CN108129696A - A kind of hollow SiC/C core-shell particles and its preparation method and application - Google Patents
A kind of hollow SiC/C core-shell particles and its preparation method and application Download PDFInfo
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- CN108129696A CN108129696A CN201711204644.2A CN201711204644A CN108129696A CN 108129696 A CN108129696 A CN 108129696A CN 201711204644 A CN201711204644 A CN 201711204644A CN 108129696 A CN108129696 A CN 108129696A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
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Abstract
The present invention relates to a kind of hollow SiC/C core-shell particles and its preparation method and application, the core-shell particles advantageously reduce density for hollow-core construction, internal layer has resistance to ablation effect for carbon material, outer layer has anti-oxidation characteristics for SiC ceramic, hollow 10~100 μm of the SiC core-shell particles diameter, 1~10 μm of wall thickness, 0.1~0.8g/cm3 of density；The method that the present invention prepares hollow SiC/C core-shell particles, overcome hollow carbosphere inoxidizability insufficient, using CVI methods one layer of indefiniteness of hollow carbosphere outer surface uniform deposition SiC ceramic layer, and it is chosen according to raw material and preparation technology parameter is optimized with preparation process, and pass through a large number of experiments and verified, SiC ceramic layer is enabled completely to coat hollow carbosphere, significantly improves the high-temperature oxidation resistance of carbosphere.
Description
Technical field
The present invention relates to a kind of hollow SiC/C core-shell particles and its preparation method and application, belong to functional composite material skill
Art field.
Background technology
Heat-resistant composite material is advanced thermal protection system (Thermal Protection System, TPS) development and design
Critical material in Novel power system and reenters formula aircraft, space probe vehicle, near space vehicle, reuse
There is immeasurable effect, performance and reliability is that associated power system and aircraft are advanced in the aircraft such as vehicle
One of with the determinant of reliability.With the development of modern space technology, aircraft with High Mach number it is long in atmosphere when
Between maneuvering flight, Aerodynamic Heating amount dramatically increases, and heating time rises appreciably, low to heat-resistant composite material density, resistance to ablation, anti-
The requirement of oxidation is more and more urgent.
Lightweight is the development trend of thermally protective materials, and people put into the light structures design and realization of composite material
Greatly make great efforts.Tiny balloon is due to low-density, high-specific surface area characteristic, also receiving and greatly paying close attention to.Hollow carbon is micro-
Function constituent element of the ball as resin base heat-resistant composite material improves the resistance to ablation characteristics of composite material and reduces the composite material
Density.But under new sustained maneuver flight environment of vehicle, oxidation resistant requirement when which can not meet long.
Invention content
It is an object of the invention to overcome the drawbacks described above of the prior art, a kind of hollow SiC/C core-shell particles are provided, in sky
The SiC ceramic layer of heart carbosphere outer surface one layer of indefiniteness of uniform deposition, can completely coat hollow carbosphere, significantly improve carbon
The high-temperature oxidation resistance of microballoon.
Another object of the present invention is to provide a kind of preparation method of hollow SiC/C core-shell particles.
A further object of the present invention is to provide a kind of application of hollow SiC/C core-shell particles.
The above-mentioned purpose of the present invention is achieved by following technical solution：
A kind of hollow SiC/C core-shell particles, the internal layer of the core-shell particles is hollow carbosphere, and outer layer is SiC ceramic, and
A diameter of 10~100 μm of the core-shell particles, wall thickness are 1~10 μm, and density is 0.1~0.8g/cm3。
In above-mentioned hollow SiC/C core-shell particles, the mass ratio of the hollow carbosphere of internal layer and outer layer SiC ceramic is 1：
0.2~2.
In above-mentioned hollow SiC/C core-shell particles, the molar ratio of Si elements and C element is 40~60 in the SiC ceramic:
60~40.
In above-mentioned hollow SiC/C core-shell particles, the outer layer SiC ceramic is synthesized and is sunk by chemical vapor infiltration method
It accumulates in hollow carbosphere outer surface, obtains the core-shell particles.
