CN112608156B - Preparation method of micro-nano mixed SiC chopped fibers - Google Patents
Preparation method of micro-nano mixed SiC chopped fibers Download PDFInfo
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- CN112608156B CN112608156B CN202011607278.7A CN202011607278A CN112608156B CN 112608156 B CN112608156 B CN 112608156B CN 202011607278 A CN202011607278 A CN 202011607278A CN 112608156 B CN112608156 B CN 112608156B
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- 239000000835 fiber Substances 0.000 title claims abstract description 123
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims description 82
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 70
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 56
- 229910052710 silicon Inorganic materials 0.000 claims description 46
- 239000010703 silicon Substances 0.000 claims description 46
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 43
- 239000004917 carbon fiber Substances 0.000 claims description 43
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 30
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 27
- 238000001816 cooling Methods 0.000 claims description 27
- 229910002804 graphite Inorganic materials 0.000 claims description 27
- 239000010439 graphite Substances 0.000 claims description 27
- 239000000843 powder Substances 0.000 claims description 25
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 18
- 238000005245 sintering Methods 0.000 claims description 18
- 229910021645 metal ion Inorganic materials 0.000 claims description 16
- 229910052786 argon Inorganic materials 0.000 claims description 15
- 238000005520 cutting process Methods 0.000 claims description 14
- 238000000227 grinding Methods 0.000 claims description 14
- 230000004913 activation Effects 0.000 claims description 13
- 238000002791 soaking Methods 0.000 claims description 13
- 239000011863 silicon-based powder Substances 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 9
- 230000001681 protective effect Effects 0.000 claims description 9
- 239000000376 reactant Substances 0.000 claims description 9
- 238000000875 high-speed ball milling Methods 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 239000004570 mortar (masonry) Substances 0.000 claims description 7
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 6
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 6
- 238000000498 ball milling Methods 0.000 claims description 4
- KTWOOEGAPBSYNW-UHFFFAOYSA-N ferrocene Chemical compound [Fe+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 KTWOOEGAPBSYNW-UHFFFAOYSA-N 0.000 claims description 4
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 4
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 4
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 4
- 230000002776 aggregation Effects 0.000 abstract description 12
- 239000002121 nanofiber Substances 0.000 abstract description 12
- 238000005054 agglomeration Methods 0.000 abstract description 11
- 238000002156 mixing Methods 0.000 abstract description 7
- 229920001410 Microfiber Polymers 0.000 abstract description 5
- 239000003658 microfiber Substances 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 3
- 229910010271 silicon carbide Inorganic materials 0.000 description 100
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 98
- 230000007246 mechanism Effects 0.000 description 19
- 239000000463 material Substances 0.000 description 14
- 239000002105 nanoparticle Substances 0.000 description 11
- 230000009286 beneficial effect Effects 0.000 description 7
- 230000008569 process Effects 0.000 description 6
- 238000001878 scanning electron micrograph Methods 0.000 description 6
- 229910010293 ceramic material Inorganic materials 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000010923 batch production Methods 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 239000004567 concrete Substances 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 238000010574 gas phase reaction Methods 0.000 description 3
- 239000013067 intermediate product Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000012876 topography Methods 0.000 description 3
- 238000009827 uniform distribution Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 239000003733 fiber-reinforced composite Substances 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
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Abstract
A preparation method of micro-nano mixed SiC chopped fibers relates to a preparation method of SiC chopped fibers. The invention aims to solve the problems of poor mixing effect and serious agglomeration of the nano fibers in the existing mixing of the micro fibers and the nano fibers. The preparation method comprises the following steps: firstly, pretreatment; secondly, preparing a SiC fibrofelt; and thirdly, preparing micro-nano mixed SiC chopped fibers. The method is used for preparing the micro-nano mixed SiC chopped fibers.
Description
Technical Field
The invention relates to a preparation method of SiC chopped fibers.
