CN106835067B - A kind of method of Zr alloy surface graphene Passivation Treatment corrosion-inhibiting coating - Google Patents
A kind of method of Zr alloy surface graphene Passivation Treatment corrosion-inhibiting coating Download PDFInfo
- Publication number
- CN106835067B CN106835067B CN201710026560.8A CN201710026560A CN106835067B CN 106835067 B CN106835067 B CN 106835067B CN 201710026560 A CN201710026560 A CN 201710026560A CN 106835067 B CN106835067 B CN 106835067B
- Authority
- CN
- China
- Prior art keywords
- graphene
- passed
- zircaloy
- reaction chamber
- atomic 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.)
- Active
Links
Classifications
-
- 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
- C23C16/26—Deposition of carbon only
-
- 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
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0227—Pretreatment of the material to be coated by cleaning or etching
-
- 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
- C23C16/32—Carbides
- C23C16/325—Silicon carbide
-
- 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
- C23C16/44—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 method of coating
- C23C16/455—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 method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
-
- 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
- C23C16/44—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 method of coating
- C23C16/50—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 method of coating using electric discharges
- C23C16/517—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 method of coating using electric discharges using a combination of discharges covered by two or more of groups C23C16/503 - C23C16/515
Abstract
A kind of method of Zr alloy surface graphene Passivation Treatment corrosion-inhibiting coating is using MPCVD method in Zr alloy surface growth in situ graphene protective layer; then zircaloy/graphene sample is placed in the reaction chamber of atomic layer deposition apparatus, carry out the deposition of silicon carbide.Since atomic layer passivation particle silicon carbide is especially sensitive to dangling bond; can preferential deposition in the defective locations of graphene, form the cluster of dispersion in the hole of graphene, grain boundaries, rather than continuous film; the defect of graphene is passivated, to realize complete protection of the graphene to zircaloy.This method is simply at low cost, and the film protective value of acquisition is excellent, has potential application in the corrosion-resistant field of nuclear-used zirconium alloy.
Description
Technical field
The present invention relates to a kind of processing methods of Zr alloy surface corrosion-inhibiting coating, specifically use microwave plasma
Vapour deposition process is learned in Zr alloy surface growth in situ graphene protective layer, zircaloy/graphene sample is then put into atom
The reaction chamber of layer depositing device, carries out a kind of side of Zr alloy surface graphene Passivation Treatment corrosion-inhibiting coating of depositing SiC
Method.
Background technique
Nuclear advanced, security reliability and economy and cladding materials performance are closely related.Existing zircaloy
Corrosion is still faced with acid test in nuclear reactor, can not be ignored, therefore the corrosion resistance gesture for improving zircaloy exists
It must go.Since the corrosion of zircaloy is generated since surface, carrying out surface modification treatment to zircaloy is to effectively improve
The important method of its corrosion resistance.There are many ways to Zr alloy surface is modified, for example, anodic oxidation, the pre- filming of autoclave,
The technologies such as plasma electrolytic oxidation, arc evaporation, spraying, sol-gel deposition, the oxidation of air high frequency, ion implanting.But
There is certain thickness by protective film prepared by current process for treating surface, changes the size of zircaloy, and thick
Protective film can reduce the thermal conductivity of zircaloy.Therefore, the important channel for overcoming these problems is exactly that develop a kind of thermal conductivity good
Ultra-thin protective layer makes the size of zircaloy and performance change reach minimum.
Graphene is a kind of two-dimentional monoatomic layer carbon material, due to being caused in academia with many special performances
Unprecedented research boom.Recent research personnel have found that graphene can be used as the super thin protective coatings of metal, protect metal material
It is not corroded.This provides new approaches for the research of Reactor fuel element cladding Zr alloy surface protective layer.Therefore, the present invention proposes
Use graphene as Zr alloy surface protective layer, it, will while guaranteeing zircaloy thermal conductivity and unaffected shape, size
Zircaloy and cooling medium are effectively isolated, and improve the corrosion resistance of zircaloy.However, graphene to the degree of protection of metal and
Its crystal structure, the number of plies, defect are closely related.High quality, flawless single crystal graphene can make its protectiveness to metal
It can maximize.But be difficult to obtain the single crystal graphene film of large area, zero-fault by existing method, it is received inside graphene
The presence of the defects of metre hole, crystal boundary seriously limits its improvement to Corrosion Resistance of Zirconium Alloys.Therefore, how to graphene
Defect is passivated processing, realizes the completely isolated of Zr alloy surface and cooling water, becomes a urgent problem to be solved.