In above-mentioned hollow SiC/C core-shell particles, a diameter of 30~60 μm of the core-shell particles, wall thickness be 3~6 μm,
Density is 0.3~0.5g/cm3。
A kind of preparation method of hollow SiC/C core-shell particles, including：
Hollow carbosphere is positioned in cvd furnace, using methyl trichlorosilane MTS as Si sources and C sources, H2And inert gas
For carrier gas, chemical vapor infiltration is carried out according to the deposition parameter of setting, obtains hollow SiC/C core-shell particles；
The deposition parameter includes：Depositing temperature is 1200~1500 DEG C, H2Flow be 300~600ml/min, indifferent gas
Body flow is 200~400ml/min, and methyl trichlorosilane MTS flows are 200~300ml/min, atmosphere pressures for 0.5~
50kPa, sedimentation time are 10~50 hours.
In the preparation method of above-mentioned hollow SiC/C core-shell particles, a diameter of 10~100 μm of the hollow carbosphere,
Wall thickness is 1~10 μm, and density is 0.05~0.25g/cm3。
In the preparation method of above-mentioned hollow SiC/C core-shell particles, Si elements and mole of C element in the SiC ceramic
Than being 40~60:60~40.
In the preparation method of above-mentioned hollow SiC/C core-shell particles, the inert gas is argon gas or helium.
In the preparation method of above-mentioned hollow SiC/C core-shell particles, the diameter of hollow SiC/C core-shell particles that is prepared
It it is 10~100 μm, wall thickness is 1~10 μm, and density is 0.1~0.8g/cm3。
In the preparation method of above-mentioned hollow SiC/C core-shell particles, the hollow SiC/C core-shell particles internal layer being prepared is empty
Heart carbosphere and the mass ratio of outer layer SiC ceramic are 1：0.2~2.
The application of above-mentioned hollow SiC/C core-shell particles, the hollow SiC/C core-shell particles are attached to fibre as function constituent element
It ties up in reinforcement, polymer matrix composites is prepared by RTM techniques.
The application of above-mentioned hollow SiC/C core-shell particles, the hollow SiC/C core-shell particles disperse in resin matrix
It is even, it is used to prepare prepreg.
The present invention has the advantages that compared with prior art：
(1), innovative design of the present invention and a kind of hollow SiC/C core-shell particles of function constituent element are prepared for, which is
Hollow-core construction advantageously reduces density, and internal layer has resistance to ablation effect for carbon material, and outer layer has anti-oxidant spy for SiC ceramic
Property, hollow 10~100 μm of the SiC core-shell particles diameter, 1~10 μm of wall thickness, 0.1~0.8g/cm of density3, the present invention is by right
The rational design of its structure composition is so that the antioxygenic property of core-shell particles significantly improves.
(2), the present invention provides a kind of preparation method of hollow SiC/C core-shell particles, and this method overcomes hollow carbosphere to resist
Oxidisability is insufficient, using CVI methods in the SiC ceramic layer of one layer of indefiniteness of hollow carbosphere outer surface uniform deposition, the present invention
It is chosen according to raw material and preparation process optimizes preparation technology parameter, and pass through a large number of experiments and verified so that
SiC ceramic layer can completely coat hollow carbosphere, significantly improve the high-temperature oxidation resistance of carbosphere.
(3), the hollow SiC/C core-shell particles that the present invention is prepared can adhere to fibre reinforcement as function constituent element
On, polymer matrix composites are prepared by RTM techniques, can both reduce the density of composite material, improve the anti-oxidant of composite material
Characteristic.
(4), the hollow SiC/C core-shell particles that the present invention is prepared can be uniformly dispersed in resin matrix, be used to prepare
Prepreg reduces the density of prepreg, improves anti-oxidation characteristics.
(5), the density of the hollow SiC/C core-shell particles of the present invention is in 0.1~0.8g/cm3Between, by adjusting sedimentation time
It is capable of the density of the flexible modulation tiny balloon, there are good anti-oxidation characteristics.
Description of the drawings
Fig. 1 is the thermal weight loss of hollow carbosphere and hollow SiC/C core-shell particles in air atmosphere in the embodiment of the present invention 2
Curve comparison figure.
Specific embodiment
The present invention is described in further detail in the following with reference to the drawings and specific embodiments：
The hollow SiC/C core-shell particles of the present invention, the internal layers of core-shell particles are hollow carbosphere, and outer layer is SiC ceramic, internal layer
Hollow carbosphere and the mass ratio of outer layer SiC ceramic are 1：0.2~2.And a diameter of the 10 of the hollow SiC/C core-shell particles~
100 μm, wall thickness is 1~10 μm, and density is 0.1~0.8g/cm3.In SiC ceramic the molar ratio of Si elements and C element for 40~
60:60~40.
