CN108585954B - Radial nanowire growing on surface of C/C-Si composite material and preparation method at normal temperature - Google Patents
Radial nanowire growing on surface of C/C-Si composite material and preparation method at normal temperature Download PDFInfo
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Abstract
The invention relates to a method for growing radial nanowires on the surface of a C/C-Si composite material and a preparation method thereof at normal temperature. And then, the C/C-Si composite material is put into a mixed solution composed of deionized water, glycerol, hydrogen peroxide and hydrofluoric acid according to different volume fractions for etching for different time. Obtaining Si nanowires radially grown on the surface of the C/C-Si composite material at normal temperature. The nanowire is a radial nanowire growing from the surface of the C/C-Si composite material, and can improve the binding force between an inner coating and an outer coating and relieve thermal expansion mismatch. Can reduce the reduction of mechanical property caused by multiple high-temperature treatments of the carbon/carbon composite material, and can effectively protect the carbon/carbon composite material.
Description
Technical Field
The invention belongs to a coating surface nanowire and a preparation method thereof, and relates to a C/C-Si composite material surface-grown radial nanowire and a preparation method thereof at normal temperature.
Background
Carbon/carbon (C/C) composites have a range of excellent properties, such as low density, corrosion resistance, high specific strength, stable coefficient of friction, good thermal and electrical conductivity, etc. The characteristic that the strength of the composite material is increased along with the temperature rise in a high-temperature environment enables the composite material to be successfully applied to the environment above 2000 ℃ as a high-temperature structure composite material. However, carbon/carbon composites suffer from an important drawback during application: these excellent high temperature properties are only maintained under inert atmosphere protection or below 450 ℃. In an aerobic environment, when the temperature is higher than 450 ℃, the carbon/carbon composite material can be oxidized, so that the mechanical property of the material is reduced sharply. This characteristic of being easily oxidized in an aerobic environment severely limits the practical application of carbon/carbon composites as thermal structural materials. How to solve the problem of oxidation of the carbon/carbon composite material in a high-temperature aerobic environment becomes a key for the application of the carbon/carbon composite material. Currently used securityThe method for protecting the carbon/carbon composite material is to prepare a multilayer antioxidant ceramic coating and a gradient antioxidant ceramic coating on the surface of the carbon/carbon composite material. But due to ceramic coating (ZrC, HfC, TaC, MoSi)2、CrSi2Etc.) and the carbon/carbon composite material have larger difference between the thermal expansion coefficients, so that the bonding force between the ceramic coating and the carbon/carbon composite material is reduced in the application process, and the cracking and peeling phenomena occur. Therefore, how to improve the bonding strength between the ceramic coating and the C/C and alleviate the thermal expansion mismatch problem is the most difficult bottleneck for the high temperature ceramic to break through in the practical application process.
The document "Oxidation protection of C/C compositions by ultra-long Long SiC nanowire-reinforced SiC-Si coating, Yanhui Chu, Hejun Li, Lu Li, Lehua Qi, Corrossion Science 2014 (84): 204-208" describes a method for toughening SiC-Si coatings with ultra-long SiC nanowires to alleviate the problem of thermal expansion mismatch between the coating and the C/C substrate and to improve the Oxidation properties of the coating. The technology shows better high-temperature oxidation resistance to a certain extent. However, since the bond between the nanowire and the SiC-Si coating is a physical bond. The binding force is small, and the prepared nano-wire is easy to fall off under the action of external force. And the nano-wire is prepared by reaction at high temperature, and the mechanical property of the carbon/carbon composite material is greatly damaged by multiple high-temperature treatments.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a C/C-Si composite material surface-grown radial nanowire and a preparation method thereof at normal temperature, which can improve the binding force between an inner coating and a substrate as well as between the inner coating and an outer coating and reduce the mechanical property reduction of the material caused by multiple high-temperature treatments.
Technical scheme
A radial nanowire grows on the surface of a C/C-Si composite material, and is characterized in that: the diameter of the radial nanowire growing along the direction vertical to the Si particle crystal surface is 500-2700nm, and the length of the nanowire is 22-88 μm.