Background
The ceramic material has excellent performances of high temperature resistance, high strength, high modulus, wear resistance, oxidation resistance and the like, so that the ceramic material can be applied to thermal structure materials. However, the ceramic material has a disadvantage of poor toughness due to directional covalent bonding between the ceramics, which greatly hinders the application of the ceramic material in the high-performance and high-reliability fields. The fiber toughening has an outstanding bridging and pulling-out action mechanism because the length of the fiber toughening is far greater than the diameter of the fiber, and the fiber toughening is an effective way for improving the brittleness and the reliability of the ceramic. Compared with other fiber materials, the silicon carbide (SiC) fiber has excellent high temperature resistance and oxidation resistance, and is a good candidate material for ceramic toughening materials.
The micron SiC fiber can improve the strength of the ceramic material at the expense of plasticity and does not remarkably improve the high-temperature performance, while a small amount of the nano SiC fiber can remarkably improve the strength of a matrix, simultaneously keep the plasticity not to be reduced and obviously improve the high-temperature performance. However, because the specific surface energy of the nano SiC fibers is large and the nano SiC fibers are easy to agglomerate, the nano SiC fiber reinforced composite material with higher volume fraction is difficult to prepare, so that the use of the nano SiC fiber reinforced material is limited. The advantages of respective size reinforcements can be fully exerted by adopting a micron and nanometer mixing mode, but at present, in order to realize micron and nanometer mixing, only the micron fibers and the nanometer fibers can be simply and mechanically mixed, the mixing effect is not good, and the aggregation of the nanometer fibers is very serious.
Disclosure of Invention
The invention provides a preparation method of micro-nano mixed SiC chopped fibers, aiming at solving the problems of poor mixing effect and serious nano fiber agglomeration of the existing mixing of micro fibers and nano fibers.
A preparation method of micro-nano mixed SiC chopped fibers is completed according to the following steps:
firstly, pretreatment:
soaking the carbon fiber felt in a hydrogen peroxide solution or a metal ion solution, and performing pre-activation treatment for 10-60 min to obtain an activated carbon fiber felt;
the mass percentage of the hydrogen peroxide solution is 10-70%; the concentration of the metal ion solution is 0.1-1 mol/L;
secondly, preparing the SiC fibrofelt:
laying reaction silicon source powder at the bottom of a graphite crucible to obtain a reaction silicon source layer, covering the activated carbon fiber felt on the surface of the reaction silicon source layer, covering a graphite crucible cover, putting the graphite crucible containing reactants into a sintering furnace, introducing argon as protective gas at the flow rate of 10-100 mL/min, heating to 1200-2000 ℃ at the heating rate of 2.5-10 ℃/min, carrying out sintering reaction for 30-180 min at the reaction temperature of 1200-2000 ℃, cooling to 300-700 ℃ at the cooling rate of 1-10 ℃/min, and naturally cooling to room temperature to obtain the SiC fiber felt;
the mass ratio of the reaction silicon source powder to the activated carbon fiber felt is 1 (1-10);
thirdly, preparing micro-nano mixed SiC chopped fibers:
and carrying out short cutting treatment on the SiC fiber mat to obtain the micro-nano mixed SiC short cut fiber.
A preparation method of micro-nano mixed SiC chopped fibers is completed according to the following steps:
firstly, pretreatment:
soaking the carbon fiber felt in a hydrogen peroxide solution for 10-60 min before activation treatment, and then soaking the carbon fiber felt in a metal ion solution for 10-60 min before activation treatment to obtain the activated carbon fiber felt;
the mass percentage of the hydrogen peroxide solution is 10-70%; the concentration of the metal ion solution is 0.1-1 mol/L;
secondly, preparing the SiC fibrofelt:
laying reaction silicon source powder at the bottom of a graphite crucible to obtain a reaction silicon source layer, covering the activated carbon fiber felt on the surface of the reaction silicon source layer, covering a graphite crucible cover, putting the graphite crucible containing reactants into a sintering furnace, introducing argon as protective gas at the flow rate of 10-100 mL/min, heating to 1200-2000 ℃ at the heating rate of 2.5-10 ℃/min, carrying out sintering reaction for 30-180 min at the reaction temperature of 1200-2000 ℃, cooling to 300-700 ℃ at the cooling rate of 1-10 ℃/min, and naturally cooling to room temperature to obtain the SiC fiber felt;
the mass ratio of the reaction silicon source powder to the activated carbon fiber felt is 1 (1-10);
thirdly, preparing micro-nano mixed SiC chopped fibers:
and carrying out short cutting treatment on the SiC fiber mat to obtain the micro-nano mixed SiC short cut fiber.
