CN105734956A - Method for preparing silicon dioxide/silicon, oxygen and carbon composition coating on surface of carbon material - Google Patents
Method for preparing silicon dioxide/silicon, oxygen and carbon composition coating on surface of carbon material Download PDFInfo
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- CN105734956A CN105734956A CN201610068486.1A CN201610068486A CN105734956A CN 105734956 A CN105734956 A CN 105734956A CN 201610068486 A CN201610068486 A CN 201610068486A CN 105734956 A CN105734956 A CN 105734956A
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
- D06M11/79—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
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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
- C23C16/22—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
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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
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
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Abstract
The invention discloses a method for preparing a silicon dioxide/silicon, oxygen and carbon composition coating on the surface of a carbon material.Silicon powder and copper powder are mixed according to the Si/Cu mass ratio of 1:2-2:1, anhydrous ethanol is added, ball-milling and drying are performed, and then Si/Cu powder is obtained; the Si/Cu powder is placed in a crucible, the carbon material is flat placed on the crucible, and then the crucible is placed in the middle of a vacuum tube type furnace; argon is introduced, under the normal pressure condition, temperature is raised to 1000-1300 DEG C at the speed of 5 DEG C/min, and an isothermal low-pressure chemical gas-phase reaction method is adopted for preparing the coating; after the temperature of the system is achieved, a vacuum pump is opened, meanwhile argon/air mixed gas is introduced, oxygen partial pressure in the system is 5-50 Pa, and the reaction system is located in a 'micro oxygen' environment.Preprocessing does not need to be performed on the carbon material, and it is guaranteed that the carbon material is not damaged seriously; besides, micro amount of oxygen reacts with Si to release a lot of heat, produced high-activity SiO2 reacts with Si to generate SiO steam, and the SiO steam amount is increased.A method for uniformly depositing the SiO2/SiOC coating on the surface of the carbon material in a controlled mode is provided.
Description
Technical field
The present invention is about preparing carbon material surface coating, particularly to one chemical vapor process in carbon material surface system
The method of prepared silicon dioxide/silica carbon composite coating.
Background technology
SiOC material is by polysiloxanes intermediate product during Pintsch process, is made up of tri-kinds of elements of Si, O, C
Vitreous material, coordination C atom instead of SiO2The position of middle part O, thus the amorphous network of entrance that is connected with Si key
Structure, and make its mechanical performance and thermal stability compared to SiO2Having had the biggest improvement, this is due to can be former with four silicon
The introducing of the carbon atom of sub-bonding promotes [SiO4] skeleton rigidity strengthen, thus cause density, modulus, creep resistant, glass
The performances such as glass transition temperature, chemical stability, high-temperature stability improve, and are suitable as coating material.But SiOC forerunner
Preparation process is complicated, Si and SiO2Being difficult to reaction when temperature is relatively low and generate gas phase SiO, reaction efficiency is substantially reduced, preparation
Expensive, and need first material with carbon element to be modified during material with carbon element coating, affect material with carbon element mechanical property.Zhenyu Ryu
Et al. use SiO2Preparation is reacted by the SiO steam produced with activated carbon fiber at 1200-1300 DEG C with Si mixed powder
SiC fiber, XPS, Raman analysis characterize product and contain SiOxCyPhase, showing that SiOC coating is prepared in this inorganic Si source can
Row.But there is presently no people to make to prepare silica/silicon oxygen carbon composite coating in this way.
Summary of the invention
The purpose of the present invention, be to provide a kind of use silica flour to carry out with the micro amount of oxygen in system reacting in " micro-oxygen environment ",
Carbon material surface uniform, controllable ground deposition SiO2The method of/SiOC coating.The present invention utilizes silica flour reaction in " micro-oxygen environment ",
The most extremely low oxygen content will not make that Si is rapid oxidized is all transformed into SiO2, it is not necessary to material with carbon element is carried out pretreatment,
Ensure that material with carbon element will not be by bigger damage；On the other hand, micro amount of oxygen and Si react the big calorimetric of releasing, local response point
Temperature raises, the SiO that the activity of generation is high2React again generation SiO steam with Si, improve SiO quantity of steam.
The present invention is achieved by following technical solution.