Above-mentioned outer layer SiC ceramic is synthesized by chemical vapor infiltration method and is deposited on hollow carbosphere outer surface, is obtained
The hollow SiC/C core-shell particles.
It is preferred that：A diameter of 30~60 μm of core-shell particles, wall thickness are 3~6 μm, and density is 0.3~0.5g/cm3。
The preparation method of the hollow SiC/C core-shell particles of the present invention, specifically includes：
Hollow carbosphere is positioned in cvd furnace, using methyl trichlorosilane MTS as Si sources and C sources, H2And inert gas
For carrier gas, chemical vapor infiltration is carried out according to the deposition parameter of setting, obtains hollow SiC/C core-shell particles；
Above-mentioned deposition parameter includes：Depositing temperature is 1200~1500 DEG C, H2Flow be 300~600ml/min, indifferent gas
Body flow is 200~400ml/min, and methyl trichlorosilane MTS flows are 200~300ml/min, atmosphere pressures for 0.5~
50kPa, sedimentation time are 10~50 hours.
A diameter of 10~100 μm of above-mentioned hollow carbosphere, wall thickness are 1~10 μm, and density is 0.05~0.25g/cm3。
The molar ratio of Si elements and C element is 40~60 in SiC ceramic:60~40.Above-mentioned inert gas is argon gas or helium.
A diameter of 10~100 μm of the hollow SiC/C core-shell particles being prepared, wall thickness are 1~10 μm, density 0.1
~0.8g/cm3.The hollow hollow carbosphere of SiC/C core-shell particles internal layer being prepared and the mass ratio of outer layer SiC ceramic are 1：
0.2~2.
The hollow SiC/C core-shell particles being prepared can adhere to as function constituent element on fibre reinforcement, pass through RTM
Technique prepares polymer matrix composites, can both reduce the density of composite material, improves the anti-oxidation characteristics of composite material.This is hollow
SiC/C core-shell particles can be uniformly dispersed in resin matrix, be used to prepare prepreg, reduce the density of prepreg, improve antioxygen
Change characteristic.
Embodiment 1
(1) hollow carbosphere is selected, a diameter of 20 μm, wall thickness is 2 μm, density 0.10g/cm3。
(2) hollow carbosphere is positioned in lower temperature deposition stove, with methyl trichlorosilane (MTS) for Si sources and C sources, H2、
Ar is carrier gas, and chemical vapor infiltration is carried out according to the deposition parameter of setting, and the hollow carbon for obtaining outer surface SiC ceramic enhancing is micro-
Ball；
The deposition parameter includes：Depositing temperature is 1200 DEG C, H2Flow is 350ml/min, and Ar flows are 250ml/
Min, MTS flow are 200ml/min, and atmosphere pressures 5kPa, sedimentation time is 15 hours.
(3) it is made of according to the hollow SiC/C core-shell particles prepared by the above method two parts, be internal layer is respectively hollow
Carbosphere, outer layer are SiC ceramic, and the mass ratio of SiC ceramic layer and hollow carbosphere is 0.3：1, hollow SiC/C core-shell particles
Density is 0.13g/cm3.The SiC ceramic Si elements and the ratio of C element are 40:60.In the hollow SiC/C core-shell particles
SiC ceramic is uniformly wrapped in the outer surface of hollow carbosphere, plays and improves the hollow anti-oxidant oxidation susceptibility of carbosphere.
(4) the function constituent element can adhere on fibre reinforcement, prepares polymer matrix composites by RTM techniques, both may be used
The density of composite material is reduced, the anti-oxidation characteristics of composite material is improved, can also be uniformly dispersed, be used to prepare in resin matrix
Prepreg reduces the density of prepreg, improves anti-oxidation characteristics.