Summary of the invention
Poor in order to solve the water-fast side corrosive nature of zirconium alloy cladding, the short problem of fuel can service life, the present invention mentions
For a kind of method of Zr alloy surface graphene Passivation Treatment corrosion-inhibiting coating.
The present invention the taken technical solution that solves the above problems is as follows.
A kind of method of Zr alloy surface graphene Passivation Treatment corrosion-inhibiting coating, the method are to follow these steps to carry out
:
(1) zircaloy is first cleaned in acetone, after being impregnated in nitric acid and hydrofluoric acid mixed solution, then in dehydrated alcohol
Sonic oscillation 2 times, each 30min, surface impurity and greasy dirt are removed, is then dried in a nitrogen environment；
(2) zircaloy is placed in the reaction chamber of microwave plasma CVD equipment, cavity is evacuated to
1Pa is hereinafter, be passed through the hydrogen of 50sccm~200sccm, and to 1000W~6000W, cavity air pressure is maintained at adjusting microwave power
2kPa~9kPa bombards zircaloy 10min~180min by hydrogen plasma, and substrate is heated and further removes the miscellaneous of surface
Matter；
(3) it is passed through methane and regulating gas ratio starts to grow graphene film, sedimentation time is 10~120s, deposition temperature
Degree is 300~600 DEG C, and gas flow methane/hydrogen is 1/60,1/80,1/100,1/200 or 1/300, and cavity air pressure is
2.7~7.4kPa, microwave power are 1300~6000 W；
(4) after the completion of depositing, methane gas and microwave power supply are closed, continuing to be passed through hydrogen makes cavity with 2~3 DEG C/s rate
100 DEG C are cooled to hereinafter, taking out sample；
(5) sample of acquisition is placed in the reaction chamber of atomic layer deposition apparatus, carries out the deposition of silicon carbide passivation particle, it will
The defect of metal surface graphene is passivated processing；
The deposition of the silicon carbide passivation particle follows these steps to carry out:
Argon gas or nitrogen are passed through into atomic layer deposition apparatus reaction chamber；
It is passed through carbonaceous material into atomic layer deposition apparatus reaction chamber, makes it that carbon geochemistry absorption occur with sample surfaces；
Silicon-containing material is passed through into atomic layer deposition apparatus reaction chamber, the carbon of silicon atom and sample surfaces in silicon-containing material
Atom forms carbon silicon bonds, and after complete reaction, sample surfaces graphene fault location forms silicon-carbide particle.
Based on the above-mentioned technical proposal, further technical characteristic is as follows.
In the reaction chamber that zircaloy is placed in microwave plasma CVD equipment, cavity is evacuated to
When 1Pa or less, it is further passed through the hydrogen of 100sccm, adjusts microwave power to 1300W, cavity air pressure is maintained at 2.6kPa, by
Hydrogen plasma bombards zircaloy 30min, and substrate is heated to and further removed the impurity on surface.
It is described be passed through methane and regulating gas ratio start grow graphene film, further sedimentation time is 120s,
Depositing temperature is 550 DEG C, and gas flow methane/hydrogen is 1/60, and cavity air pressure is 4.0kPa, and microwave power is 1300W.
The carbonaceous material that is passed through into atomic layer deposition apparatus reaction chamber is carbon tetrachloride, and the flow velocity of carbon tetrachloride is
10sccm~400sccm, inlet period are 0.5s~1s.
The silicon-containing material that is passed through into atomic layer deposition apparatus reaction chamber is silane, the flow velocity of silane be 10sccm~
100sccm, the inlet period of silane are 0.5s~1s.