1. the method preparing silica/silicon oxygen carbon composite coating at carbon material surface, has following steps:
(1) silica flour and copper powder being mixed with mass ratio Si/Cu=1:2-2:1, addition dehydrated alcohol, as disperse medium, is placed in
Ball milling 1 hour in ball grinder, to the two mix homogeneously；Take out mixed slurry and be placed in 50 DEG C of drying baker drying, obtain Si/Cu
Uniformly mixed powder；
(2) the Si/Cu powder body of step (1) is placed in alumina crucible, material with carbon element is lain against on alumina crucible
Side, then crucible is placed on the middle part of the boiler tube of aluminium oxide vacuum tube furnace；
(3) in the aluminium oxide vacuum tube furnace of step (2), being passed through argon, argon flow amount is 500mL/min, normal pressure
Under the conditions of, it is warming up to 1000 DEG C～1300 DEG C with 5 DEG C/min, is incubated 1～4h, use the reaction of isothermal low pressure chemical phase
Method prepares coating；
(4) after the system of step (3) reaches 1000 DEG C～1300 DEG C of temperature, opening vacuum pump, the system pressure of making is less than
50kPa, is passed through argon/air mixed gas simultaneously, and wherein argon flow amount is 500mL/min, and air mass flow is 0.25
ML/min, in system, partial pressure of oxygen is 5-50Pa, makes whole reaction system be in " micro-oxygen environment "；Pass through O2With Si
The carbon fiber surface that jointly acts on prepare SiO2/ SiOC coating.
The rotating speed of the ball grinder in described step (1) is 400r/min.
Material with carbon element in described step (2) can be one-dimensional carbon fibre fabric, Two-dimensional Carbon fabric, three-dimensional dimension carbon fiber
Any one in fabric, CNT, carbon nano-tube film or carbon felt.
The aluminium oxide vacuum tube furnace of described step (2) is warming up to 1150 DEG C.
The present invention utilizes silica flour reaction in " micro-oxygen environment ", and on the one hand need not that material with carbon element is carried out pre-treatment ensures C equally
Material will not be by bigger damage；On the other hand, micro amount of oxygen and Si react the big calorimetric of releasing, and local response point temperature raises,
The high SiO of activity produced2React again generation SiO steam with Si, improve SiO quantity of steam.Provide a kind of at carbon material
Uniform, controllable ground, material surface deposition SiO2The method of/SiOC coating.
Accompanying drawing explanation
Fig. 1 is SiO of the present invention2/ SiOC coating preparation facilities schematic diagram；
Fig. 2 is carbon fiber coating layer low power scanogram obtained in embodiment 1；
Fig. 3 is carbon fiber coating layer low power scanogram obtained in embodiment 2.
Detailed description of the invention
The present invention, using silica flour and copper powder (analytical pure) as raw material, by mixing, ball milling, is dried to obtain presoma, will be mixed
Closing powder to be placed in tube furnace, micro amount of oxygen and Si react the big calorimetric of releasing, and local response point temperature raises, and produces activity high
SiO2React again generation SiO steam with Si, improve constantly SiO quantity of steam, make Si slowly aoxidize in " micro-oxygen environment ",
It is partially converted to SiO2, thus deposit SiO at carbon material surface uniform, controllable2/ SiOC coating.
The present invention is done the brightest below in conjunction with specific embodiment.
Embodiment 1
(1) silica flour and copper powder being mixed with mass ratio Si/Cu=44:56, addition dehydrated alcohol, as disperse medium, is placed in ball
With 400r/min rotating speed ball milling 1 hour in grinding jar, to the two mix homogeneously.Take out mixed slurry to be placed in 50 DEG C of drying baker
10h, to drying, obtains the uniform mixed powder of Si/Cu；
(2) Si/Cu powder body is placed in alumina crucible, material with carbon element is lain against above alumina crucible, then by crucible
It is placed in the middle part of the boiler tube of aluminium oxide vacuum tube furnace and (sees Fig. 1)；
(3) being passed through argon in the aluminium oxide vacuum tube furnace of step (2), argon flow amount is 500mL/min, normal pressure bar
Under part, it is warming up to 1150 DEG C with 5 DEG C/min, is incubated 4h, prepares coating with isothermal low pressure chemical phase reaction method；
(4) after the system of step (3) reaches 1150 DEG C, opening vacuum pump, system pressure is less than 50kPa, leads to simultaneously
Entering argon/air mixed gas, argon is carrier gas and diluent gas, and air provides oxygen source, and wherein argon flow amount is 500
ML/min, air mass flow is 0.25mL/min, and in system, partial pressure of oxygen is 5Pa, makes whole reaction system be in " micro-oxygen ring
Border " in；Pass through O2SiO is prepared with the carbon fiber surface that jointly acts on of Si2/ SiOC coating.
Fig. 1 is the morphology characterization of embodiment 1, it can be seen that SiO2/ SiOC uniform coating thickness, surfacing.