The invention has the beneficial effects that:
the invention relates to a preparation method of micro-nano mixed SiC chopped fibers, which has simple process, low cost and easy batch production, wherein the one-step method is adopted to simultaneously prepare the SiC fibers with micron and nano sizes which are uniformly mixed and do not generate agglomeration phenomenon, and the advantages of the two sizes are effectively combined to cause excellent performance leap. The carbon fiber felt is used as a template, and in the process of carrying out carbothermic reduction reaction with silicon powder, the diameter of the obtained micron fiber is 8-12 microns, and the reaction mechanism is that the carbon fiber directly reacts with a gaseous intermediate silicon source to obtain the micron fiber; the obtained nano fiber is 50-100 nm, and the reaction mechanism is that intermediate products of CO and SiO participate in gas phase reaction. The micro-nano mixed SiC chopped fiber is formed by a generation mechanism with coexistence of a gas-solid reaction mechanism and a gaseous reaction mechanism. And in the reaction process, the two reaction mechanisms are simultaneously carried out, so that the product has the characteristic of uniform distribution under microscopic-angle morphology observation and is not easy to generate agglomeration. The micro-nano mixed chopped fiber can meet the application environment with diversified size requirements on SiC, and the micron and nano mixed chopped fiber has application prospects in the fields of filtration, high-temperature protection materials, heat-proof materials, wave absorption and the like which are beneficial to enrichment of SiC materials.
The invention relates to a preparation method of micro-nano mixed SiC chopped fibers.
Drawings
FIG. 1 is a microscopic morphology diagram of nano-sized SiC chopped fibers in the micro-nano mixed SiC chopped fibers prepared in the first embodiment;
FIG. 2 is a micro-topography of micro-nano mixed SiC chopped fibers prepared in the first embodiment;
FIG. 3 is a microscopic morphology of nano-sized SiC chopped fibers in the micro-nano hybrid SiC chopped fibers prepared in example two;
FIG. 4 is a micro-topography of micro-nano hybrid SiC chopped fibers prepared in example two;
FIG. 5 is a microscopic morphology view of nano-sized SiC chopped fibers in the micro-nano mixed SiC chopped fibers prepared in example III;
FIG. 6 is a micro-topography of micro-nano mixed SiC chopped fibers prepared in example III;
fig. 7 is an XRD spectrum, wherein 1 is the micro-nano mixed SiC chopped fiber prepared in the first example, 2 is the micro-nano mixed SiC chopped fiber prepared in the second example, and 3 is the micro-nano mixed SiC chopped fiber prepared in the third example.
Detailed Description
The first embodiment is as follows: the embodiment of the invention relates to a preparation method of micro-nano mixed SiC chopped fibers, which is completed according to the following steps:
firstly, pretreatment:
soaking the carbon fiber felt in a hydrogen peroxide solution or a metal ion solution, and performing pre-activation treatment for 10-60 min to obtain an activated carbon fiber felt;
the mass percentage of the hydrogen peroxide solution is 10-70%; the concentration of the metal ion solution is 0.1-1 mol/L;
secondly, preparing the SiC fibrofelt:
laying reaction silicon source powder at the bottom of a graphite crucible to obtain a reaction silicon source layer, covering the activated carbon fiber felt on the surface of the reaction silicon source layer, covering a graphite crucible cover, putting the graphite crucible containing reactants into a sintering furnace, introducing argon as protective gas at the flow rate of 10-100 mL/min, heating to 1200-2000 ℃ at the heating rate of 2.5-10 ℃/min, carrying out sintering reaction for 30-180 min at the reaction temperature of 1200-2000 ℃, cooling to 300-700 ℃ at the cooling rate of 1-10 ℃/min, and naturally cooling to room temperature to obtain the SiC fiber felt;
the mass ratio of the reaction silicon source powder to the activated carbon fiber felt is 1 (1-10);
thirdly, preparing micro-nano mixed SiC chopped fibers:
and carrying out short cutting treatment on the SiC fiber mat to obtain the micro-nano mixed SiC short cut fiber.
The beneficial effects of the embodiment are as follows:
the embodiment is a preparation method of micro-nano mixed SiC chopped fibers, which is simple in process, low in cost and easy for batch production, and the SiC fibers with two sizes of micron and nano which are uniformly mixed and do not generate agglomeration are simultaneously prepared by adopting a one-step method, so that the advantages of the two sizes are effectively combined to cause excellent performance leap. The carbon fiber felt is used as a template, and in the process of carrying out carbothermic reduction reaction with silicon powder, the diameter of the obtained micron fiber is 8-12 microns, and the reaction mechanism is that the carbon fiber directly reacts with a gaseous intermediate silicon source to obtain the micron fiber; the obtained nano fiber is 50-100 nm, and the reaction mechanism is that intermediate products of CO and SiO participate in gas phase reaction. The micro-nano mixed SiC chopped fiber is formed by a generation mechanism with coexistence of a gas-solid reaction mechanism and a gaseous reaction mechanism. And in the reaction process, the two reaction mechanisms are simultaneously carried out, so that the product has the characteristic of uniform distribution under microscopic-angle morphology observation and is not easy to generate agglomeration. The micro-nano mixed chopped fiber can meet the application environment with diversified size requirements on SiC, and the micron and nano mixed chopped fiber has application prospects in the fields of filtration, high-temperature protection materials, heat-proof materials, wave absorption and the like which are beneficial to enrichment of SiC materials.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the carbon fiber felt in the step one is 100g/m of unit mass2～800g/m2The carbon fiber felt of (1); the thickness of the carbon fiber felt in the step one is 3 mm-10 mm. The rest is the same as the first embodiment.
The third concrete implementation mode: this embodiment is different from the first or second embodiment in that: the metal ion solution in the first step is ferric sulfate solution, ferrocene solution, nickel nitrate solution or nickel sulfate solution. The other is the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: the reaction silicon source powder in the second step is a mixture of silicon dioxide powder and silicon powder in a molar ratio of 1 (1-6). The others are the same as the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: the short cutting treatment in the third step is grinding, high-speed ball milling or high-speed mixer treatment; the grinding is carried out in a mortar at a constant speed for 1-5 h; the high-speed ball milling is carried out for 30-240 min under the condition that the ball milling speed is 150-300 r/min; the high-speed mixer is used for processing for 1-5 h under the conditions that the power is 1-50 Hz and the rotating speed is 60-120 r/min. The rest is the same as the first to fourth embodiments.
The sixth specific implementation mode: the embodiment of the invention relates to a preparation method of micro-nano mixed SiC chopped fibers, which is completed according to the following steps:
firstly, pretreatment:
soaking the carbon fiber felt in a hydrogen peroxide solution for 10-60 min before activation treatment, and then soaking the carbon fiber felt in a metal ion solution for 10-60 min before activation treatment to obtain the activated carbon fiber felt;
the mass percentage of the hydrogen peroxide solution is 10-70%; the concentration of the metal ion solution is 0.1-1 mol/L;
secondly, preparing the SiC fibrofelt:
laying reaction silicon source powder at the bottom of a graphite crucible to obtain a reaction silicon source layer, covering the activated carbon fiber felt on the surface of the reaction silicon source layer, covering a graphite crucible cover, putting the graphite crucible containing reactants into a sintering furnace, introducing argon as protective gas at the flow rate of 10-100 mL/min, heating to 1200-2000 ℃ at the heating rate of 2.5-10 ℃/min, carrying out sintering reaction for 30-180 min at the reaction temperature of 1200-2000 ℃, cooling to 300-700 ℃ at the cooling rate of 1-10 ℃/min, and naturally cooling to room temperature to obtain the SiC fiber felt;
the mass ratio of the reaction silicon source powder to the activated carbon fiber felt is 1 (1-10);
thirdly, preparing micro-nano mixed SiC chopped fibers:
and carrying out short cutting treatment on the SiC fiber mat to obtain the micro-nano mixed SiC short cut fiber.