A kind of method of Zr alloy surface graphene Passivation Treatment corrosion-inhibiting coating provided by the present invention is above-mentioned, with existing skill
Art is compared, and this method directly grows graphene in Zr alloy surface using MPCVD method, by graphite
The growth temperature of alkene drops to 300~600 DEG C, to will not influence the microscopic structure of zircaloy；Existed using technique for atomic layer deposition
Graphene surface depositing silicon silicon, atomic layer passivation particle is especially sensitive to dangling bond, defective bit of the meeting preferential deposition in graphene
It sets, forms the cluster of dispersion in the hole of graphene, grain boundaries, rather than continuous film, the defect of graphene is carried out blunt
Change, to realize complete protection of the graphene to zircaloy.
Detailed description of the invention
Fig. 1 is the schematic diagram that zircaloy sample corrodes in cooling medium.In figure: 1 is zircaloy, and 2 be zirconium oxide, and 3 are
Hydrone in cooling medium, 4 be zirconium atom.
Fig. 2 is the schematic diagram that zircaloy/graphene sample is corroded in cooling medium.In figure: 1 is zircaloy, and 2 be oxidation
Zirconium, 3 be graphene, and 4 be the hydrone in cooling medium.
Fig. 3 is the schematic diagram that zircaloy/graphene corrodes in cooling medium after graphene defect passivation is handled.In figure: 1
It is passivation particle for zircaloy, 2,3 be graphene, and 4 be the hydrone in cooling medium.
Specific embodiment
A specific embodiment of the invention is further illustrated below.
Implement a kind of method of Zr alloy surface graphene Passivation Treatment corrosion-inhibiting coating, this method is to follow these steps to carry out
:
Clean Step 1: zircaloy is placed in acetone, impregnated in nitric acid and hydrofluoric acid mixed solution, after again in nothing
Sonic oscillation 2 times in water-ethanol, each 30min, it is therefore an objective to impurity and greasy dirt of Zr alloy surface etc. are removed, then in nitrogen ring
It is dried under border.
Step 2: zircaloy is placed in the reaction chamber of microwave plasma CVD equipment, and cavity is taken out
Vacuum is to 1Pa hereinafter, be passed through the hydrogen of 50sccm~200sccm again, and adjusting microwave power is 1000W~6000W, after by chamber
When body air pressure is maintained at 2kPa~9kPa, zircaloy 10min~180min is bombarded by hydrogen plasma, then simultaneously by substrate heating
Further remove the impurity on surface.
Step 3: be passed through methane and regulating gas ratio start grow graphene film, sedimentation time is 10~120s, sink
Accumulated temperature degree is 300~600 DEG C, and gas flow methane/hydrogen is 1/60,1/80,1/100,1/200 or 1/300, cavity air pressure
It is 2.7~7.4kPa, microwave power is 1300~6000 W.
Step 4: close methane gas and microwave power supply after the completion of deposition, continuing to be passed through hydrogen makes cavity with 2~3 DEG C/s
Rate is cooled to 100 DEG C hereinafter, taking out sample.
Step 5: the sample of acquisition to be placed in the reaction chamber of atomic layer deposition apparatus, the heavy of silicon carbide passivation particle is carried out
Product, is passivated processing for the defect of metal surface graphene；Wherein, the deposition of silicon carbide passivation particle be follow these steps into
Capable:
It is that argon gas or nitrogen are passed through into the reaction chamber of atomic layer deposition apparatus first；
It followed by is passed through carbonaceous material into the reaction chamber of atomic layer deposition apparatus, makes it that carbon geochemistry occur with sample surfaces
Absorption；
It is finally that silicon-containing material is passed through into the reaction chamber of atomic layer deposition apparatus, silicon atom and sample in silicon-containing material
The carbon atom on surface forms carbon silicon bonds, and after complete reaction, sample surfaces graphene fault location forms silicon-carbide particle.