A method for preparing the radial nanowire growing on the surface of the C/C-Si composite material at normal temperature is characterized by comprising the following steps:
step 1, preparing a Si coating on the surface of a carbon/carbon composite material: placing the carbon/carbon composite material in the mixed powder in a graphite crucible;
putting the graphite crucible into a vacuum heating furnace, introducing argon as protective atmosphere, heating at the speed of 5-10 ℃/min, raising the temperature of the furnace from room temperature to 1800-2300 ℃, and preserving the temperature for 1-3 hours; then cooling to room temperature at a cooling speed of 10-20 ℃/min;
taking the crucible out of the heating furnace, taking the carbon/carbon composite material out, ultrasonically cleaning the carbon/carbon composite material for 10-30 min by using water and absolute ethyl alcohol, and drying the carbon/carbon composite material in a drying oven at the temperature of 70-80 ℃ for 12-30h to obtain a C/C-Si composite material;
the mixed powder comprises the following components: mixing Si powder 80-95 wt% and Al 5-20 wt%2O3Mixing the powder, placing the mixture into a rosin ball ink tank, carrying out ball milling treatment for 3-4 h, and drying the mixture in a drying oven at the temperature of 70-80 ℃ for 12-24 h to obtain the rosin ball ink;
step 2, growing radial nanowires on the surface of the Si coating by an etching method:
1. immersing the C/C-Si composite material into concentrated sulfuric acid and hydrogen peroxide with the volume ratio of 1:1 for 2 min; then taking out and putting into the monodisperse polystyrene microsphere solution, and standing for 2-4h in an oven at 50-70 ℃; taking out the C/C-Si composite material, putting the C/C-Si composite material into a culture dish, and naturally drying the C/C-Si composite material for 10 to 20 hours at the room temperature of between 20 and 30 ℃;
2. then putting the C/C-Si composite material into a metal spraying sputtering instrument, and vacuumizing to 4-6 multiplied by 10-2Pa, adjusting the current value to be 8-10mA, and spraying gold for 30-60 s;
3. sequentially putting the C/C-Si composite material treated in the step 2 into the solution A, the solution B and the solution C for etching, wherein the solution etching is carried out for 2-5min each time;
4. drying the etched C/C-Si composite material in an oven at the temperature of 60-80 ℃ for 10-24h, and taking out to obtain the nanowires radially grown on the surface of the Si coating;
each part of the monodisperse polystyrene microsphere solution is as follows: adding 1-2ml of monodisperse polystyrene microsphere solution into 50ml of absolute ethyl alcohol, and ultrasonically stirring and mixing;
each solution A is as follows: mixing 45-62% of deionized water, 6-16% of hydrogen peroxide and 31-47% of hydrofluoric acid solution by volume fraction;
each solution B is as follows: mixing 20-30% of deionized water, 10-30% of glycerol, 0.4-10% of hydrogen peroxide and 20-40% of hydrofluoric acid by volume fraction;
each solution C is: mixing 15-30% of deionized water, 15-30% of glycerol, 3-10% of hydrogen peroxide and 15-40% of hydrofluoric acid by volume fraction;
the concentrated sulfuric acid is a concentrated sulfuric acid solution with the concentration of 98%;
the hydrogen peroxide is hydrogen peroxide solution with the concentration of 35 percent;
the hydrofluoric acid is a hydrofluoric acid solution with the concentration of 40%.
The carbon/carbon composite material is pretreated, polished, ultrasonically cleaned by water and absolute ethyl alcohol in sequence and dried.
The mixed powder in the step 1 is tiled in a graphite crucible, the pretreated carbon/carbon composite material is placed in the graphite crucible, and then the carbon/carbon composite material is covered by the mixed powder; the pretreated carbon/carbon composite material is positioned in the middle of the graphite crucible, and the graphite crucible is filled with the carbon/carbon composite material and the mixed powder.
The particle size of the microspheres in the monodisperse polystyrene microsphere solution in the step 1 is 500nm, and the solid content of the solution is 5%.
The purity of the Si powder is 99.5%, and the granularity is 400 meshes.
The Al is2O3The purity of the powder was 99.5% and the particle size was 300 mesh.
