CN109594060A - A kind of preparation method of fine grain silicon carbide clad - Google Patents

A kind of preparation method of fine grain silicon carbide clad Download PDF

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Publication number
CN109594060A
CN109594060A CN201811222217.1A CN201811222217A CN109594060A CN 109594060 A CN109594060 A CN 109594060A CN 201811222217 A CN201811222217 A CN 201811222217A CN 109594060 A CN109594060 A CN 109594060A
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preparation
gas
silicon carbide
fine
clad
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CN201811222217.1A
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张锋
林俊
杨旭
李子威
王鹏
朱智勇
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Shanghai Institute of Applied Physics of CAS
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Shanghai Institute of Applied Physics of CAS
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Priority to CN201811222217.1A priority Critical patent/CN109594060A/en
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—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
    • C23C16/442—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 fluidised bed process
    • 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
    • C23C16/22—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
    • C23C16/56—After-treatment
    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21C—NUCLEAR REACTORS
    • G21C21/00—Apparatus or processes specially adapted to the manufacture of reactors or parts thereof
    • G21C21/02—Manufacture of fuel elements or breeder elements contained in non-active casings
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E30/00—Energy generation of nuclear origin
    • Y02E30/30—Nuclear fission reactors

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Plasma & Fusion (AREA)
  • General Engineering & Computer Science (AREA)
  • High Energy & Nuclear Physics (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Chemical Vapour Deposition (AREA)

Abstract

The present invention relates to a kind of preparation methods of fine grain silicon carbide clad, include the following steps: S1, provide substrate；Temperature is set as 1150-1250 DEG C in fluidized-bed chemical vapor deposition device by S2, it is passed through methyl trichlorosilane steam, carrier band gas is hydrogen and argon gas gaseous mixture, obtains being coated on the silicon carbide layer in substrate, wherein, volume fraction accounting of the hydrogen in carrier band gas is 12%-18%；S3, the high annealing at ar gas environment and 1400-1600 DEG C obtain fine and close fine grain silicon carbide clad.The preparation method of fine grain silicon carbide clad according to the present invention, is not related to reaction gas propylene, so as to avoid the introduced carbon impurity of propylene in the prior art.In fact, the present invention will not introduce corresponding silicon impurities, to obtain the pure phase β-SiC clad of grain refining by reducing temperature and adjusting carrier band gas.