Based on above-mentioned specific embodiment, the second specific embodiment is that zircaloy is placed in microwave plasma chemical gas
In the reaction chamber of phase depositing device, cavity is evacuated to 1Pa hereinafter, selection is passed through the hydrogen of 100sccm, adjusting microwave power
To 1300W, cavity air pressure is maintained at 2.6kPa, bombards zircaloy 30min by hydrogen plasma, substrate is heated and removes surface
Metal oxide and impurity.
Based on above-mentioned specific embodiment, third specific embodiment is to be passed through methane and regulating gas ratio starts to grow
Graphene film, selecting sedimentation time is 120s, and depositing temperature is 550 DEG C, and gas flow methane/hydrogen is 1/60, cavity gas
Pressure is 4.0kPa, and microwave power is 1300W.
Based on above-mentioned specific embodiment, the 4th specific embodiment is to be passed through to contain into atomic layer deposition apparatus reaction chamber
Carbonizable substance is carbon tetrachloride, and the flow velocity of carbon tetrachloride is 10sccm~400sccm, and inlet period is 0.5s~1s.
Based on above-mentioned specific embodiment, the 5th specific embodiment is to be passed through to contain into atomic layer deposition apparatus reaction chamber
Silicon matter is silane, and the flow velocity of silane is 10sccm~100sccm, and the inlet period of silane is 0.5s~1s.
A specific embodiment of the invention is further illustrated below by embodiment.
Embodiment 1
Graphene, specific steps are directly grown in Zr alloy surface by MPCVD method are as follows:
Zircaloy is cleaned in acetone, and in nitric acid and hydrofluoric acid mixed solution after immersion, then the sonic oscillation in dehydrated alcohol
2 times, each 30min, the impurity and greasy dirt on surface are removed, is then dried in a nitrogen environment；Then by the zircaloy after cleaning
It is put into the reaction chamber of microwave plasma CVD equipment, cavity is evacuated to 1Pa hereinafter, being passed through 100sccm
Hydrogen, adjust microwave power to 1300W, cavity air pressure is maintained at 2.6kPa, with hydrogen plasma bombard zircaloy 30min,
So that substrate is heated to suitable temperature and the further impurity on removing surface；After zircaloy is pre-processed, it is passed through methane simultaneously
Adjusting methane/hydrogen is 1/60, and cavity air pressure is 3.0kPa, microwave power 1300W, and 120s is reacted at 500 DEG C, grows stone
Black alkene film；After the completion of deposition, methane gas and microwave power supply are closed, continuing to be passed through hydrogen keeps cavity cold with 2~3 DEG C/s rate
But to 100 DEG C hereinafter, taking out sample；
The sample that above-mentioned MPCVD method obtains is put into the reaction chamber of atomic layer deposition apparatus,
The deposition for carrying out silicon carbide passivation particle, is passivated processing for the defect of Zr alloy surface graphene.Silicon carbide passivation particle
Preparation include the following steps: to be passed through argon gas into atomic layer deposition apparatus reaction chamber；Into atomic layer deposition apparatus reaction chamber
It is passed through 100sccm carbon tetrachloride, inlet period is 0.5s~1s, makes carbonaceous material and sample surfaces that carbon geochemistry absorption occur；To
10sccm silane is passed through in atomic layer deposition apparatus reaction chamber, inlet period is 0.5s~1s.Silicon atom and sample in silane
The carbon atom on surface forms carbon silicon bonds, and after complete reaction, sample surfaces graphene fault location forms silicon-carbide particle.