Embodiment 2
(1) silica flour and copper powder being mixed with mass ratio Si/Cu=44:56, addition dehydrated alcohol, as disperse medium, is placed in ball
With 400r/min rotating speed ball milling 1 hour in grinding jar, to the two mix homogeneously；Take out mixed slurry to be placed in 50 DEG C of drying baker
10h, to drying, obtains the uniform mixed powder of Si/Cu；
(2) being placed in alumina crucible by Si/Cu powder body, lain against by material with carbon element above alumina crucible, crucible is placed
(Fig. 1 is seen) in the middle part of the boiler tube of aluminium oxide vacuum tube furnace；
(3) being passed through argon in the aluminium oxide vacuum tube furnace of step (2), argon flow amount is 500mL/min, normal pressure bar
Under part, it is warming up to 1300 DEG C with 5 DEG C/min and is incubated 4h, preparing coating with isothermal low pressure chemical phase reaction method；
(4) after the system of step (3) reaches 1300 DEG C, open vacuum pump, make system pressure be less than 50kPa, simultaneously
Being passed through argon/air mixed gas, argon is carrier gas and diluent gas, and air provides oxygen source, and wherein argon flow amount is 500
ML/min, air mass flow is 0.25mL/min, and in system, partial pressure of oxygen is 5Pa, makes whole reaction system be in " micro-oxygen environment "
In.Pass through O2SiO is prepared with the carbon fiber surface that jointly acts on of Si2/ SiOC coating.
Fig. 2 is the morphology characterization of embodiment 2, it can be seen that SiOC/SiO2Coating surface is similar to Fructus Momordicae charantiae surface, and temperature is described
Degree affects coating morphology.
Embodiment 3
(1) silica flour and copper powder being mixed with mass ratio Si/Cu=44:56, addition dehydrated alcohol, as disperse medium, is placed in ball
With 400r/min rotating speed ball milling 1 hour in grinding jar, to the two mix homogeneously.Take out mixed slurry to be placed in 50 DEG C of drying baker
10h, to drying, obtains the uniform mixed powder of Si/Cu；
(2) being placed in alumina crucible by Si/Cu powder body, lain against by material with carbon element above alumina crucible, crucible is placed
(Fig. 1 is seen) in the middle part of the boiler tube of aluminium oxide vacuum tube furnace；
(3) being passed through argon in the aluminium oxide vacuum tube furnace of step (2), argon flow amount is 500mL/min, normal pressure bar
Under part, it is warming up to 1150 DEG C with 5 DEG C/min and is incubated 1h, preparing coating with isothermal low pressure chemical phase reaction method；
(4) after the system of step (3) reaches 1150 DEG C, open vacuum pump, make system pressure be less than 50kPa, simultaneously
Being passed through argon/air mixed gas, argon is carrier gas and diluent gas, and air provides oxygen source, and wherein argon flow amount is 500
ML/min, air mass flow is 0.25mL/min, and in system, partial pressure of oxygen is 50Pa, makes whole reaction system be in " micro-oxygen ring
Border " in；Pass through O2SiO is prepared with the carbon fiber surface that jointly acts on of Si2/ SiOC coating.
Embodiment 4
(1) silica flour and copper powder being mixed with mass ratio Si/Cu=44:56, addition dehydrated alcohol, as disperse medium, is placed in ball
With 400r/min rotating speed ball milling 1 hour in grinding jar, to the two mix homogeneously.Take out mixed slurry to be placed in 50 DEG C of drying baker
10h, to drying, obtains the uniform mixed powder of Si/Cu；
(2) being placed in alumina crucible by Si/Cu powder body, lain against by material with carbon element above alumina crucible, crucible is placed
(Fig. 1 is seen) in the middle part of the boiler tube of aluminium oxide vacuum tube furnace；
(3) being passed through argon in the aluminium oxide vacuum tube furnace of step (2), argon flow amount is 500mL/min, normal pressure bar
Under part, it is warming up to 1300 DEG C with 5 DEG C/min and is incubated 1h, preparing coating with isothermal low pressure chemical phase reaction method；
(4) after the system of step (3) reaches 1300 DEG C, open vacuum pump, make system pressure be less than 50kPa, simultaneously
Being passed through argon/air mixed gas, argon is carrier gas and diluent gas, and air provides oxygen source, and wherein argon flow amount is 500
ML/min, air mass flow is 0.25mL/min, and in system, partial pressure of oxygen is 50Pa, makes whole reaction system be in " micro-oxygen ring
Border " in.Pass through O2SiO is prepared with the carbon fiber surface that jointly acts on of Si2/ SiOC coating；
The above-mentioned description to embodiment is easy for those skilled in the art and is understood that and applies the present invention.It is familiar with this
These embodiments are easily made various amendment by the personnel of art, and General Principle described herein is applied to other
Without through performing creative labour in embodiment.Therefore, the invention is not restricted to embodiment here, those skilled in the art
All should be within protection scope of the present invention according to the announcement of the present invention, the improvement made for the present invention and amendment.
