CN109608824B - Preparation method of nano silicon nitride fiber/epoxy resin composite material - Google Patents
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/06—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials
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- 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
- C08K7/26—Silicon- containing compounds
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
Abstract
The invention discloses a preparation method of a nano silicon nitride fiber/epoxy resin composite material, which is prepared by impregnating a mixed material of epoxy resin, an epoxy resin curing agent and an accelerant into a porous nano silicon nitride fiber frame and curing at a high temperature, wherein the volume fraction of nano silicon nitride fibers in the nano silicon nitride fiber/epoxy resin composite material is 20-60 vol%. The nano silicon nitride fiber in the epoxy resin composite material prepared by the invention is a continuous phase, so that the high-low temperature mechanical property, the thermal conductivity, the high-temperature creep resistance and the fracture toughness of the composite material can be greatly improved. In addition, the preparation process is simple and easy to operate, and the content of the nano silicon nitride fibers in the composite material can be changed by regulating and controlling the porosity of the porous nano silicon nitride material.
Description
Technical Field
The invention belongs to the field of polymer composite materials, and particularly relates to a preparation method of a nano silicon nitride fiber/epoxy resin composite material.
Background
The polymer-based nano composite material draws great attention in academia and industry, and a plurality of physical properties and mechanical properties of the polymer-based nano composite material can be improved only by a small amount of nano inorganic filler. The high-thermal-conductivity nano epoxy resin composite material is a multiphase system composite material which takes a polymer as a matrix, takes a nano inorganic material as a filler and is accompanied with fiber reinforcement. The composite material is widely applied to chemical heat exchange and corrosion-resistant occasions, and the composite material is required to have high heat conduction, can resist certain temperature and pressure, and has good mechanical property and corrosion resistance.
Compared with granular inorganic particles, the fiber or whisker inorganic particles can obviously improve the thermal conductivity and fracture toughness of the composite material. Nano Si3N4The fiber has high thermal conductivity, good high-low temperature mechanical property, excellent stability and corrosion resistance, and can effectively improve the thermal conductivity and mechanical property of the epoxy composite material when being used as a reinforcing phase. However, when the nano silicon nitride/epoxy composite material is prepared by the traditional direct mixing-vacuum casting method, an effective heat conducting network can be formed only when the filler content reaches a certain threshold value, which also causes the increase of the interface thermal resistance of the composite material and the great reduction of the mechanical property and the processing property. On the other hand, for nano-scale fiber or whisker materials, the fiber content is difficult to uniformly disperse when exceeding a certain amount, and defects are easy to exist; the epoxy composite material prepared by the traditional direct mixing method has low mass fraction (generally lower than 3 wt.%) of the nanofiber filler, and the application of the nanofiber composite material is limited to a great extent.
Heretofore, the preparation methods of epoxy resin-based nanocomposites mainly include direct mixing, intercalation compounding, sol-gel and in-situ polymerization. A method for simply, rapidly and effectively preparing the uniformly dispersed nano epoxy resin composite material with high fiber content is still lacked, and the fibers are difficult to form an effective heat conducting network in an epoxy resin matrix.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of a nano silicon nitride fiber/epoxy resin composite material.