Claims (3)
1. a kind of method of Zr alloy surface graphene Passivation Treatment corrosion-inhibiting coating, the method follows these steps to carry out:
(1) zircaloy is first cleaned in acetone, after being impregnated in nitric acid and hydrofluoric acid mixed solution, then the ultrasound in dehydrated alcohol
Oscillation 2 times, each 30min removes surface impurity and greasy dirt, then dries in a nitrogen environment；
(2) zircaloy is placed in the reaction chamber of microwave plasma CVD equipment, by cavity be evacuated to 1Pa with
Under, be passed through the hydrogen of 50sccm~200sccm, adjust microwave power to 1000W~6000W, cavity air pressure be maintained at 2kPa~
9kPa bombards zircaloy 10min~180min by hydrogen plasma, and substrate is heated to and further removed the impurity on surface；
(3) it is passed through methane and regulating gas ratio starts to grow graphene film, sedimentation time is 10~120s, and depositing temperature is
300~600 DEG C, gas flow methane/hydrogen is 1/60,1/80,1/100,1/200 or 1/300, cavity air pressure is 2.7~
7.4kPa, microwave power are 1300~6000W；
(4) after the completion of depositing, methane gas and microwave power supply are closed, continuing to be passed through hydrogen keeps cavity cooling with 2~3 DEG C/s rate
To 100 DEG C hereinafter, taking out sample；
(5) sample of acquisition is placed in the reaction chamber of atomic layer deposition apparatus, the deposition of silicon carbide passivation particle is carried out, by metal
The defect of surface graphene is passivated processing；
The deposition of the silicon carbide passivation particle follows these steps to carry out:
Argon gas or nitrogen are passed through into atomic layer deposition apparatus reaction chamber；
It is passed through carbonaceous material into atomic layer deposition apparatus reaction chamber, makes it that carbon geochemistry absorption occur with sample surfaces；
Silicon-containing material is passed through into atomic layer deposition apparatus reaction chamber, the carbon atom of silicon atom and sample surfaces in silicon-containing material
Carbon silicon bonds are formed, after complete reaction, sample surfaces graphene fault location forms silicon-carbide particle；
The carbonaceous material that is passed through into atomic layer deposition apparatus reaction chamber is carbon tetrachloride, and the flow velocity of carbon tetrachloride is 10sccm
~400sccm, inlet period are 0.5s~1s；
The silicon-containing material that is passed through into atomic layer deposition apparatus reaction chamber is silane, the flow velocity of silane be 10sccm~
100sccm, the inlet period of silane are 0.5s~1s.
2. the method for Zr alloy surface graphene Passivation Treatment corrosion-inhibiting coating according to claim 1, described by zircaloy
It is placed in the reaction chamber of microwave plasma CVD equipment, when cavity is evacuated to 1Pa or less, is further passed through
The hydrogen of 100sccm adjusts microwave power to 1300W, and cavity air pressure is maintained at 2.6kPa, bombards zircaloy by hydrogen plasma
Substrate is heated and is removed the impurity on surface by 30min.
3. the method for Zr alloy surface graphene Passivation Treatment corrosion-inhibiting coating according to claim 1, described to be passed through methane
And regulating gas ratio starts to grow graphene film, further sedimentation time is 120s, and depositing temperature is 550 DEG C, gas
Flow methane/hydrogen is 1/60, and cavity air pressure is 4.0kPa, and microwave power is 1300W.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710026560.8A CN106835067B (en) | 2017-01-14 | 2017-01-14 | A kind of method of Zr alloy surface graphene Passivation Treatment corrosion-inhibiting coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710026560.8A CN106835067B (en) | 2017-01-14 | 2017-01-14 | A kind of method of Zr alloy surface graphene Passivation Treatment corrosion-inhibiting coating |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106835067A CN106835067A (en) | 2017-06-13 |
| CN106835067B true CN106835067B (en) | 2019-01-22 |
Family
ID=59124222
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710026560.8A Active CN106835067B (en) | 2017-01-14 | 2017-01-14 | A kind of method of Zr alloy surface graphene Passivation Treatment corrosion-inhibiting coating |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106835067B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109201021B (en) * | 2018-11-26 | 2019-09-27 | 西安科技大学 | A kind of gas adsorption agent and preparation method thereof |