The beneficial effects of the embodiment are as follows:
the embodiment is a preparation method of micro-nano mixed SiC chopped fibers, which is simple in process, low in cost and easy for batch production, and the SiC fibers with two sizes of micron and nano which are uniformly mixed and do not generate agglomeration are simultaneously prepared by adopting a one-step method, so that the advantages of the two sizes are effectively combined to cause excellent performance leap. The carbon fiber felt is used as a template, and in the process of carrying out carbothermic reduction reaction with silicon powder, the diameter of the obtained micron fiber is 8-12 microns, and the reaction mechanism is that the carbon fiber directly reacts with a gaseous intermediate silicon source to obtain the micron fiber; the obtained nano fiber is 50-100 nm, and the reaction mechanism is that intermediate products of CO and SiO participate in gas phase reaction. The micro-nano mixed SiC chopped fiber is formed by a generation mechanism with coexistence of a gas-solid reaction mechanism and a gaseous reaction mechanism. And in the reaction process, the two reaction mechanisms are simultaneously carried out, so that the product has the characteristic of uniform distribution under microscopic-angle morphology observation and is not easy to generate agglomeration. The micro-nano mixed chopped fiber can meet the application environment with diversified size requirements on SiC, and the micron and nano mixed chopped fiber has application prospects in the fields of filtration, high-temperature protection materials, heat-proof materials, wave absorption and the like which are beneficial to enrichment of SiC materials.
The seventh embodiment: the sixth embodiment is different from the sixth embodiment in that: the carbon fiber felt in the step one is 100g/m of unit mass2～800g/m2The carbon fiber felt of (1); the thickness of the carbon fiber felt in the step one is 3 mm-10 mm. The rest is the same as the sixth embodiment.
The specific implementation mode is eight: the present embodiment differs from one of the sixth or seventh embodiments in that: the metal ion solution in the first step is ferric sulfate solution, ferrocene solution, nickel nitrate solution or nickel sulfate solution. The others are the same as the sixth or seventh embodiments.
The specific implementation method nine: this embodiment differs from one of the sixth to eighth embodiments in that: the reaction silicon source powder in the second step is a mixture of silicon dioxide powder and silicon powder in a molar ratio of 1 (1-6). The others are the same as the embodiments six to eight.
The detailed implementation mode is ten: the present embodiment differs from one of the sixth to ninth embodiments in that: the short cutting treatment in the third step is grinding, high-speed ball milling or high-speed mixer treatment; the grinding is carried out in a mortar at a constant speed for 1-5 h; the high-speed ball milling is carried out for 30-240 min under the condition that the ball milling speed is 150-300 r/min; the high-speed mixer is used for processing for 1-5 h under the conditions that the power is 1-50 Hz and the rotating speed is 60-120 r/min. The others are the same as in the sixth to ninth embodiments.
The following examples were used to demonstrate the beneficial effects of the present invention:
the first embodiment is as follows:
a preparation method of micro-nano mixed SiC chopped fibers is completed according to the following steps:
firstly, pretreatment:
soaking the carbon fiber felt in a hydrogen peroxide solution for 30min before activation treatment, then soaking the carbon fiber felt in a ferric sulfate solution for 30min before activation treatment to obtain an activated carbon fiber felt;
the mass percent of the hydrogen peroxide solution is 30 percent; the concentration of the ferric sulfate solution is 0.1 mol/L;
secondly, preparing the SiC fibrofelt:
laying reaction silicon source powder at the bottom of a graphite crucible to obtain a reaction silicon source layer, covering the activated carbon fiber felt on the surface of the reaction silicon source layer, covering a graphite crucible cover, putting the graphite crucible containing reactants into a sintering furnace, introducing argon as a protective gas at the flow rate of 20mL/min, heating the temperature to 1300 ℃ at the heating rate of 2.5 ℃/min, carrying out sintering reaction for 120min at the reaction temperature of 1300 ℃, cooling to 700 ℃ at the cooling rate of 5 ℃/min, and naturally cooling to room temperature to obtain the SiC fiber felt;
the mass ratio of the reaction silicon source powder to the activated carbon fiber felt is 1: 2;
thirdly, preparing micro-nano mixed SiC chopped fibers:
and carrying out short cutting treatment on the SiC fiber mat to obtain the micro-nano mixed SiC short cut fiber.