Pretreatment of the carbon/carbon composite material: and sequentially grinding and polishing the carbon/carbon composite material by using No. 180, No. 320 and No. 400 sand paper, then sequentially ultrasonically cleaning for 30-40 min by using water and absolute ethyl alcohol, and drying for 12-30h in a drying oven at 70-80 ℃.
Advantageous effects
The invention provides a method for growing radial nanowires on the surface of a C/C-Si composite material and preparing the C/C-Si composite material at normal temperature, which comprises the steps of preparing a silicon coating on the surface of a carbon/carbon composite material in a vacuum heating furnace by an embedding method to obtain the C/C-Si composite material; the grain size of the Si coating prepared by the invention is 6-16 μm. And then soaking the C/C-Si composite material by adopting a mixed solution of concentrated sulfuric acid and hydrogen peroxide, putting the surface of the C/C-Si composite material into a monodisperse polystyrene microsphere solution, drying, and spraying gold in a gold spraying sputtering instrument. And then, the C/C-Si composite material is put into a mixed solution composed of deionized water, glycerol, hydrogen peroxide and hydrofluoric acid according to different volume fractions for etching for different time. Thus obtaining the Si nanowires radially grown on the surface of the C/C-Si composite material at normal temperature. The nanowire prepared by the method has uniform appearance and is radially increased. The diameter of the nanowire gradually changes along the radial direction. The nanowires are about 22-88 μm in length. The bonding force between the inner coating and the outer coating can be improved and the thermal expansion mismatch can be relieved by utilizing the radial nanowires growing from the surface of the C/C-Si composite material. When the nano-wire is applied in an oxidation or ablation environment, the nano-wire grown from the interior of the material has a better bridging effect. And the radial nanowires prepared on the surface of the C/C-Si composite material at normal temperature can reduce the reduction of mechanical properties of the carbon/carbon composite material caused by multiple high-temperature treatments, and can effectively protect the carbon/carbon composite material.
The invention adopts the mode of etching the Si coating prepared on the surface of the carbon/carbon composite material at normal temperature to prepare the radial nanowire on the surface of the C/C-Si composite material, so that the diameter of the prepared nanowire is about 500-2700nm, and the length of the nanowire is about 22-88 mu m. The nano-wire grows along the direction vertical to the crystal face of the Si particle, and the nano-wire and the composite material are chemically combined. At present, the method for preparing the nanowire on the surface of the C/C composite material mainly comprises an electrophoresis method and an in-situ growth method, the prepared nanowire is physically combined with the composite material (fig. 4a and b), and the in-situ growth method needs to be carried out at a high temperature of 1600-. The radial Si nanowire prepared by the method is prepared at normal temperature, not only has the advantage of good bonding strength, but also has fewer times of high-temperature treatment, and the composite material can keep better high-temperature mechanical property. And because the reaction is carried out at normal temperature, the process flow is greatly simplified, and the energy consumption is reduced. The method can be used for solving the problem of weak binding force between the inner coating and the substrate and between the inner coating and the outer coating.
Drawings
FIG. 1 is an SEM photograph of a Si coating prepared on the surface of a carbon/carbon composite as prepared in example 1
FIG. 2 is SEM photograph of the surface of the nanowire prepared by etching at normal temperature on the surface of the C/C-Si composite material prepared in example 1
FIG. 3 is an SEM photograph of nanowires grown from the surface of a Si coating layer of nanowires prepared by etching at normal temperature on the surface of a C/C-Si composite material prepared in example 2
FIG. 4a is a representation of the prior art documents "Lu Li, Hejun Li, Yunyu Li, Xuemein Yin, Qingliang Shen, Qiangang Fu, A SiC-ZrB2-a cross-sectional SEM photograph of SiC nanowires prepared on the Surface of a C/C composite by electrophoretic deposition as disclosed in ZrC coating by electrophoretic deposition to a deposited SiC nanowire to protect C/C composites against thermal shock and oxidation, Applied Surface Science 349(2015)465- "471;
FIG. 4b is a SEM photograph of a cross section of a SiC nanowire prepared on the surface of a C/C-SiC composite material by an in-situ growth method, which is disclosed in the prior art document, namely, the research on SiC nanowire toughened silicon-based and hafnium-based high-temperature oxidation-resistant and anti-ablation coatings, Ph, university of northwest industries, Ph, 2016:99.