The invention is realized by adopting the following technical scheme:
a preparation method of a nano silicon nitride fiber/epoxy resin composite material is characterized in that the nano silicon nitride fiber/epoxy resin composite material is prepared by impregnating a mixed material of epoxy resin, an epoxy resin curing agent and an accelerator into a porous nano silicon nitride fiber frame and carrying out high-temperature curing, wherein the volume fraction of mullite fiber in the mullite fiber/epoxy resin composite material is 20-50 vol%, and the preparation method specifically comprises the following steps:
1) preparing a porous nano silicon nitride fiber framework: according to the mass percentage, 20-90 wt% of carbon nano tube and 0-70 wt% of alpha-Si3N4And forming a green body by compression molding with 10-20 wt% of rare earth oxide mixed powder, placing SiO powder at the bottom of a crucible, placing the green body on a porous BN support in the middle of the crucible, placing the crucible in a multifunctional sintering furnace, introducing nitrogen, keeping the temperature at 1500-1700 ℃ for 1-6 hours, and performing carbothermic reduction nitridation reaction to generate a porous silicon nitride green body, wherein the mass ratio of SiO to carbon nano tubes is (8-12): 1; continuously heating to 1750-1850 ℃ for liquid phase sintering for 0.5-2 hours, wherein phase transformation occurs in the process, and thus a porous nano silicon nitride fiber framework is obtained;
2) preparing a nano silicon nitride fiber/epoxy resin composite material: grinding and flattening the surface of the porous nano silicon nitride fiber frame obtained in the step 1), then placing the porous nano silicon nitride fiber frame into absolute ethyl alcohol containing 2-5 wt% of silane coupling agent for surface modification, keeping the temperature at 60-80 ℃ for 2-5 h, taking out and drying for 24 h; stirring the mixed solution of the epoxy resin, the curing agent and the accelerator at a high speed for 2-4 h, uniformly mixing, and defoaming in vacuum for 2-4 h; placing the preheated porous nano silicon nitride fiber framework in a mixed solution of epoxy resin, an accelerant and a curing agent for soaking for 1-3 hours; curing under a set curing system to obtain the nano silicon nitride fiber/epoxy resin composite material.
The invention has the further improvement that in the step 1), the average grain diameter of the selected silicon nitride is 0.2-0.5 mu m, and the forming pressure is 20-80 MPa.
The invention is further improved in that in the step 1), the selected rare earth oxide is Y2O3，Lu2O3，Yb2O3，La2O3Or Eu2O3。
The further improvement of the invention is that the pressure for compression molding in the step 1) is 10-80 MPa, and the pressure maintaining time is 1 min.
The invention is further improved in that the pressure of the nitrogen atmosphere in the step 1) is 2.5-7 atm.
The invention is further improved in that the temperature rising speed of the multifunctional sintering furnace in the step 1) from room temperature to 1100 ℃ is 500-700 ℃/h, and the temperature rising speed of the multifunctional sintering furnace from 1100 ℃ to the sintering temperature is 100-300 ℃/h.
The method is further improved in that the temperature rising speed of the carbothermic nitriding temperature in the step 1) to the liquid phase sintering temperature is 50-100 ℃/h.
The invention is further improved in that the epoxy resin in the step 2) is selected from any one of bisphenol A type epoxy resin, bisphenol F type epoxy resin or bisphenol S type epoxy resin.
The further improvement of the invention is that in the step 2), the epoxy resin curing agent is methyl tetrahydrophthalic anhydride, and the accelerator is trisphenol.
The invention is further improved in that the curing temperature system in the step 2) is as follows: and preserving the heat for 24-48 h at 130 ℃.
The invention has the following beneficial technical effects:
the invention abandons the traditional direct mixing method to prepare the epoxy resin composite material. According to the method, epoxy resin is filled in the porous nano silicon nitride fiber material through a vacuum impregnation method, so that the nano silicon nitride fiber/epoxy resin composite material is prepared. Firstly, gas-solid reaction of carbon nano tube and SiO is combined with high-temperature liquid phase sintering to prepare porous nano silicon nitride material, and the silicon nitride has nano fibrous shape. By regulating alpha-Si in the starting material3N4The content and the forming pressure can control the porosity (50-80%) of the porous ceramic; and then the epoxy resin is filled into the pores of the porous mullite material by a vacuum impregnation method to obtain the compact bicontinuous phase nano silicon nitride fiber/epoxy resin composite material, wherein the compactness reaches more than 99 percent. The nano silicon nitride fiber in the epoxy resin composite material with the structure is a continuous phase and can be largeThe high and low temperature mechanical property, the thermal conductivity, the high temperature creep resistance and the fracture toughness of the composite material are greatly improved. In addition, the preparation process is simple and easy to operate, and the content of the nano silicon nitride fibers in the composite material can be changed by regulating and controlling the porosity of the porous mullite material.
Drawings
Fig. 1 is an SEM image of the nano silicon nitride fiber/epoxy resin composite material obtained in example 5.
Detailed Description
The invention will now be further described with reference to examples and figures, but the practice of the invention is not limited thereto.
Example one
1) Preparing a porous nano silicon nitride fiber framework: according to the mass percentage, 20 wt% of carbon nano tube and 70 wt% of alpha-Si with the diameter of 0.2 mu m3N4And 10 wt% of Y2O3The mixed powder is molded to form a green body, and the molding pressure is 20 MPa; placing SiO powder at the bottom of a crucible, wherein the mass ratio of SiO to carbon nano tubes is 10:1, placing a green body on a porous BN support in the middle of the crucible, placing the crucible in a multifunctional sintering furnace, introducing nitrogen, keeping the temperature at 1500 ℃ for 6 hours, heating the temperature to 1100 ℃ at room temperature at a heating speed of 500 ℃/h, heating the temperature from 1100 ℃ to 1500 ℃ at a heating speed of 100 ℃/h, and carrying out carbothermic reduction nitridation reaction to generate a porous silicon nitride green body, wherein the mass ratio of SiO to carbon nano tubes is 10: 1; and continuously heating to 1750 ℃ for liquid phase sintering, keeping the temperature for 0.5 hour, wherein the heating rate is 100 ℃/h, and phase transformation occurs in the process to obtain the porous nano silicon nitride fiber framework with the porosity of 70%.
2) Preparing a nano silicon nitride fiber/epoxy resin composite material: grinding and flattening the surface of the porous nano silicon nitride fiber frame obtained in the step 1), then placing the porous nano silicon nitride fiber frame in absolute ethyl alcohol containing 2 wt% of silane coupling agent for surface modification, keeping the temperature at 60 ℃ for 5 hours, taking out and drying for 24 hours; stirring the mixed solution of bisphenol A epoxy resin, curing agent and accelerator at a high speed for 4h, uniformly mixing, and defoaming in vacuum for 2 h; placing the preheated porous nano silicon nitride fiber framework in a mixed solution of epoxy resin, an accelerant and a curing agent for soaking for 1 h; and curing the mixture in a vacuum oven at 130 ℃ for 24 hours to obtain the nano silicon nitride fiber/epoxy resin composite material with the silicon nitride volume fraction of 30 vol%.
Example two
1) Preparing a porous nano silicon nitride fiber framework: according to the mass percentage, 50 wt% of carbon nano tube and 30 wt% of alpha-Si with the diameter of 0.5 mu m3N4And 20 wt% of Yb2O3The mixed powder is molded into a green body with the molding pressure of 40 MPa; placing SiO powder at the bottom of a crucible, wherein the mass ratio of SiO to carbon nano tubes is 8:1, placing a green body on a porous BN support in the middle of the crucible, placing the crucible in a multifunctional sintering furnace, introducing nitrogen, keeping the temperature at 1600 ℃ for 3 hours, raising the temperature of a chamber to 1100 ℃ at the heating speed of 700 ℃/h and raising the temperature from 1100 ℃ to 1600 ℃ at the heating speed of 300 ℃/h, and carrying out carbothermic reduction nitridation reaction to generate a porous silicon nitride green body, wherein the mass ratio of SiO to carbon nano tubes is 10: 1; and continuously heating to 1850 ℃ for liquid phase sintering, wherein the heating rate is 100 ℃/h, keeping the temperature for 2 hours, and phase transformation occurs in the process to obtain the porous nano silicon nitride fiber framework with the porosity of 40%.
2) Preparing a nano silicon nitride fiber/epoxy resin composite material: grinding and flattening the surface of the porous nano silicon nitride fiber frame obtained in the step 1), then placing the porous nano silicon nitride fiber frame in absolute ethyl alcohol containing 5 wt% of silane coupling agent for surface modification, keeping the temperature at 80 ℃ for 2 hours, taking out and drying for 24 hours; stirring the mixed solution of bisphenol A epoxy resin, curing agent and accelerator at a high speed for 2h, uniformly mixing, and defoaming in vacuum for 4 h; placing the preheated porous nano silicon nitride fiber framework in a mixed solution of epoxy resin, an accelerant and a curing agent for soaking for 3 hours; and curing the mixture in a vacuum oven at 130 ℃ for 36 hours to obtain the nano silicon nitride fiber/epoxy resin composite material with the silicon nitride volume fraction of 60 vol%.
EXAMPLE III
1) Preparing a porous nano silicon nitride fiber framework: according to the mass percentage, 90 wt% of carbon nano tube and 10 wt% of La are mixed2O3The mixed powder is molded into a green body with the molding pressure of 80 MPa; placing SiO powder inPlacing the green body on a porous BN support in the middle of a crucible at the bottom of the crucible, wherein the mass ratio of SiO to carbon nanotubes is 12:1, placing the crucible in a multifunctional sintering furnace, introducing nitrogen, keeping the temperature at 1700 ℃ for 1 hour, raising the temperature from the room temperature to 1100 ℃ at a heating rate of 600 ℃/h, raising the temperature from 1100 ℃ to 1700 ℃ at a heating rate of 200 ℃/h, and carrying out carbothermic reduction nitridation reaction to generate a porous silicon nitride green body, wherein the mass ratio of SiO to carbon nanotubes is 10: 1; and continuously heating to 1800 ℃ for liquid phase sintering, wherein the heating rate is 200 ℃/h, keeping the temperature for 2 hours, and phase transformation occurs in the process to obtain the porous nano silicon nitride fiber framework with the porosity of 75%.
2) Preparing a nano silicon nitride fiber/epoxy resin composite material: grinding and flattening the surface of the porous nano silicon nitride fiber frame obtained in the step 1), then placing the porous nano silicon nitride fiber frame in absolute ethyl alcohol containing 4 wt% of silane coupling agent for surface modification, keeping the temperature at 70 ℃ for 4 hours, taking out and drying for 24 hours; stirring the mixed solution of bisphenol A epoxy resin, curing agent and accelerator at a high speed for 3h, uniformly mixing, and defoaming in vacuum for 3 h; placing the preheated porous nano silicon nitride fiber framework in a mixed solution of epoxy resin, an accelerant and a curing agent for soaking for 2 hours; and curing the mixture in a vacuum oven at 130 ℃ for 48 hours to obtain the nano silicon nitride fiber/epoxy resin composite material with the silicon nitride volume fraction of 25 vol%.
Example four
1) Preparing a porous nano silicon nitride fiber framework: 60 wt% of carbon nano tube and 30 wt% of 0.4 mu m alpha-Si according to mass percentage3N4And 10 wt% of Lu2O3The mixed powder is molded to form a green body, and the molding pressure is 60 MPa; placing SiO powder at the bottom of a crucible, wherein the mass ratio of SiO to carbon nano tubes is 10:1, placing a green body on a porous BN support in the middle of the crucible, placing the crucible in a multifunctional sintering furnace, introducing nitrogen, keeping the temperature at 1650 ℃ for 2 hours, heating the temperature to 1100 ℃ at the room temperature at the heating speed of 600 ℃/h, heating the temperature from 1100 ℃ to 1650 ℃ at the heating speed of 200 ℃/h, and carrying out carbothermic reduction nitridation reaction to generate a porous silicon nitride green body, wherein the mass ratio of SiO to carbon nano tubes is 10: 1; continuously heating to 1750 ℃ for liquid phase sintering, wherein the heating rate isKeeping the temperature at 150 ℃/h for 1 hour, and carrying out phase transformation in the process to obtain the porous nano silicon nitride fiber framework with the porosity of 60 percent.
2) Preparing a nano silicon nitride fiber/epoxy resin composite material: grinding and flattening the surface of the porous nano silicon nitride fiber frame obtained in the step 1), then placing the porous nano silicon nitride fiber frame in absolute ethyl alcohol containing 3 wt% of silane coupling agent for surface modification, keeping the temperature at 80 ℃ for 5 hours, taking out and drying for 24 hours; stirring the mixed solution of bisphenol F type epoxy resin, curing agent and accelerator at a high speed for 3h, uniformly mixing, and defoaming in vacuum for 3 h; placing the preheated porous nano silicon nitride fiber framework in a mixed solution of epoxy resin, an accelerant and a curing agent for soaking for 2 hours; and curing the mixture in a vacuum oven at 130 ℃ for 24 hours to obtain the nano silicon nitride fiber/epoxy resin composite material with the silicon nitride volume fraction of 40 vol%.
EXAMPLE five
1) Preparing a porous nano silicon nitride fiber framework: 55 wt% of carbon nano tube and 30 wt% of 0.2 mu m alpha-Si according to mass percentage3N4And 15 wt% of Eu2O3The mixed powder is molded into a green body with the molding pressure of 70 MPa; placing SiO powder at the bottom of a crucible, wherein the mass ratio of SiO to carbon nano tubes is 11:1, placing a green body on a porous BN support in the middle of the crucible, placing the crucible in a multifunctional sintering furnace, introducing nitrogen, keeping the temperature at 1650 ℃ for 2 hours, heating the temperature to 1100 ℃ at the room temperature at the heating speed of 600 ℃/h, heating the temperature from 1100 ℃ to 1650 ℃ at the heating speed of 200 ℃/h, and carrying out carbothermic reduction nitridation reaction to generate a porous silicon nitride green body, wherein the mass ratio of SiO to carbon nano tubes is 10: 1; and continuously heating to 1750 ℃ for liquid phase sintering, wherein the heating rate is 150 ℃/h, keeping the temperature for 1 hour, and phase transformation occurs in the process to obtain the porous nano silicon nitride fiber framework with the porosity of 50%.
2) Preparing a nano silicon nitride fiber/epoxy resin composite material: grinding and flattening the surface of the porous nano silicon nitride fiber frame obtained in the step 1), then placing the porous nano silicon nitride fiber frame in absolute ethyl alcohol containing 3 wt% of silane coupling agent for surface modification, keeping the temperature at 80 ℃ for 5 hours, taking out and drying for 24 hours; stirring the mixed solution of bisphenol F type epoxy resin, curing agent and accelerator at a high speed for 3h, uniformly mixing, and defoaming in vacuum for 3 h; placing the preheated porous nano silicon nitride fiber framework in a mixed solution of epoxy resin, an accelerant and a curing agent for soaking for 2 hours; and curing for 48 hours in a vacuum oven at 130 ℃ to obtain the nano silicon nitride fiber/epoxy resin composite material with the silicon nitride volume fraction of 50 vol%.
EXAMPLE six
The epoxy resin is bisphenol S type epoxy resin, other process parameters are the same as those of the first embodiment, porous silicon nitride ceramic with the porosity of 68% is obtained, and finally the nano silicon nitride fiber/epoxy resin composite material with the silicon nitride volume fraction of 32 vol% is prepared.
EXAMPLE seven
The epoxy resin is bisphenol S type epoxy resin, other process parameters are the same as those of the two embodiments, porous silicon nitride ceramics with 39% porosity are obtained, and finally the nano silicon nitride fiber/epoxy resin composite material with 61 vol% of silicon nitride volume fraction is obtained.
EXAMPLE seven
The epoxy resin is bisphenol A type epoxy resin, other process parameters are the same as those in the fifth embodiment, porous silicon nitride ceramic with the porosity of 49% is obtained, and finally the nano silicon nitride fiber/epoxy resin composite material with the silicon nitride volume fraction of 51 vol% is prepared.
FIG. 1 is a microstructure photograph of the nano silicon nitride fiber/epoxy resin composite material obtained in example 1 of the present invention. As shown in the figure, the epoxy resin is uniformly impregnated into the porous nano silicon nitride ceramic framework, the nano silicon nitride is fibrous and is mutually overlapped, and the bonding state of the silicon nitride fiber/epoxy resin interface is good.
Claims (4)
1. A preparation method of a nano silicon nitride fiber/epoxy resin composite material is characterized in that the nano silicon nitride fiber/epoxy resin composite material is prepared by impregnating a mixed material of epoxy resin, an epoxy resin curing agent and an accelerant into a porous nano silicon nitride fiber framework and carrying out high-temperature curing, wherein the volume fraction of nano silicon nitride in the nano silicon nitride fiber/epoxy resin composite material is 20-50 vol%, and the preparation method specifically comprises the following steps:
1) preparing a porous nano silicon nitride fiber framework: according to the mass percentage, 20-90 wt% of carbon nano tube and 0-70 wt% of alpha-Si3N4And forming a green body by compression molding with 10-20 wt% of rare earth oxide mixed powder, placing SiO powder at the bottom of a crucible, placing the green body on a porous BN support in the middle of the crucible, placing the crucible in a multifunctional sintering furnace, introducing nitrogen, keeping the temperature of the crucible at 1500-1700 ℃ for 1-6 hours under the atmosphere pressure of 2.5-7 atm, and carrying out carbothermic reduction nitridation reaction to generate a porous silicon nitride green body, wherein the mass ratio of SiO to carbon nano tubes is (8-12): 1; continuously heating to 1750-1850 ℃ for liquid phase sintering for 0.5-2 hours, wherein phase transformation occurs in the process, and thus a porous nano silicon nitride fiber framework is obtained; the selected rare earth oxide is Y2O3，Lu2O3，Yb2O3，La2O3Or Eu2O3(ii) a The temperature rising speed of the multifunctional sintering furnace from room temperature to 1100 ℃ is 500-700 ℃/h, and the temperature rising speed of the multifunctional sintering furnace from 1100 ℃ to the sintering temperature is 100-300 ℃/h; the temperature rising speed of the carbothermal nitridation temperature rising to the liquid phase sintering temperature is 50-100 ℃/h;
2) preparing a nano silicon nitride fiber/epoxy resin composite material: grinding and flattening the surface of the porous nano silicon nitride fiber frame obtained in the step 1), then placing the porous nano silicon nitride fiber frame into absolute ethyl alcohol containing 2-5 wt% of silane coupling agent for surface modification, keeping the temperature at 60-80 ℃ for 2-5 h, taking out and drying for 24 h; stirring the mixed solution of the epoxy resin, the curing agent and the accelerator at a high speed for 2-4 h, uniformly mixing, and defoaming in vacuum for 2-4 h; placing the preheated porous nano silicon nitride fiber framework in a mixed solution of epoxy resin, an accelerant and a curing agent for soaking for 1-3 hours; curing under a set curing system to obtain the nano silicon nitride fiber/epoxy resin composite material, wherein the epoxy resin is any one of bisphenol A type epoxy resin, bisphenol F type epoxy resin or bisphenol S type epoxy resin, the epoxy resin curing agent is methyl tetrahydrophthalic anhydride, and the accelerator is trisphenol.
2. The method for preparing the nano silicon nitride fiber/epoxy resin composite material according to claim 1, wherein in the step 1), the average particle size of the selected silicon nitride is 0.2-0.5 μm, and the forming pressure is 20-80 MPa.
3. The method for preparing the nano silicon nitride fiber/epoxy resin composite material according to claim 1, wherein the compression molding pressure in the step 1) is 10-80 MPa, and the pressure holding time is 1 min.
4. The method for preparing the nano silicon nitride fiber/epoxy resin composite material according to claim 1, wherein the curing temperature schedule in the step 2) is as follows: and preserving the heat for 24-48 h at 130 ℃.
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