Description

A kind of preparation method of fine grain silicon carbide clad
Technical field
The present invention relates to nuclear material preparation technical fields, relate more specifically to a kind of preparation of fine grain silicon carbide clad Method.
Background technique
Coated fuel particles are due to its intrinsic safety, in very high temperature gas cooled reactor, molten salt reactor, small modular reactor Have wide practical use in equal forth generations reaction.Coated fuel particles are respectively by fuel core, loose pyrolysis layer of charcoal (buffer), interior fine and close pyrolytic carbon layer (IPyC), silicon carbide layer (SiC layer) and outer fine and close pyrolytic carbon layer (OPyC) form.Wherein SiC layer has resistance to neutron irradiation, the burn into of resistance to fission products high-temperature thermodynamics characteristic of good performance, therefore SiC is cladding The key stratum structure of grain.Not only it is used to stop fission gas and metal fission product to external diffusion, also there is load bearing work With being the first barrier of reactor safety.
Research shows that: the SiC involucrum of fine grain can effectively improve its mechanical property, significantly reduce fission product Ag diffusion and The chemical erosion of Pd.Therefore it is directed to coated particle, in the SiC for preparing submicron order crystal grain (100nm-1 μm) proposed in recent years Involucrum is the most effective most direct method for promoting SiC involucrum performance.The method for preparing fine grain SiC clad at present usually exists Propylene is added in reaction gas, to crack the carbon of generation under propylene high-temperature as the crystalline substance for reducing SiC layer in a manner of heterogeneous forming core Particle size.However, the method is easy to introduce carbon impurity in SiC clad, SiC layer purity is reduced.
Summary of the invention
In order to solve the above-mentioned problems of the prior art, the present invention is intended to provide a kind of fine grain silicon carbide clad Preparation method.
The preparation method of fine grain silicon carbide clad of the present invention, includes the following steps: S1, provides substrate；S2, In fluidized-bed chemical vapor deposition device, temperature is set as 1150-1250 DEG C, is passed through methyl trichlorosilane steam, is carried Gas is hydrogen and argon gas gaseous mixture, obtains being coated on the silicon carbide layer in substrate, wherein volume of the hydrogen in carrier band gas Score accounting is 12%-18%；S3, the high annealing at ar gas environment and 1400-1600 DEG C obtain fine and close fine grain carbonization Silicon clad.
Wherein, the structure of silicon carbide layer is influenced by reaction temperature, carrier band gas composition and annealing temperature, by adjusting technique Parameter, available crystallite dimension less than the grain refining of 1 micron (such as between 150-250nm) pure phase β-SiC clad, That is, by the way that depositing temperature is selected as 1150-1250 DEG C, while volume fraction accounting of the hydrogen in carrier band gas being selected as 12%-18%, and annealing temperature is selected as 1400-1600 DEG C, fine and close fine grain silicon carbide clad can be obtained.Tool Body, the application is by being reduced to 1150-1250 DEG C for depositing temperature, so that atomic surface mobility is lower, to obtain crystalline substance The lesser silicon carbide of grain；The brought incomplete problem of reaction is reduced for temperature, the application is by carrying gas for hydrogen Volume fraction accounting in body is selected as 12%-18%, inhibits SiCl caused by reaction not exclusively using hydrogen2Equal silane Class impurity, to eliminate the silicon impurities in silicon carbide layer；The poor problem of brought crystallinity, the application are reduced for temperature By the way that annealing temperature is selected as 1400-1600 DEG C, to eliminate the defects of crystal, crystallinity is improved.In fact, the application Step S2 in methyl trichlorosilane reaction generate SiC during, be decomposed into CH first4, CH3Cl, C2H4In carbon containing Between product, SiCl2, SiCl4, HSiCl3Etc. siliceous intermediate product, these intermediate products further react the decomposition for generating SiC, By the way that volume fraction accounting of the hydrogen in carrier band gas is selected as 12%-18%, the centre in reaction process can be influenced The decomposition of product, so that the amount of the siliceous intermediate product in reaction process reduces, so that silicon impurities can not be formed.Moreover, Annealing temperature in the step S3 of the application is it is also contemplated that the purity of clad, because β-SiC is being higher than 1600 DEG C of temperature Easily it is changed into α-SiC down.
The step S1 includes: S11a, provides fuel core；S12a is firing in fluidized-bed chemical vapor deposition device Loose pyrolysis layer of charcoal is coated in material core；S13a is coated in loose pyrolysis layer of charcoal in fluidized-bed chemical vapor deposition device Interior densification pyrolytic carbon layer is to provide substrate.
The fuel core is UO2。
In the step S12a, temperature is set as 1450 DEG C, is passed through reaction gas acetylene, obtains being coated on fuel kernel Loose pyrolytic carbon layer on core.
In the step S13a, temperature is set as 1260 DEG C, the mixed gas of propylene and argon gas is passed through, is coated Interior fine and close pyrolytic carbon layer on loose pyrolytic carbon layer.
The step S2 further include: in fluidized-bed chemical vapor deposition device, cladding is outer fine and close hot on the silicon carbide layer Solve carbon-coating.
In the step S2, temperature is set as 1260 DEG C, the mixed gas of propylene and argon gas is passed through, is coated on Outer fine and close pyrolytic carbon layer on silicon carbide layer.
The step S1 includes: S11b, provides substrate；S12b is polished directly to provide substrate substrate surface.
In the step S2, hydrogen flowing quantity 1.2-1.5L/min, argon flow 8.5-8.8L/min.It is excellent at one In the embodiment of choosing, the flow of methyl trichlorosilane steam is 45g/h.
The preparation method of fine grain silicon carbide clad according to the present invention, is not related to reaction gas propylene, to avoid Propylene in the prior art introduced carbon impurity.In fact, the present invention is by reduction temperature and adjusts carrier band gas, also not Corresponding silicon impurities can be introduced, to obtain the pure phase β-SiC clad of grain refining.In short, fine grain carbon according to the present invention The preparation method of SiClx clad, simple process is controllable, high yield rate, is suitble to large-scale production.
Detailed description of the invention
Fig. 1 is the XRD spectrum of the fine grain SiC clad of coated fuel particles according to the present invention；
Fig. 2 is the Raman spectrum of the fine grain SiC clad of the coated fuel particles；
Fig. 3 is the surface electron microscope of the fine grain SiC clad of the coated fuel particles；
Fig. 4 is the cross-section diagram of the fine grain SiC clad of the coated fuel particles.
Specific embodiment
With reference to the accompanying drawing, presently preferred embodiments of the present invention is provided, and is described in detail.
Embodiment 1: the UO of about 500 microns of diameter of cladding2.Fine grain SiC layer is prepared at 1150 DEG C
The cladding work of clad carries out in fluidized-bed chemical vapor deposition device, and fluidized bed chemical vapor sinks first Product device is heated to 1450 DEG C under an argon atmosphere, and being passed through reaction gas is acetylene, and carrier gas argon gas is coated the time 2 minutes, obtained Loose pyrolytic carbon layer.Temperature is reduced to 1260 DEG C, the mixed gas of propylene and argon gas is passed through, the reaction time 10 minutes, obtains Interior densification pyrolytic carbon layer.
Fluidized-bed chemical vapor deposition unit temp is down to 1150 DEG C, is passed through methyl trichlorosilane (MTS) steam, flow For 45g/h, carrier gas is hydrogen and argon gas gaseous mixture, hydrogen flowing quantity 1.5L/min, argon flow 8.5L/min.Reaction time For 3h, SiC clad is obtained, the reaction time can determine according to required SiC layer thickness.Temperature is risen to 1260 DEG C later, is passed through The mixed gas of propylene and argon gas the reaction time 10 minutes, obtains outer fine and close pyrolytic carbon layer.
Preparation gained coated particle is heated to 1500 DEG C, high annealing 10h under ar gas environment, obtains fine and close and is free of miscellaneous The coated fuel particles of the fine grain SiC clad of matter.
Fig. 1 is the XRD spectrum of the fine grain SiC clad of the coated fuel particles, and Fig. 2 is the thin of the coated fuel particles The Raman spectrum of crystal grain SiC clad, wherein β-SiC is contained only in the spectrogram of XRD spectrum and Raman spectrum, without α-SiC or The peak of C, Si illustrate in product without containing these impurity substances.Fig. 3 is the fine grain SiC clad of the coated fuel particles Surface electron microscope, wherein through SiC crystallite dimension known to the scale bar in figure between 150-250nm.Fig. 4 is cladding combustion Expect the cross-section diagram of the fine grain SiC clad of particle, there is no hole on section, illustrates SiC layer densification.
Embodiment 2: SiC plane coating is prepared on graphite substrate surface
Graphite substrate surface is polished directly, is put into after ultrasonic cleaning in fluidized-bed chemical vapor deposition device.
Chemical deposition unit temp is risen to 1250 DEG C, is passed through MTS steam, flow 45g/h, carrier gas is hydrogen and argon gas Gaseous mixture, hydrogen flowing quantity 1.2L/min, argon flow 8.8L/min.Reaction time is 3h, obtains SiC coating, when reaction Between can according to required SiC layer thickness determine.
Preparation gained sample is heated to 1600 DEG C, high annealing 5h under ar gas environment, obtains fine and close and free from foreign meter Fine grain SiC coating.
Above-described, only presently preferred embodiments of the present invention, the range being not intended to limit the invention, of the invention is upper Stating embodiment can also make a variety of changes.Made by i.e. all claims applied according to the present invention and description Simply, equivalent changes and modifications fall within the claims of the invention patent.The not detailed description of the present invention is Routine techniques content.

Claims (10)

1. a kind of preparation method of fine grain silicon carbide clad, which comprises the steps of:
S1 provides substrate；
Temperature is set as 1150-1250 DEG C in fluidized-bed chemical vapor deposition device by S2, is passed through methyl trichlorosilane steaming Vapour, carrier band gas is hydrogen and argon gas gaseous mixture, obtains being coated on the silicon carbide layer in substrate, wherein hydrogen is in carrier band gas In volume fraction accounting be 12%-18%；
S3, the high annealing at ar gas environment and 1400-1600 DEG C obtain fine and close fine grain silicon carbide clad.
2. preparation method according to claim 1, which is characterized in that the step S1 includes:
S11a provides fuel core；
S12a coats loose pyrolysis layer of charcoal in fluidized-bed chemical vapor deposition device in fuel core；
S13a coats interior fine and close pyrolytic carbon layer in loose pyrolysis layer of charcoal in fluidized-bed chemical vapor deposition device to provide Substrate.
3. preparation method according to claim 2, which is characterized in that the fuel core is UO2。
4. preparation method according to claim 2, which is characterized in that in the step S12a, temperature is set as 1450 DEG C, it is passed through reaction gas acetylene, obtains being coated on the loose pyrolytic carbon layer in fuel core.
5. preparation method according to claim 2, which is characterized in that in the step S13a, temperature is set as 1260 DEG C, it is passed through the mixed gas of propylene and argon gas, obtains being coated on the interior fine and close pyrolytic carbon layer on loose pyrolytic carbon layer.
6. preparation method according to claim 2, which is characterized in that the step S2 further include: in fluidized bed chemistry gas In phase precipitation equipment, outer fine and close pyrolytic carbon layer is coated on the silicon carbide layer.
7. preparation method according to claim 6, which is characterized in that in the step S2, temperature is set as 1260 DEG C, it is passed through the mixed gas of propylene and argon gas, obtains coating outer fine and close pyrolytic carbon layer on the silicon carbide layer.
8. preparation method according to claim 1, which is characterized in that the step S1 includes:
S11b provides substrate；
S12b is polished directly to provide substrate substrate surface.
9. preparation method according to claim 8, which is characterized in that the substrate is graphite.
10. preparation method according to claim 1, which is characterized in that in the step S2, hydrogen flowing quantity 1.2- 1.5L/min, argon flow 8.5-8.8L/min.
CN201811222217.1A 2018-10-19 2018-10-19 A kind of preparation method of fine grain silicon carbide clad Pending CN109594060A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111916227A (en) * 2020-08-07 2020-11-10 中国科学院上海应用物理研究所 Metal-coated fuel and preparation method thereof
CN114220561A (en) * 2021-11-10 2022-03-22 华能核能技术研究院有限公司 Preparation method and equipment of surface coating of high-temperature gas cooled reactor absorption ball
CN114349541A (en) * 2021-12-23 2022-04-15 西安交通大学 Preparation method of multilayer ceramic diffusion couple injected with metal ions

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CN105139898A (en) * 2015-06-30 2015-12-09 清华大学 Novel coated fuel particle and preparation method thereof
CN105970185A (en) * 2016-04-22 2016-09-28 苏州派欧技术咨询服务有限公司 Preparation method for carbon nanotube-SiC film
CN106631112A (en) * 2016-12-29 2017-05-10 中国科学院上海应用物理研究所 Preparation method of hollow ceramic microsphere

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CN105139898A (en) * 2015-06-30 2015-12-09 清华大学 Novel coated fuel particle and preparation method thereof
CN105970185A (en) * 2016-04-22 2016-09-28 苏州派欧技术咨询服务有限公司 Preparation method for carbon nanotube-SiC film
CN106631112A (en) * 2016-12-29 2017-05-10 中国科学院上海应用物理研究所 Preparation method of hollow ceramic microsphere

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111916227A (en) * 2020-08-07 2020-11-10 中国科学院上海应用物理研究所 Metal-coated fuel and preparation method thereof
CN114220561A (en) * 2021-11-10 2022-03-22 华能核能技术研究院有限公司 Preparation method and equipment of surface coating of high-temperature gas cooled reactor absorption ball
CN114349541A (en) * 2021-12-23 2022-04-15 西安交通大学 Preparation method of multilayer ceramic diffusion couple injected with metal ions

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