/CN110102751B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0980916A2 (en) * | 1998-07-30 | 2000-02-23 | Ford Motor Company | Sprayforming bulk deposits of allotropic metal |
| CN1404424A (en) * | 2000-02-18 | 2003-03-19 | 加拿大电子学粉末公司 | Nickel powder for use as electrodes in base metal electrode multilayered ceramic capacitors |
| JP2002309323A (en) * | 2001-04-12 | 2002-10-23 | Toyama Prefecture | Functionally gradient material composed of low-melting point metal and oxide ceramics, and its manufacturing method |
| CN1406693A (en) * | 2001-09-04 | 2003-04-02 | 深圳华科纳米技术开发有限公司 | Preparation for fine-superfines under normal pressure and its apparatus |
| CN101500733A (en) * | 2006-06-19 | 2009-08-05 | 卡伯特公司 | Metal-containing nanoparticles, their synthesis and use |
| CN101362200A (en) * | 2008-09-20 | 2009-02-11 | 大连理工大学 | Synthesis method of metallic oxide coated dissimilar metal 'core/shell'nano-particles |
| CN104674218A (en) * | 2015-03-21 | 2015-06-03 | 西北有色金属研究院 | Preparation method of titanium substrate surface high-temperature antioxidant composite coating |
| CN108247072A (en) * | 2016-12-29 | 2018-07-06 | 江民德 | A kind of method that spherical 3D printing powder is prepared using plasma |
| CN107904473A (en) * | 2017-10-25 | 2018-04-13 | 广东新秀新材料股份有限公司 | Preparation method of the high tenacity without electromagnetic shielding ceramic composite |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114752113A (en) * | 2022-04-25 | 2022-07-15 | 电子科技大学长三角研究院(湖州) | Method for enhancing FeSiAl wave-absorbing material by plasma densification of acrylic polyurethane |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110102751B (en) | 2021-04-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR101108692B1 (en) | Dense rare earth metal oxides coating to seal the porous ceramic surface, and the method of rare earth metal oxides coating layer | |
| WO2009096138A1 (en) | Soft magnetic material and process for producing the soft magnetic material | |
| CN102212823B (en) | Method for arranging film sensor on alloy substrate | |
| CN105453249A (en) | Retainer, method for producing same and use thereof | |
| CN116092909A (en) | Plasma etching reactor | |
| CN105990081B (en) | Plasma processing apparatus and preparation method thereof | |
| US8463342B2 (en) | Nano-fabricated superconducting radio-frequency composites, method for producing nano-fabricated superconducting rf composites | |
| CN103374697A (en) | Surface treatment method and product of diamond-like carbon film layer | |
| US20140199561A1 (en) | Coated article and method for manufacturing same | |
| CN110102751A (en) | Metallic particles anti oxidation layer plasma technology of preparing | |
| CN106435489A (en) | Preparation method for oxidation resisting self-healing Cr/NiCr coatings on niobium-based surface | |
| CN107630184B (en) | A method of niobium silicide coating is prepared in niobium or niobium alloy surface | |
| CN106521202B (en) | A kind of preparation method of molybdenum hafnium alloy plate | |
| CN112746253A (en) | Steel-based surface composite modified layer and preparation method thereof | |
| JPS60176981A (en) | Ceramic enhancement | |
| CN105132888B (en) | A kind of composite deposition method of high-temperature oxidation resistant coating | |
| CN112374911A (en) | Surface treatment method of graphite substrate and preparation method of TaC coating | |
| CN106278264A (en) | A kind of high density chromic lanthanum ceramics heater manufacture method | |
| KR20180034340A (en) | Manufacturing method of translucent yttria by hot pressing sintering | |
| JP4562483B2 (en) | Method for producing soft magnetic material | |
| CN104428272A (en) | Method of treating a surface layer of a device consisting of alumina and respective device, particularly x-ray tube component | |
| CN104894505A (en) | Vacuum plasma spraying forming method for ultra-thick coating | |
| CN108070859A (en) | Refractory metal surfaces lamellar composite Ir/W high-temperature oxidation resistant coatings and preparation method thereof | |
| KR101766970B1 (en) | Functional Coating Film Manufacturing Method and Functional Coating Film | |
| CN104715994B (en) | Inductive type plasma process chamber and its anticorrosive insulated window and manufacture method |
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 | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |