CN108530099B - Block carbon reinforcement/carbon composite material and preparation method thereof - Google Patents
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Abstract
The invention belongs to the technical field of material preparation, and particularly relates to a block carbon reinforcement/carbon composite material obtained by solid-phase reaction sintering and a preparation method thereof. The carbon fiber cloth is dried to obtain a prefabricated body of the carbon fiber cloth containing the diamond powder, then the prefabricated body is cut according to the required specification and laminated together, and pressure is applied under the protective atmosphere to obtain the carbon reinforcement/carbon composite material after high-temperature sintering. The block carbon reinforcement/carbon composite material prepared by the invention has high density and good mechanical property, and can be used for wear-resistant materials, electrode materials, nuclear energy industry and the like.
Description
Technical Field
The invention belongs to the technical field of material preparation, and particularly relates to a block carbon reinforcement/carbon composite material and a preparation method thereof.
Background
The carbon material has important application from zero-dimensional fullerene to one-dimensional carbon nanotube, to two-dimensional graphene, and finally to common three-dimensional carbon material graphite and diamond along with the history development process of human beings. The attention is increasing from single carbon materials to two-phase or even multi-phase carbon/carbon composites, and the application range is also increasing. However, the development bottleneck of the current carbon material, especially the composite material composed of carbon phase, is that the relative density of the prepared product is not very high, the synthesis method is mostly prepared by liquid phase impregnation or vapor deposition, the production period is longer, and the requirement on the growth environment is harsh. Compared with the traditional preparation of the carbon/carbon composite material, the preparation method has the advantages of short production period, relatively improved product density, simple preparation method and strong operability, and enlarges the application field of the carbon/carbon composite material.
Disclosure of Invention
In order to overcome the defects of the prior art and overcome the problem of long preparation period of the high-density and high-strength carbon/carbon composite material, the invention provides a block carbon reinforcement/carbon composite material obtained by solid-phase reaction sintering and a preparation method thereof. The invention is to evenly disperse the nano-diamond powder in the solvent, then dip the carbon fiber cloth in a slurry container containing the nano-diamond powder, then dry the carbon fiber cloth dipped with the slurry, cut the carbon fiber cloth according to the required specification, laminate the carbon fiber cloth together, apply pressure under the protective atmosphere and sinter the carbon fiber cloth at high temperature to obtain the carbon reinforcement/carbon composite material.
The invention adopts the specific technical scheme that:
a method for preparing a block carbon reinforcement/carbon composite material comprises the steps of preparing a precursor of the composite material, and converting the precursor into the block carbon reinforcement/carbon composite material through pressure sintering.
Further, the precursor: after diamond powder is uniformly dispersed in a solvent, carbon fiber cloth coated with an adhesive on the surface is soaked in a slurry container containing nano diamond powder, and then the carbon fiber cloth soaked with the slurry is dried to obtain the nano diamond carbon fiber cloth.
Further, the preparation process of the precursor of the composite material comprises the following steps:
(1) preparation of diamond dispersion: respectively weighing 2.4-2.6 g of modified diamond powder with the particle size of 80-100 nm and 0.24-0.26 g of modified diamond powder with the particle size of 40-50 nm, grinding and mixing; adding 50ml of solvent into the ground mixed powder, and performing ultrasonic dispersion for 20-30 min; obtaining stable diamond dispersion liquid;
(2) preparing a precursor of the bulk carbon reinforcement/carbon composite material: dipping the carbon fiber cloth coated with the adhesive on the surface in a prepared diamond dispersion liquid, drying and curing to obtain a prefabricated body of the carbon fiber cloth containing diamond powder;
in the step (1), the solvent is absolute ethyl alcohol.
In the step (2), the adhesive is an epoxy resin adhesive.
Further, the sintering process is that the precursor lamination of the composite material is placed in a mould and sintered under a protective atmosphere; applying 40-100 MPa pressure to the die during sintering; and when the highest sintering temperature is reached, preserving the heat for 2-8 min, and decompressing and cooling to room temperature. At high temperature, the diamond particles are transformed into graphite phase through phase transformation, and the graphite phase is filled in gaps among the carbon fiber cloth, so that the compact block carbon reinforcement/carbon composite material is obtained.
The mold is a graphite mold.
The protective atmosphere is argon.
When the sintering mode is spark plasma sintering; the heating rate is 100-150 ℃/min.
The initial temperature of pressurization is 900 ℃.
Compared with the prior art, the invention has the beneficial effects that:
the invention adopts a solid phase sintering mode to prepare the carbon/carbon composite material, and utilizes the advantages that the density of diamond is high, the atom activity of the diamond is high at high temperature, and the diamond is converted into a graphite phase with lower density through phase transformation volume expansion to fill the gaps among carbon fibers so as to improve the density of the product. Compared with the traditional carbon/carbon composite material, the traditional carbon/carbon composite material is mostly prepared by a liquid phase or gas phase method, the requirement on the growth environment is strict, the periodicity is longer, and the product density is not very high. The bulk carbon reinforcement/carbon composite material obtained by solid-phase reaction sintering has the advantages of high compactness of 90%, short production period, simple process and strong operability, and enlarges the application field of the carbon/carbon composite material, in particular to occasions with higher required performance, such as aerospace, military industry production and the like.
Drawings
FIG. 1 is a schematic flow diagram of the present invention for preparing a bulk carbon reinforcement/carbon composite.
Detailed Description
The following examples are provided to illustrate specific embodiments of the present invention in further detail.
Example 1:
as shown in the flow of the attached figure 1, the preparation method of the bulk carbon reinforcement/carbon composite material comprises the steps of preparation of a composite material precursor and sintering of the bulk carbon reinforcement/carbon composite material, and comprises the following specific steps:
(1) preparing a composite material precursor:
preparing a diamond dispersion liquid: respectively weighing 2.5g of surface-modified diamond powder with the particle size of 100nm and 0.25g of surface-modified diamond powder with the particle size of 50nm, putting the powder into a mortar for mixing, grinding for 10min, putting the ground powder into a 100ml beaker, dropwise adding 50ml of absolute ethyl alcohol into the beaker, putting the beaker into an ultrasonic cleaning instrument, and ultrasonically dispersing for 30min by adopting 120w power to obtain a stable diamond dispersion liquid;
preparing precursor powder of the block carbon reinforcement/carbon composite material: and (3) soaking the carbon fiber cloth coated with the epoxy resin adhesive on the surface in the prepared diamond dispersion liquid, drying and curing the prefabricated body of the carbon fiber cloth containing the diamond powder. (2) Sintering of the composite material:
cutting and laminating a prefabricated body of carbon fiber cloth containing diamond powder according to a certain shape, then placing the prefabricated body into a graphite mold with the inner diameter of 10mm, sintering by adopting discharge plasma under the protection of argon, wherein the heating rate is 150 ℃/min during sintering, the sintering temperature is 1600 ℃, the axial pressure is 40MPa, diamond particles are transformed into a graphite phase through the phase at high temperature, and the graphite phase is filled in gaps among the carbon fiber cloth, so that the compact 72% block carbon reinforcement/carbon composite material is obtained.
Example 2:
as shown in the flow of the attached figure 1, the preparation method of the bulk carbon reinforcement/carbon composite material comprises the steps of preparation of a composite material precursor and sintering of the bulk carbon reinforcement/carbon composite material, and comprises the following specific steps:
(1) preparing a composite material precursor:
preparing a diamond dispersion liquid: respectively weighing 2.5g of surface-modified diamond powder with the particle size of 100nm and 0.25g of surface-modified diamond powder with the particle size of 50nm, putting the powder into a mortar for mixing, grinding for 10min, putting the ground powder into a 100ml beaker, dropwise adding 50ml of absolute ethyl alcohol into the beaker, putting the beaker into an ultrasonic cleaning instrument, and ultrasonically dispersing for 30min by adopting 120w power to obtain a stable diamond dispersion liquid;
preparing precursor powder of the block carbon reinforcement/carbon composite material: and (3) soaking the carbon fiber cloth coated with the epoxy resin adhesive on the surface in the prepared diamond dispersion liquid, drying and curing the prefabricated body of the carbon fiber cloth containing the diamond powder. (2) Sintering of the composite material:
cutting and laminating a prefabricated body of carbon fiber cloth containing diamond powder according to a certain shape, placing the prefabricated body into a graphite mold with the inner diameter of 10mm, and sintering by adopting discharge plasma under the protection of argon, wherein the heating rate is 150 ℃/min, the sintering temperature is 1700 ℃, the axial pressure is 40MPa, and the heat preservation time is 5 min; at high temperature, the diamond particles are transformed into graphite phase through phase transformation, and the graphite phase is filled in gaps among the carbon fiber cloth, so that the block carbon reinforcement/carbon composite material with the density of 74.3% is obtained.
Example 3:
as shown in the flow of the attached figure 1, the preparation method of the bulk carbon reinforcement/carbon composite material comprises the steps of preparation of a composite material precursor and sintering of the bulk carbon reinforcement/carbon composite material, and comprises the following specific steps:
(1) preparing a composite material precursor:
preparing a diamond dispersion liquid: respectively weighing 2.5g of surface-modified diamond powder with the particle size of 100nm and 0.25g of surface-modified diamond powder with the particle size of 50nm, putting the powder into a mortar for mixing, grinding for 10min, putting the ground powder into a 100ml beaker, dropwise adding 50ml of absolute ethyl alcohol into the beaker, putting the beaker into an ultrasonic cleaning instrument, and ultrasonically dispersing for 30min by adopting 120w power to obtain a stable diamond dispersion liquid;
preparing precursor powder of the block carbon reinforcement/carbon composite material: and (3) soaking the carbon fiber cloth coated with the epoxy resin adhesive on the surface in the prepared diamond dispersion liquid, drying and curing the prefabricated body of the carbon fiber cloth containing the diamond powder. (2) Sintering of the composite material:
cutting and laminating a prefabricated body of carbon fiber cloth containing diamond powder according to a certain shape, placing the prefabricated body into a graphite mold with the inner diameter of 10mm, and sintering by adopting discharge plasma under the protection of argon, wherein the heating rate is 150 ℃/min, the sintering temperature is 1700 ℃, the axial pressure is 70MPa, and the heat preservation time is 5 min; at high temperature, the diamond particles are transformed into graphite phase through phase transformation, and the graphite phase is filled in gaps among the carbon fiber cloth, so that the block carbon reinforcement/carbon composite material with the density reaching 82.5% is obtained.
Example 4:
as shown in the flow of the attached figure 1, the preparation method of the bulk carbon reinforcement/carbon composite material comprises the steps of preparation of a composite material precursor and sintering of the bulk carbon reinforcement/carbon composite material, and comprises the following specific steps:
(1) preparing a composite material precursor:
preparing a diamond dispersion liquid: respectively weighing 2.5g of surface-modified diamond powder with the particle size of 100nm and 0.25g of surface-modified diamond powder with the particle size of 50nm, putting the powder into a mortar for mixing, grinding for 10min, putting the ground powder into a 100ml beaker, dropwise adding 50ml of absolute ethyl alcohol into the beaker, putting the beaker into an ultrasonic cleaning instrument, and ultrasonically dispersing for 30min by adopting 120w power to obtain a stable diamond dispersion liquid;
preparing precursor powder of the block carbon reinforcement/carbon composite material: and (3) soaking the carbon fiber cloth coated with the epoxy resin adhesive on the surface in the prepared diamond dispersion liquid, drying and curing the prefabricated body of the carbon fiber cloth containing the diamond powder. (2) Sintering of the composite material:
cutting and laminating a prefabricated body of carbon fiber cloth containing diamond powder according to a certain shape, placing the prefabricated body into a graphite mold with the inner diameter of 10mm, and sintering by adopting discharge plasma under the protection of argon, wherein the heating rate is 100 ℃/min, the sintering temperature is 1600 ℃, the axial pressure is 100MPa, and the heat preservation time is 5 min; at high temperature, the diamond particles are transformed into graphite phase through phase transformation, and the graphite phase is filled in gaps among the carbon fiber cloth, so that the block carbon reinforcement/carbon composite material with the density reaching 90.8% is obtained.
The above description is only for the purpose of illustrating embodiments of the present invention and is not to be construed as limiting the scope of the present invention, and modifications and variations of the above described embodiments may be made by those skilled in the art without departing from the spirit of the present invention.
Claims (4)
1. A preparation method of a block carbon reinforcement/carbon composite material is characterized by comprising the following steps: uniformly dispersing diamond powder in a solvent, soaking carbon fiber cloth in a slurry container containing nano diamond powder, drying the carbon fiber cloth soaked with the slurry, cutting according to the required specification, laminating the carbon fiber cloth, applying pressure under a protective atmosphere, and sintering at a high temperature to obtain the carbon reinforcement/carbon composite material; the method comprises the following steps:
(1) preparation of diamond dispersion: respectively weighing 2.4-2.6 g of modified diamond powder with the particle size of 80-100 nm and 0.24-0.26 g of modified diamond powder with the particle size of 40-50 nm, grinding and mixing; adding 50ml of solvent into the ground mixed powder, and performing ultrasonic dispersion for 20-30 min; obtaining stable diamond dispersion liquid;
(2) preparing a precursor of the bulk carbon reinforcement/carbon composite material: dipping the carbon fiber cloth coated with the adhesive on the surface in a prepared diamond dispersion liquid, drying and curing to obtain a prefabricated body of the carbon fiber cloth containing diamond powder;
(3) preparing a block carbon reinforcement/carbon composite material: cutting the prepared carbon fiber cloth preform containing diamond powder according to the required specification, laminating the carbon fiber cloth preform and the diamond powder preform together, applying pressure under a protective atmosphere, and sintering at a high temperature to obtain the carbon reinforcement/carbon composite material;
the sintering process comprises the following specific steps: weighing a precursor lamination of the composite material, and placing the precursor lamination into a mold, wherein the mold is a graphite mold; sintering under a protective atmosphere, wherein the protective atmosphere is argon; pressurizing the die at 900 ℃, wherein the applied pressure is 40-70 MPa; when the highest sintering temperature is reached, the highest temperature is 1600-1700 ℃; preserving heat for a certain time, wherein the heat preservation time is 2-8 min; then decompressing and cooling to room temperature;
when the sintering is discharge plasma sintering, the heating rate is 100-150 ℃/min.
2. The method of making a bulk carbon reinforcement/carbon composite of claim 1, wherein: the diamond powder is compounded by adopting at least two diamonds with different grain diameters.
3. The method of making a bulk carbon reinforcement/carbon composite of claim 1, wherein: in the step (1), the solvent is absolute ethyl alcohol.
4. The method of making a bulk carbon reinforcement/carbon composite of claim 1, wherein: in the step (2), the adhesive is an epoxy resin adhesive.
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