The unit mass of the carbon fiber felt in the step one is 700g/m2The carbon fiber felt of (1); the thickness of the carbon fiber felt is 5 mm.
The reaction silicon source powder in the second step is a mixture of silicon dioxide powder and silicon powder mixed according to a molar ratio of 1: 1.
The short cutting treatment in the third step is grinding; the grinding is carried out in a mortar at a constant speed for 1 hour.
And the argon in the step two is high-purity argon with the purity of more than or equal to 99.99 percent.
FIG. 1 is a microscopic morphology diagram of nano-sized SiC chopped fibers in the micro-nano mixed SiC chopped fibers prepared in the first embodiment; the presence of nano-sized fibers can be clearly seen in the SEM image at a larger magnification; fig. 2 is a microscopic morphology of the micro-nano mixed SiC chopped fiber prepared in the first embodiment, SiC fibers of two sizes of micron and nano can be simultaneously observed from an SEM image with a small magnification, and the micron and nano fibers are uniformly mixed without agglomeration. As can be seen from the figure, the diameter of the obtained micro-fiber is 8-12 μm, and the obtained nano-fiber is 50-100 nm.
Example two:
a preparation method of micro-nano mixed SiC chopped fibers is completed according to the following steps:
firstly, pretreatment:
soaking the carbon fiber felt in a hydrogen peroxide solution, and performing pre-activation treatment for 30min to obtain activated carbon fiber felt;
the mass percent of the hydrogen peroxide solution is 30 percent;
secondly, preparing the SiC fibrofelt:
laying reaction silicon source powder at the bottom of a graphite crucible to obtain a reaction silicon source layer, covering the activated carbon fiber felt on the surface of the reaction silicon source layer, covering a graphite crucible cover, putting the graphite crucible containing reactants into a sintering furnace, introducing argon as a protective gas at the flow rate of 20mL/min, heating the temperature to 1400 ℃ at the heating rate of 2.5 ℃/min, carrying out sintering reaction for 120min at the reaction temperature of 1400 ℃, cooling to 700 ℃ at the cooling rate of 10 ℃/min, and naturally cooling to room temperature to obtain the SiC fiber felt;
the mass ratio of the reaction silicon source powder to the activated carbon fiber felt is 1: 2;
thirdly, preparing micro-nano mixed SiC chopped fibers:
and carrying out short cutting treatment on the SiC fiber mat to obtain the micro-nano mixed SiC short cut fiber.
The unit mass of the carbon fiber felt in the step one is 700g/m2The carbon fiber felt of (1); the thickness of the carbon fiber felt is 5 mm.
The reaction silicon source powder in the second step is a mixture of silicon dioxide powder and silicon powder mixed according to a molar ratio of 1: 1.
The short cutting treatment in the third step is grinding; the grinding is carried out in a mortar at a constant speed for 1 hour.
And the argon in the step two is high-purity argon with the purity of more than or equal to 99.99 percent.
Fig. 3 is a microscopic morphology of nano-sized SiC chopped fibers in the micro-nano hybrid SiC chopped fibers prepared in the first example, and the existence of nano-sized fibers can be clearly seen in an SEM image with a large magnification; fig. 4 is a microscopic morphology of the micro-nano mixed SiC chopped fiber prepared in the first embodiment, SiC fibers of two sizes of micron and nano can be simultaneously observed from an SEM image with a small magnification, and the micron and nano fibers are uniformly mixed without agglomeration. As can be seen from the figure, the diameter of the obtained micro-fiber is 8-12 μm, and the obtained nano-fiber is 50-100 nm.
Example three:
a preparation method of micro-nano mixed SiC chopped fibers is completed according to the following steps:
firstly, pretreatment:
soaking the carbon fiber felt in a hydrogen peroxide solution, and performing pre-activation treatment for 30min to obtain activated carbon fiber felt;
the mass percent of the hydrogen peroxide solution is 30 percent;
secondly, preparing the SiC fibrofelt:
laying reaction silicon source powder at the bottom of a graphite crucible to obtain a reaction silicon source layer, covering the activated carbon fiber felt on the surface of the reaction silicon source layer, covering a graphite crucible cover, putting the graphite crucible containing reactants into a sintering furnace, introducing argon as a protective gas at the flow rate of 20mL/min, heating the temperature to 1500 ℃ at the heating rate of 2.5 ℃/min, carrying out sintering reaction for 120min under the condition that the reaction temperature is 1500 ℃, cooling to 700 ℃ at the cooling rate of 2.5 ℃/min, and naturally cooling to room temperature to obtain the SiC fiber felt;
the mass ratio of the reaction silicon source powder to the activated carbon fiber felt is 1: 2;
thirdly, preparing micro-nano mixed SiC chopped fibers:
and carrying out short cutting treatment on the SiC fiber mat to obtain the micro-nano mixed SiC short cut fiber.
The unit mass of the carbon fiber felt in the step one is 700g/m2The carbon fiber felt of (1); the above-mentionedThe thickness of the carbon fiber felt of (2) was 5 mm.
The reaction silicon source powder in the second step is a mixture of silicon dioxide powder and silicon powder mixed according to a molar ratio of 1: 1.
The short cutting treatment in the third step is grinding; the grinding is carried out in a mortar at a constant speed for 1 hour.
And the argon in the step two is high-purity argon with the purity of more than or equal to 99.99 percent.
Fig. 5 is a microscopic morphology of nano-sized SiC chopped fibers in the micro-nano hybrid SiC chopped fibers prepared in example three, and the existence of nano-sized fibers can be clearly seen in an SEM image with a large magnification; fig. 6 is a microscopic morphology of the micro-nano mixed SiC chopped fiber prepared in the first embodiment, SiC fibers of two sizes of micron and nano can be simultaneously observed in an SEM image with a small magnification, and the micron and nano sized fibers are uniformly mixed without agglomeration. As can be seen from the figure, the diameter of the obtained micro-fiber is 8-12 μm, and the obtained nano-fiber is 50-100 nm.
Fig. 7 is an XRD spectrum, wherein 1 is the micro-nano mixed SiC chopped fiber prepared in the first example, 2 is the micro-nano mixed SiC chopped fiber prepared in the second example, and 3 is the micro-nano mixed SiC chopped fiber prepared in the third example; the characteristic peaks of the sample prepared in the first embodiment except the characteristic peak of the residual part C correspond to the characteristic peak of 3C-SiC, which shows that the reaction of the carbon fiber felt at the first embodiment is incomplete, but the generated micron-sized and nano-sized SiC has better appearance. The characteristic peaks of the samples prepared in the second example all correspond to the characteristic peaks of 3C-SiC, which shows that the reaction of the carbon fiber felt at the second temperature of the second example is complete, and SiC is completely generated. The characteristic peaks of the samples prepared in the third example all correspond to the characteristic peaks of 3C-SiC, which shows that the reaction of the carbon fiber felt at the third temperature of the example is complete and SiC is completely generated.