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
reference is made to fig. 1, 2 and 3. The following examples illustrate the growth of radial nanowires on the surface of a C/C-Si composite material at room temperature and illustrate the present invention in detail. The microstructure of the nanowire on the surface of the C/C-Si composite material is controlled by controlling the concentration and time of the etching solution, so that the shape of the nanowire is uniform, and the binding force between the inner coating and the outer coating is improved.
Example 1:
step 1: pre-treated carbon/carbon composites
The density is 1.74g/cm3The carbon/carbon composite material is sequentially polished by 180 # sand paper, 320 # sand paper and 400 # sand paper, then is sequentially ultrasonically cleaned by water and absolute ethyl alcohol for 30min, and is dried at 80 DEG CDrying in a drying box for 12h for later use;
step 2: preparation of Si coating on surface of carbon/carbon composite material
1) Respectively weighing 90% of Si powder and 10% of Al powder by mass percent2O3Putting the powder into a rosin ball ink tank, carrying out ball milling treatment for 4h, and drying in a drying oven at the temperature of 80 ℃ for 12h for later use;
2) laying the mixed powder prepared in the step 1) in a graphite crucible, wherein the thickness of the powder is about 1/2 of the height of the graphite crucible. The pretreated carbon/carbon composite was then placed in a graphite crucible, and the carbon/carbon composite was subsequently covered with a mixed powder having a thickness of about 1/2 a of the height of the graphite crucible.
3) Putting the graphite crucible into a vacuum heating furnace, introducing argon as protective atmosphere, heating at the speed of 5 ℃/min, heating the furnace temperature from room temperature to 2000 ℃, and preserving the temperature for 3 hours; then the temperature is reduced to the room temperature at the speed of 20 ℃/min. And taking the crucible out of the heating furnace, taking the carbon/carbon composite material out, ultrasonically cleaning the carbon/carbon composite material for 20min by using water and absolute ethyl alcohol, and drying the carbon/carbon composite material for 12h in a drying oven at the temperature of 80 ℃ to obtain the C/C-Si composite material.
The purity of the Si powder is 99.5%, and the granularity is 400 meshes.
The Al is2O3The purity of the powder was 99.5% and the particle size was 300 mesh.
And step 3: growing radial nano-wire on the surface of Si coating by etching method
1) 50ml of absolute ethyl alcohol is put into a beaker, then 1ml of monodisperse polystyrene microsphere solution (with the particle size of 500nm and the solid content of 5%) is taken by a straw and added into the absolute ethyl alcohol, and the mixture is stirred for 10min by ultrasonic wave for standby.
2) The prepared C/C-Si composite material is immersed in a mixed solution of concentrated sulfuric acid and hydrogen peroxide in a volume ratio of 1:1 for 2 min. Then taking out and putting into the prepared monodisperse polystyrene microsphere solution, and standing in an oven at 50 ℃ for 2 h. Taking out the C/C-Si composite material, putting the C/C-Si composite material into a culture dish, and naturally drying the C/C-Si composite material for 12 hours at the room temperature of 25 ℃.
3) Putting the C/C-Si composite material into a metal spraying sputtering instrument, and vacuumizing to 5 multiplied by 10-2Pa, and adjusting the current value to 10 mA. And spraying gold for 50 s. Then taking the C/C-Si composite materialAnd (6) discharging.
4) Deionized water with the volume fraction of 50%, 6% hydrogen peroxide and 44% hydrofluoric acid solution are respectively taken to prepare a solution A.
And preparing a solution B by using 30% of deionized water, 25% of glycerol, 5% of hydrogen peroxide and 40% of hydrofluoric acid in percentage by volume.
A solution C is prepared from 25% by volume of deionized water, 30% by volume of glycerol, 10% by volume of hydrogen peroxide and 35% by volume of hydrofluoric acid.
The concentrated sulfuric acid is a concentrated sulfuric acid solution with the concentration of 98%.
The hydrogen peroxide is hydrogen peroxide solution with the concentration of 35%.
The hydrofluoric acid is a hydrofluoric acid solution with the concentration of 40%.