| CN109797374A (en) * | 2019-01-15 | 2019-05-24 | 芜湖启迪半导体有限公司 | A kind of preparation method and its batch preparation of silicon carbide substrates |
| CN109852944B (en) * | 2019-01-25 | 2020-08-04 | 中国科学院半导体研究所 | Graphene preparation method based on microwave plasma chemical vapor deposition |
| CN113076640B (en) * | 2021-03-31 | 2022-06-10 | 中国核动力研究设计院 | Zirconium-based alloy irradiation damage software simulation system and method based on cluster dynamics |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090174435A1 (en) * | 2007-10-01 | 2009-07-09 | University Of Virginia | Monolithically-Integrated Graphene-Nano-Ribbon (GNR) Devices, Interconnects and Circuits |
| US8198707B2 (en) * | 2009-01-22 | 2012-06-12 | Board Of Regents, The University Of Texas System | Establishing a uniformly thin dielectric layer on graphene in a semiconductor device without affecting the properties of graphene |
| CN102304701A (en) * | 2011-09-26 | 2012-01-04 | 中国科学院微电子研究所 | Preparation method of silicon carbide film |
| CN104143576A (en) * | 2014-08-08 | 2014-11-12 | 苏州宏久航空防热材料科技有限公司 | Solar photovoltaic silicon wafer with CVD graphene-SiC film |
| CN105220128B (en) * | 2015-11-16 | 2018-03-16 | 哈尔滨工业大学 | A kind of preparation method of Zr alloy surface original position vertical-growth graphene anticorrosive coat |
-
2017
- 2017-01-14 CN CN201710026560.8A patent/CN106835067B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN106835067A (en) | 2017-06-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106835067B (en) | A kind of method of Zr alloy surface graphene Passivation Treatment corrosion-inhibiting coating | |
| CN107785241B (en) | A method of preparing beta-gallium oxide film on a silicon substrate | |
| CN102534808B (en) | Method for obtaining high-quality silicon carbide surfaces | |
| CN104313684A (en) | Method for preparing hexagonal boron nitride (h-BN) two-dimensional atomic crystal | |
| CN106756870A (en) | A kind of method that plasma enhanced chemical vapor deposition grows Graphene | |
| CN105274500A (en) | Method for preparing graphene through plasma-enhanced chemical vapor deposition | |
| CN108871890A (en) | A method of TEM sample is prepared using graphene as protective layer | |
| CN105624642A (en) | Method for directly depositing diamond film on graphite substrate | |
| CN105800602A (en) | Method for directly growing graphene on insulating substrate through remote catalysis of copper particle | |
| CN105441902A (en) | Epitaxial silicon carbide-graphene composite film preparation method | |
| CN103352202A (en) | Controllable preparation method of normal-pressure chemical-vapor-deposition large-area high-quality double-layer graphene film | |
| CN103924208A (en) | Method for preparing multilayer graphene thin film | |
| CN107188161A (en) | Graphene and preparation method thereof | |
| CN105439126B (en) | A kind of grade single crystal graphene preparation method | |
| CN106517165A (en) | Method for growing graphene by metal-assisted internal/external carbon sources combination mode on 6H/4H-SiC silicon surface | |
| Peng et al. | Influence of radiofrequency power on compositional, structural and optical properties of amorphous silicon carbonitride films | |
| CN110468384B (en) | Diffusion-resistant layer of single-crystal high-temperature alloy and coating interface and preparation method thereof | |
| CN106835066A (en) | A kind of method of metal surface Graphene Passivation Treatment corrosion-inhibiting coating | |
| CN104477995B (en) | A kind of MoO2the preparation method of nanometer sheet and MoO2nanometer sheet | |
| Sato et al. | Network structure of a-SiO: H layers fabricated by plasma-enhanced chemical vapor deposition: Comparison with a-SiC: H layers | |
| Zhou et al. | Mechanochemical grinding diamond film using titanium-coated diamond active abrasives prepared by vacuum micro-evaporation coating | |
| Wang et al. | CVD diamond films as wear-resistant coatings for relief valve components in the coal liquefaction equipment | |
| CN113529166B (en) | Method for growing large-area diamond single crystal | |
| CN103165469A (en) | Preparing method of side grid graphene transistor on silicon (Si) substrate based on copper (Cu) membrane annealing | |
| CN107761071A (en) | The preparation method of zero defect peak graphene film |
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 |