Each raw material cited by the present invention can realize the present invention, and the bound value of raw material, interval value can realize this
Invent, then this is illustrated the most one by one.
Claims (4)
1. the method preparing silica/silicon oxygen carbon composite coating at carbon material surface, has following steps:
(1) silica flour and copper powder being mixed with mass ratio Si/Cu=1:2-2:1, addition dehydrated alcohol, as disperse medium, is placed in
Ball milling 1 hour in ball grinder, to the two mix homogeneously；Take out mixed slurry and be placed in 50 DEG C of drying baker drying, obtain Si/Cu
Uniformly mixed powder；
(2) the Si/Cu powder body of step (1) is placed in alumina crucible, material with carbon element is lain against on alumina crucible
Side, then crucible is placed on the middle part of the boiler tube of aluminium oxide vacuum tube furnace；
(3) in the aluminium oxide vacuum tube furnace of step (2), being passed through argon, argon flow amount is 500mL/min, normal pressure
Under the conditions of, it is warming up to 1000 DEG C～1300 DEG C with 5 DEG C/min, is incubated 1～4h, use the reaction of isothermal low pressure chemical phase
Method prepares coating；
(4) after the system of step (3) reaches 1000 DEG C～1300 DEG C of temperature, opening vacuum pump, the system pressure of making is less than
50kPa, is passed through argon/air mixed gas simultaneously, and wherein argon flow amount is 500mL/min, and air mass flow is 0.25
ML/min, in system, partial pressure of oxygen is 5-50Pa, makes whole reaction system be in " micro-oxygen environment "；Pass through O2With Si
The carbon fiber surface that jointly acts on prepare SiO2/ SiOC coating.
One the most according to claim 1 prepares SiO at carbon material surface2The method of/SiOC coating, its feature exists,
The rotating speed of the ball grinder in described step (1) is 400r/min.
One the most according to claim 1 prepares SiO at carbon material surface2The method of/SiOC coating, its feature exists,
Material with carbon element in described step (2) can be one-dimensional carbon fibre fabric, Two-dimensional Carbon fabric, three-dimensional dimension carbon fibre fabric,
Any one in CNT, carbon nano-tube film or carbon felt.
One the most according to claim 1 prepares SiO at carbon material surface2The method of/SiOC coating, its feature exists,
The aluminium oxide vacuum tube furnace of described step (2) is warming up to 1150 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112830787A (en) * | 2021-01-15 | 2021-05-25 | 天津大学 | Preparation method of amorphous silicon-oxygen-carbon composite ceramic thermal barrier coating |
| CN114875398A (en) * | 2022-04-07 | 2022-08-09 | 西安建筑科技大学 | Rare earth element modified wear-resistant refractory high-entropy alloy coating and preparation method thereof |
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| EP1347080A1 (en) * | 2002-03-13 | 2003-09-24 | VAW Aluminium-Technologie GmbH | Silicon metal lining |
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| CN103101258A (en) * | 2013-01-30 | 2013-05-15 | 哈尔滨工业大学（威海） | SiOC/C laminated composite ceramic and preparation method thereof |
| CN104529401A (en) * | 2015-01-14 | 2015-04-22 | 景德镇陶瓷学院 | Preparing method for silica carbon ceramic material with large-specific surface area micropore and mesoporous |
| CN104752691A (en) * | 2013-12-27 | 2015-07-01 | 北京有色金属研究总院 | Silicon/carbon composite anode material for lithium ion batteries and preparation method thereof |
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| EP1347080A1 (en) * | 2002-03-13 | 2003-09-24 | VAW Aluminium-Technologie GmbH | Silicon metal lining |
| US20060204673A1 (en) * | 2005-03-14 | 2006-09-14 | Masami Takayasu | Semiconductor manufacturing method for inter-layer insulating film |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112830787A (en) * | 2021-01-15 | 2021-05-25 | 天津大学 | Preparation method of amorphous silicon-oxygen-carbon composite ceramic thermal barrier coating |
| CN114875398A (en) * | 2022-04-07 | 2022-08-09 | 西安建筑科技大学 | Rare earth element modified wear-resistant refractory high-entropy alloy coating and preparation method thereof |
| CN114875398B (en) * | 2022-04-07 | 2024-04-19 | 西安建筑科技大学 | Rare earth element modified wear-resistant refractory high-entropy alloy coating and preparation method thereof |
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Address after: 300350 District, Jinnan District, Tianjin Haihe Education Park, 135 beautiful road, Beiyang campus of Tianjin University Patentee after: Tianjin University Address before: 300072 Tianjin City, Nankai District Wei Jin Road No. 92 Patentee before: Tianjin University |
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| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20171027 Termination date: 20220129 |