5) And sequentially placing the C/C-Si composite material into the A-B-C-B-A solution, wherein the etching time is respectively 3min, 5min, 2min, 3min and 2 min.
6) And drying the etched C/C-Si composite material in an oven at 60 ℃ for 24 hours. And taking out the C/C-Si composite material to obtain the nanowires radially grown on the surface of the Si coating.
Example 2
Step 1: pre-treated carbon/carbon composites
The density is 1.72g/cm3Sequentially grinding and polishing the carbon/carbon composite material by 180 # sand paper, 320 # sand paper and 400 # sand paper, then sequentially ultrasonically cleaning the composite material by water and absolute ethyl alcohol for 35min, and drying the composite material in a drying oven at the temperature of 80 ℃ for 24h for later use;
step 2: preparation of Si coating on surface of carbon/carbon composite material
1) Respectively weighing 85% of Si powder and 15% of Al powder by mass percent2O3Putting the powder into a rosin ball ink tank, carrying out ball milling treatment for 3h, and drying for 24h in a drying oven at 70 ℃ for later use;
2) laying the mixed powder prepared in the step 1) in a graphite crucible, wherein the thickness of the powder is about 1/2 of the height of the graphite crucible. The pretreated carbon/carbon composite was then placed in a graphite crucible, and the carbon/carbon composite was subsequently covered with a mixed powder having a thickness of about 1/2 a of the height of the graphite crucible.
3) Putting the graphite crucible into a vacuum heating furnace, introducing argon as protective atmosphere, heating at the speed of 10 ℃/min, heating the furnace temperature to 2200 ℃ from room temperature, and preserving the temperature for 2 hours; then the temperature is reduced to room temperature at the speed of 20 ℃/min. And taking the crucible out of the heating furnace, taking the carbon/carbon composite material out, ultrasonically cleaning the carbon/carbon composite material for 30min by using water and absolute ethyl alcohol, and drying the carbon/carbon composite material for 12h in a drying oven at the temperature of 80 ℃ to obtain the C/C-Si composite material.
The purity of the Si powder is 99.5%, and the granularity is 400 meshes.
The Al is2O3The purity of the powder was 99.5% and the particle size was 300 mesh.
And step 3: growing radial nano-wire on the surface of Si coating by etching method
1) 50ml of absolute ethyl alcohol is put into a beaker, then 2ml of monodisperse polystyrene microsphere solution (with the particle size of 500nm and the solid content of 5%) is taken by a straw and added into the absolute ethyl alcohol, and the mixture is stirred for 5min by ultrasonic wave for standby.
2) The prepared C/C-Si composite material is immersed in concentrated sulfuric acid and hydrogen peroxide with the volume ratio of 1:1 for 2 min. Then taking out and putting into the prepared monodisperse polystyrene microsphere solution, and standing for 4 hours in an oven at 70 ℃. Taking out the C/C-Si composite material, putting the C/C-Si composite material into a culture dish, and naturally drying the C/C-Si composite material for 10 hours at the room temperature of 25 ℃.
3) Putting the C/C-Si composite material into a metal spraying sputtering instrument, and vacuumizing to 5 multiplied by 10-2Pa, and adjusting the current value to 10 mA. And spraying gold for 60 s. And then taking out the C/C-Si composite material.
4) Deionized water with the volume fraction of 50%, hydrogen peroxide with the volume fraction of 16% and hydrofluoric acid solution with the volume fraction of 34% are respectively taken to prepare the solution A.
And preparing a solution B by using 30% of deionized water, 25% of glycerol, 10% of hydrogen peroxide and 35% of hydrofluoric acid in percentage by volume.
A solution C is prepared from deionized water with the volume fraction of 25%, glycerol with the volume fraction of 30%, hydrogen peroxide with the volume fraction of 5% and hydrofluoric acid with the volume fraction of 40%.
The concentrated sulfuric acid is a concentrated sulfuric acid solution with the concentration of 98%.
The hydrogen peroxide is hydrogen peroxide solution with the concentration of 35%.
The hydrofluoric acid is a hydrofluoric acid solution with the concentration of 40%.
5) And sequentially placing the C/C-Si composite material into the A-B-C-B-A solution for etching for 3min, 5min, 2min, 3min and 2min respectively.