Embodiment 2
(1) hollow carbosphere is selected, a diameter of 50 μm, wall thickness is 5 μm, density 0.20g/cm3；
(2) SiC ceramic is included by CVI methods in the step of hollow carbosphere outside deposition SiC, this method：
Hollow carbosphere is positioned in lower temperature deposition stove, with methyl trichlorosilane (MTS) for Si sources and C sources, H2, Ar be
Carrier gas carries out chemical vapor infiltration according to the deposition parameter of setting, obtains the hollow carbosphere of outer surface SiC enhancings；
The deposition parameter includes：Depositing temperature is 1400 DEG C, H2Flow is 500ml/min, and Ar flows are 300ml/
Min, MTS flow are 200ml/min, and atmosphere pressures 50kPa, sedimentation time is 50 hours.
(3) it is made of according to the hollow SiC/C core-shell particles prepared by the above method two parts, be internal layer is respectively hollow
Carbosphere, outer layer are SiC ceramic, and the mass ratio of SiC ceramic layer and hollow carbosphere is 1：1, hollow SiC/C core-shell particles it is close
It spends for 0.4g/cm3.SiC material Si elements and the ratio of C element are 50:50.SiC ceramic is equal in the hollow SiC/C core-shell particles
The even outer surface for being wrapped in hollow carbosphere.
As shown in Figure 1 for hollow carbosphere in the embodiment of the present invention 2 and hollow SiC/C core-shell particles in air atmosphere
Thermogravimetric curve comparison diagram, solid line is hollow carbosphere in figure, and dotted line is hollow SiC/C core-shell particles, as seen from the figure, high temperature item
(800 degrees Celsius) hollow SiC/C core-shell particles quality retention is 4 times of hollow carbon sphere under part, plays and significantly improves hollow carbon
The effect of microballoon antioxygenic property.
(4) the function constituent element can adhere on fibre reinforcement, prepares polymer matrix composites by RTM techniques, both may be used
The density of composite material is reduced, the anti-oxidation characteristics of composite material is improved, can also be uniformly dispersed, be used to prepare in resin matrix
Prepreg reduces the density of prepreg, improves anti-oxidation characteristics.
Embodiment 3
(1) hollow carbosphere is selected, a diameter of 100 μm, wall thickness is 10 μm, density 0.25g/cm3；
(2) SiC ceramic is included by CVI methods in the step of hollow carbosphere outside deposition SiC, this method：
Hollow carbosphere is positioned in lower temperature deposition stove, with methyl trichlorosilane (MTS) for Si sources and C sources, H2, Ar be
Carrier gas carries out chemical vapor infiltration according to the deposition parameter of setting, obtains the hollow carbosphere of outer surface SiC ceramic enhancing；
The deposition parameter includes：Depositing temperature is 1500 DEG C, H2Flow is 300ml/min, and Ar flows are 300ml/
Min, MTS flow are 200ml/min, and atmosphere pressures 30kPa, sedimentation time is 25 hours.
(3) it is made of according to the hollow SiC/C core-shell particles prepared by the above method two parts, be internal layer is respectively hollow
Carbosphere, outer layer are SiC ceramic, and the mass ratio of SiC ceramic layer and hollow carbosphere is 2：1, hollow SiC/C core-shell particles it is close
It spends for 0.8g/cm3.SiC material Si elements and the ratio of C element are 60:40.SiC ceramic is equal in the hollow SiC/C core-shell particles
The even outer surface for being wrapped in hollow carbosphere plays and improves the hollow anti-oxidant oxidation susceptibility of carbosphere.
(4) the function constituent element can adhere on fibre reinforcement, prepares polymer matrix composites by RTM techniques, both may be used
The density of composite material is reduced, the anti-oxidation characteristics of composite material is improved, can also be uniformly dispersed, be used to prepare in resin matrix
Prepreg reduces the density of prepreg, improves inoxidizability.
The above, best specific embodiment only of the invention, but protection scope of the present invention is not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, the change or replacement that can be readily occurred in,
It should be covered by the protection scope of the present invention.
The content not being described in detail in description of the invention belongs to the known technology of professional and technical personnel in the field.
Claims (13)
1. a kind of hollow SiC/C core-shell particles, it is characterised in that：The internal layer of the core-shell particles is hollow carbosphere, and outer layer is
SiC ceramic, and a diameter of 10~100 μm of the core-shell particles, wall thickness are 1~10 μm, and density is 0.1~0.8g/cm3。
2. hollow SiC/C core-shell particles according to claim 1, it is characterised in that：The hollow carbosphere of internal layer with it is outer
The mass ratio of layer SiC ceramic is 1：0.2~2.
3. hollow SiC/C core-shell particles according to claim 1, it is characterised in that：Si elements and C in the SiC ceramic
The molar ratio of element is 40~60:60~40.
4. the hollow SiC/C core-shell particles according to one of claims 1 to 3, it is characterised in that：The outer layer SiC ceramic
It is synthesized by chemical vapor infiltration method and is deposited on hollow carbosphere outer surface, obtain the core-shell particles.
5. the hollow SiC/C core-shell particles according to one of claims 1 to 3, it is characterised in that：The core-shell particles it is straight
Diameter is 30~60 μm, wall thickness is 3~6 μm, density is 0.3~0.5g/cm3。
6. a kind of preparation method of hollow SiC/C core-shell particles, it is characterised in that including：
Hollow carbosphere is positioned in cvd furnace, using methyl trichlorosilane MTS as Si sources and C sources, H2With inert gas to carry
Gas carries out chemical vapor infiltration according to the deposition parameter of setting, obtains hollow SiC/C core-shell particles；
The deposition parameter includes：Depositing temperature is 1200~1500 DEG C, H2Flow be 300~600ml/min, inert gas flow
It measures as 200~400ml/min, methyl trichlorosilane MTS flows are 200~300ml/min, and atmosphere pressures are 0.5~50kPa,
Sedimentation time is 10~50 hours.
7. the preparation method of hollow SiC/C core-shell particles according to claim 6, it is characterised in that：The hollow carbon is micro-
A diameter of 10~100 μm of ball, wall thickness are 1~10 μm, and density is 0.05~0.25g/cm3。
8. the preparation method of hollow SiC/C core-shell particles according to claim 6, it is characterised in that：In the SiC ceramic
The molar ratio of Si elements and C element is 40~60:60~40.
9. the preparation method of hollow SiC/C core-shell particles according to claim 6, it is characterised in that：The inert gas
For argon gas or helium.
10. the preparation method of hollow SiC/C core-shell particles according to claim 6, it is characterised in that：The sky being prepared
A diameter of 10~100 μm of heart SiC/C core-shell particles, wall thickness are 1~10 μm, and density is 0.1~0.8g/cm3。
11. the preparation method of hollow SiC/C core-shell particles according to claim 6, it is characterised in that：The sky being prepared
The heart hollow carbosphere of SiC/C core-shell particles internal layers and the mass ratio of outer layer SiC ceramic are 1：0.2~2.
12. the application of one of claims 1 to 3 hollow SiC/C core-shell particles, it is characterised in that：The hollow SiC/C cores
Shell microballoon is attached to as function constituent element on fibre reinforcement, and polymer matrix composites are prepared by RTM techniques.
13. the application of one of claims 1 to 3 hollow SiC/C core-shell particles, it is characterised in that：The hollow SiC/C cores
Shell microballoon is uniformly dispersed in resin matrix, is used to prepare prepreg.
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| CN102344294A (en) * | 2011-06-30 | 2012-02-08 | 山东理工大学 | Method for preparing carbon-silicon carbide composite material by using chemical gas-phase permeation method |
| CN106567246A (en) * | 2016-10-31 | 2017-04-19 | 航天材料及工艺研究所 | Method used for preparing SiC reinforced low-density porous carbon fiber thermal insulation composite material via chemical vapor infiltration |
| CN106744965A (en) * | 2016-11-29 | 2017-05-31 | 中国工程物理研究院激光聚变研究中心 | A kind of method for preparing SiC tiny balloons |
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2017
- 2017-11-27 CN CN201711204644.2A patent/CN108129696A/en active Pending
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| CN101003942A (en) * | 2006-12-29 | 2007-07-25 | 哈尔滨工业大学 | Method for preparing coat of silicon carbide on surface of carbon fiber |
| US8105649B1 (en) * | 2007-08-09 | 2012-01-31 | Imaging Systems Technology | Fabrication of silicon carbide shell |
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| CN106567246A (en) * | 2016-10-31 | 2017-04-19 | 航天材料及工艺研究所 | Method used for preparing SiC reinforced low-density porous carbon fiber thermal insulation composite material via chemical vapor infiltration |
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Application publication date: 20180608 |