Claims (6)
1. A preparation method of micro-nano mixed SiC chopped fibers is characterized by comprising the following steps:
firstly, pretreatment:
soaking the carbon fiber felt in a hydrogen peroxide solution or a metal ion solution, and performing pre-activation treatment for 10-60 min to obtain an activated carbon fiber felt;
the mass percentage of the hydrogen peroxide solution is 10-70%; the concentration of the metal ion solution is 0.1-1 mol/L;
the carbon fiber felt has a unit mass of 100g/m2～800g/m2The carbon fiber felt of (1); the thickness of the carbon fiber felt is 3 mm-10 mm;
secondly, preparing the SiC fibrofelt:
laying reaction silicon source powder at the bottom of a graphite crucible to obtain a reaction silicon source layer, covering the activated carbon fiber felt on the surface of the reaction silicon source layer, covering a graphite crucible cover, putting the graphite crucible containing reactants into a sintering furnace, introducing argon as protective gas at the flow rate of 10-100 mL/min, heating to 1200-2000 ℃ at the heating rate of 2.5-10 ℃/min, carrying out sintering reaction for 30-180 min at the reaction temperature of 1200-2000 ℃, cooling to 300-700 ℃ at the cooling rate of 1-10 ℃/min, and naturally cooling to room temperature to obtain the SiC fiber felt;
the mass ratio of the reaction silicon source powder to the activated carbon fiber felt is 1 (1-10);
thirdly, preparing micro-nano mixed SiC chopped fibers:
carrying out short-cut treatment on the SiC fiber mat to obtain micro-nano mixed SiC short-cut fibers;
the short cutting treatment is grinding, high-speed ball milling or high-speed mixer treatment; the grinding is carried out in a mortar at a constant speed for 1-5 h; the high-speed ball milling is carried out for 30-240 min under the condition that the ball milling speed is 150-300 r/min; the high-speed mixer is used for processing for 1-5 h under the conditions that the power is 1-50 Hz and the rotating speed is 60-120 r/min.
2. The method for preparing micro-nano mixed SiC chopped fibers according to claim 1, wherein the metal ion solution in the first step is a ferric sulfate solution, a ferrocene solution, a nickel nitrate solution or a nickel sulfate solution.
3. The preparation method of the micro-nano mixed SiC chopped fiber according to claim 1, wherein the reaction silicon source powder in the second step is a mixture of silicon dioxide powder and silicon powder in a molar ratio of 1 (1-6).
4. A preparation method of micro-nano mixed SiC chopped fibers is characterized by comprising the following steps:
firstly, pretreatment:
soaking the carbon fiber felt in a hydrogen peroxide solution for 10-60 min before activation treatment, and then soaking the carbon fiber felt in a metal ion solution for 10-60 min before activation treatment to obtain the activated carbon fiber felt;
the mass percentage of the hydrogen peroxide solution is 10-70%; the concentration of the metal ion solution is 0.1-1 mol/L;
the carbon fiber felt has a unit mass of 100g/m2～800g/m2The carbon fiber felt of (1); the thickness of the carbon fiber felt is 3 mm-10 mm;
secondly, preparing the SiC fibrofelt:
laying reaction silicon source powder at the bottom of a graphite crucible to obtain a reaction silicon source layer, covering the activated carbon fiber felt on the surface of the reaction silicon source layer, covering a graphite crucible cover, putting the graphite crucible containing reactants into a sintering furnace, introducing argon as protective gas at the flow rate of 10-100 mL/min, heating to 1200-2000 ℃ at the heating rate of 2.5-10 ℃/min, carrying out sintering reaction for 30-180 min at the reaction temperature of 1200-2000 ℃, cooling to 300-700 ℃ at the cooling rate of 1-10 ℃/min, and naturally cooling to room temperature to obtain the SiC fiber felt;
the mass ratio of the reaction silicon source powder to the activated carbon fiber felt is 1 (1-10);
thirdly, preparing micro-nano mixed SiC chopped fibers:
carrying out short-cut treatment on the SiC fiber mat to obtain micro-nano mixed SiC short-cut fibers;
the short cutting treatment is grinding, high-speed ball milling or high-speed mixer treatment; the grinding is carried out in a mortar at a constant speed for 1-5 h; the high-speed ball milling is carried out for 30-240 min under the condition that the ball milling speed is 150-300 r/min; the high-speed mixer is used for processing for 1-5 h under the conditions that the power is 1-50 Hz and the rotating speed is 60-120 r/min.
5. The method for preparing micro-nano mixed SiC chopped fibers according to claim 4, wherein the metal ion solution in the first step is a ferric sulfate solution, a ferrocene solution, a nickel nitrate solution or a nickel sulfate solution.
6. The preparation method of the micro-nano mixed SiC chopped fiber according to claim 4, wherein the reaction silicon source powder in the second step is a mixture of silicon dioxide powder and silicon powder in a molar ratio of 1 (1-6).
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