6) And drying the etched C/C-Si composite material in an oven at 80 ℃ for 12 hours. And taking out the C/C-Si composite material to obtain the nanowires radially grown on the surface of the Si coating.
Fig. 1 is an SEM photograph of the Si coating prepared on the surface of the carbon/carbon composite prepared in example 1. It can be seen that the Si coating prepared on the surface of the carbon/carbon composite material is compact, the particles are uniform and fine, and the particle size is about 6-16 μm. The combination among the particles is better.
FIG. 2 is an SEM photograph of the surface of the nanowire prepared in example 1 and etched at normal temperature on the surface of the C/C-Si composite material. It can be seen that the nanowires prepared on the surface of the C/C-Si composite material after etching treatment have uniform morphology and radially increase. The diameter of the nanowire gradually becomes thicker along the radial direction. The nanowires are about 22-88 μm in length.
FIG. 3 is SEM photograph of the surface of the nanowire prepared in example 2 by etching at room temperature on the surface of the C/C-Si composite material, and it can be seen that the nanowire grows out of the surface of the Si coating layer and is chemically bonded to the Si coating layer.
FIGS. 4a and b are SEM images of cross-sections of a SiC nanowire prepared on the surface of a C/C composite material by an electrophoretic deposition method (FIG. 4a) and a SiC nanowire prepared on the surface of a C/C-SiC composite material by an in-situ growth method (FIG. 4b), respectively, in the prior art. The nanowires can be seen to float on the surface of the C/C composite, C/C-SiC composite. The binding force is weaker than that of the nanowires grown from the coating itself (fig. 3).
Claims (7)
1. A preparation method for growing radial nanowires on the surface of a C/C-Si composite material is characterized by comprising the following steps: the diameter of the radial nanowire growing along the direction vertical to the crystal plane of the Si particle is 500-2700nm, and the length of the nanowire is 22-88 μm;
the preparation method comprises the following specific steps:
step 1, preparing a Si coating on the surface of a carbon/carbon composite material: placing the carbon/carbon composite material in the mixed powder in a graphite crucible;
putting the graphite crucible into a vacuum heating furnace, introducing argon as protective atmosphere, heating at the speed of 5-10 ℃/min, raising the temperature of the furnace from room temperature to 1800-2300 ℃, and preserving the temperature for 1-3 hours; then cooling to room temperature at a cooling rate of 10-20 ℃/min;
taking the crucible out of the heating furnace, taking the carbon/carbon composite material out, ultrasonically cleaning the carbon/carbon composite material for 10-30 min by using water and absolute ethyl alcohol, and drying the carbon/carbon composite material in a drying oven at the temperature of 70-80 ℃ for 12-30h to obtain a C/C-Si composite material;
the mixed powder comprises the following components: mixing Si powder 80-95 wt% and Al 5-20 wt%2O3Mixing the powder, placing the mixture into a rosin ball milling tank, carrying out ball milling treatment for 3-4 h, and drying the mixture in a drying oven at the temperature of 70-80 ℃ for 12-24 h to obtain the rosin-containing oil;
step 2, growing radial nanowires on the surface of the C/C-Si composite material coating by an etching method:
(1) immersing the C/C-Si composite material into concentrated sulfuric acid and hydrogen peroxide with the volume ratio of 1:1 for 2 min; then taking out and putting into a monodisperse polystyrene microsphere solution, and standing for 2-4h in an oven at 50-70 ℃; taking out the C/C-Si composite material, putting the C/C-Si composite material into a culture dish, and naturally drying the C/C-Si composite material for 10 to 20 hours at the room temperature of between 20 and 30 ℃;
(2) then putting the C/C-Si composite material into a metal spraying sputtering instrument, and vacuumizing to 4-6 multiplied by 10-2Pa, adjusting the current value to be 8-10mA, and spraying gold for 30-60 s;
(3) sequentially placing the C/C-Si composite material treated in the step (2) into the solution A, the solution B and the solution C for etching, wherein the solution etching is carried out for 2-5min each time;
(4) drying the etched C/C-Si composite material in an oven at the temperature of 60-80 ℃ for 10-24h, and taking out to obtain the nanowires radially grown on the surface of the Si coating;
the monodisperse polystyrene microsphere solution is prepared by the following steps: adding 1-2ml of monodisperse polystyrene microsphere solution into 50ml of absolute ethyl alcohol, and ultrasonically stirring and mixing;
the solution A is: mixing 45-62% of deionized water, 6-16% of hydrogen peroxide and 31-47% of hydrofluoric acid solution by volume fraction;
the solution B is: mixing 20-30% of deionized water, 10-30% of glycerol, 0.4-10% of hydrogen peroxide and 20-40% of hydrofluoric acid by volume fraction;
the solution C is: mixing 15-30% of deionized water, 15-30% of glycerol, 3-10% of hydrogen peroxide and 15-40% of hydrofluoric acid by volume fraction;
the concentrated sulfuric acid is a concentrated sulfuric acid solution with the concentration of 98%;
the hydrogen peroxide is hydrogen peroxide solution with the concentration of 35 percent;
the hydrofluoric acid is a hydrofluoric acid solution with the concentration of 40%.
2. The method for preparing radial nanowires grown on the surface of the C/C-Si composite material according to claim 1, wherein the method comprises the following steps: the carbon/carbon composite material is pretreated, polished, ultrasonically cleaned by water and absolute ethyl alcohol in sequence and dried.
3. The method for preparing radial nanowires grown on the surface of the C/C-Si composite material according to claim 1, wherein the method comprises the following steps: the mixed powder in the step 1 is tiled in a graphite crucible, the pretreated carbon/carbon composite material is placed in the graphite crucible, and then the carbon/carbon composite material is covered by the mixed powder; the pretreated carbon/carbon composite material is positioned in the middle of the graphite crucible, and the graphite crucible is filled with the carbon/carbon composite material and the mixed powder.
4. The method for preparing radial nanowires grown on the surface of the C/C-Si composite material according to claim 1, wherein the method comprises the following steps: the particle size of the microspheres in the monodisperse polystyrene microsphere solution in the step 2 is 500nm, and the solid content of the solution is 5%.
5. The method for preparing radial nanowires grown on the surface of the C/C-Si composite material according to claim 1, wherein the method comprises the following steps: the purity of the Si powder is 99.5%, and the granularity is 400 meshes.
6. The method for preparing radial nanowires grown on the surface of the C/C-Si composite material according to claim 1, wherein the method comprises the following steps: the Al is2O3The purity of the powder was 99.5% and the particle size was 300 mesh.
7. The method for preparing radial nanowires grown on the surface of the C/C-Si composite material according to claim 2, wherein the method comprises the following steps: pretreatment of the carbon/carbon composite material: and sequentially grinding and polishing the carbon/carbon composite material by using No. 180, No. 320 and No. 400 sand paper, then sequentially ultrasonically cleaning for 30-40 min by using water and absolute ethyl alcohol, and drying for 12-30h in a drying oven at 70-80 ℃.
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| CN101891145A (en) * | 2009-05-22 | 2010-11-24 | 熊长宏 | Silicon nanowire preparation by gas-liquid-solid phase method |
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| CN107903067A (en) * | 2017-12-01 | 2018-04-13 | 苏州宏久航空防热材料科技有限公司 | A kind of growth in situ SiC nanowire enhancing SiC ceramic based composites and preparation method thereof |
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| CN101891145A (en) * | 2009-05-22 | 2010-11-24 | 熊长宏 | Silicon nanowire preparation by gas-liquid-solid phase method |
| CN103553616A (en) * | 2013-10-23 | 2014-02-05 | 中国科学院上海硅酸盐研究所 | In-situ growth SiC nanowire enhanced C/SiC composite material and preparation method thereof |
| CN107032816A (en) * | 2017-05-10 | 2017-08-11 | 西北工业大学 | A kind of silicon carbide nanometer line enhancing C/C SiC ZrB2The preparation method of ceramic matric composite |
| CN107903067A (en) * | 2017-12-01 | 2018-04-13 | 苏州宏久航空防热材料科技有限公司 | A kind of growth in situ SiC nanowire enhancing SiC ceramic based composites and preparation method thereof |
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