CN114771042A - Diamond carbon fiber composite material and preparation method thereof - Google Patents
Diamond carbon fiber composite material and preparation method thereof Download PDFInfo
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- CN114771042A CN114771042A CN202210458098.XA CN202210458098A CN114771042A CN 114771042 A CN114771042 A CN 114771042A CN 202210458098 A CN202210458098 A CN 202210458098A CN 114771042 A CN114771042 A CN 114771042A
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Abstract
The invention relates to a diamond carbon fiber composite material and a preparation method thereof, wherein the material is formed by overlapping self-supporting diamond diaphragms and carbon fiber layers which are alternately arranged in sequence along the up-down direction, and the top layer and the bottom layer of the material are both self-supporting diamond diaphragms; the carbon fiber layer may be pure carbon fiber or a composite body with diamond powder distributed in the carbon fiber. When the material is prepared, firstly, the CVD diamond film is subjected to shape cutting, thickness trimming and surface smoothing; then sequentially laying a carbon fiber layer and a diamond film on the surface of the diamond film, and bonding the carbon fiber layer and the diamond film together through a bonding agent; and finally, applying static pressure between the upper diamond film and the lower diamond film, discharging surplus adhesive and bubbles, and removing the static pressure after the adhesive is cured to obtain the diamond-carbon fiber composite material. The diamond carbon fiber composite material has the advantages of high heat conductivity, high strength, high toughness and low density, and is simple in preparation process, low in cost and easy for large-scale and batch production.
Description
Technical Field
The invention belongs to the technical field of thermal management materials and preparation thereof, and particularly relates to a diamond carbon fiber composite material and a preparation method thereof.
Background
With the rapid development of electronic technology, the power of components in the thermal control system of electronic equipment in the field of military and civilian is higher and higher, and the thermal management becomes more important, even becoming the bottleneck of the development of high-power electronic devices. However, at present, it is increasingly difficult for general-purpose metals (Al, Cu), ceramics (SiC, AlN), metal matrix composite materials (Cu/Mo, Al/SiC), and the like to meet the heat dissipation requirements of high-power electronic devices. Therefore, developing a new generation of high thermal conductivity material to ensure stable operation of the thermal control system of the high-power electronic device becomes a research and development focus in the field of thermal management materials.
Unlike metal which relies on peripheral electrons for heat transfer, diamond relies on phonons for heat transfer, and the thermal conductivity of the diamond at room temperature can reach 2000W/(m.K) at most, which is 5 times that of copper. Meanwhile, the diamond has excellent insulating property and low thermal expansion coefficient and density, so that the diamond becomes the best material for thermal management application of high-power electronic equipment. Currently, there are three main types of diamond applications in thermal management materials: CVD diamond film was used alone; welding the CVD diamond film and metal to form a composite radiating fin; diamond powder/particles and metals such as copper, aluminum and the like form a composite material. Diamond alone as a heat sink material faces the following problems: the diamond thick film has long growth period, difficult deep processing and high cost; the diamond film is hard and brittle, has poor toughness and is easy to break. The problems of welding the diamond film and the metal are as follows: the diamond has high chemical inertia and poor infiltration with metal materials, and is difficult to form good interface combination; the difference between the thermal expansion coefficients of diamond and metal is large, and thermal shock can cause deformation disorder. The compounding of diamond powder/particles with metals such as copper, aluminum and the like has the problems of high interface thermal resistance and small compounding thermal conductivity.
The carbon fiber has high tensile strength and small thermal expansion coefficient (even negative value-1.5 multiplied by 10)-6/° c), light specific gravity and the like. If the diamond and the carbon fiber are compounded, the advantages of ultrahigh heat conduction of the diamond and the advantages of high strength and high toughness of the carbon fiber are hopefully integrated. Although carbon fiber and diamond are the same carbon material, the carbon fiber and the diamond have different structures and are difficult to compound, so that a composite material of the carbon fiber and the diamond is not developed at present. According to the invention, through the structural and functional integrated design of the material, the diamond carbon fiber composite heat management material with high heat conductivity, high strength, high toughness and low density is prepared and obtained, and the heat dissipation requirement of a high-power electronic device is met.
Disclosure of Invention
Aiming at the problem that the heat management material in the prior art cannot meet the increasing heat dissipation requirements of high-power electronic devices, the invention provides a diamond carbon fiber composite material.
The invention is realized by the following two technical schemes:
the first technical scheme provided by the invention is as follows:
a diamond carbon fiber composite material is formed by overlapping self-supporting diamond diaphragms and carbon fiber layers which are sequentially and alternately arranged in an up-down direction, and the top layer and the bottom layer of the diamond carbon fiber composite material are self-supporting diamond diaphragms; the carbon fiber layer is a carbon fiber-cured binder composite, and the structure of the composite is a carbon fiber reinforced cured binder, as shown in fig. 1.
According to a preferable technical scheme, in the diamond-carbon fiber composite material, the self-supporting diamond diaphragm is prepared by a CVD method, the thermal conductivity is more than or equal to 600W/(m.K), the flatness is less than or equal to 0.1mm, the parallelism is less than or equal to 0.1mm, and the roughness Ra is less than or equal to 0.05 mm; the thickness of the self-supporting diamond diaphragm is 0.3 mm-1 mm, and the thickness of the carbon fiber layer is 0.1 mm-0.3 mm.
Furthermore, the invention also provides a preparation method of the diamond-carbon fiber composite material, which solves the problems that diamond is difficult to deposit on the surface of carbon fiber in a film form, and the diamond and the carbon fiber are difficult to connect and compound. The preparation method specifically comprises the following steps:
step 1: selecting a self-supporting diamond film with proper diameter and thickness according to the size requirement of the diamond carbon fiber composite material on the self-supporting diamond film, cutting the self-supporting diamond film into a set shape by adopting a laser cutting machine, and then performing thickness trimming and surface smoothing treatment on the self-supporting diamond film obtained by cutting by adopting a laser faceting machine to obtain the self-supporting diamond film meeting the composite requirement;
step 2: uniformly blending a binder and absolute ethyl alcohol, soaking carbon fibers in a blending solution for 1-5 minutes, taking out the carbon fibers, placing the carbon fibers in the air for 10-30 minutes, then flatly paving and bonding the carbon fibers soaked with the binder on a self-supporting diamond membrane, placing a layer of self-supporting diamond membrane on a carbon fiber layer, and repeating the process of alternately flatly paving the carbon fibers soaked with the binder and the self-supporting diamond membrane until the composite thickness meets the requirement to obtain a composite layer structure;
and step 3: clamping the side face of the composite layer structure after the composite through a clamping frame to ensure the flatness of the composite layer structure, meanwhile, placing a heavy object on the surface of the top layer self-supporting diamond membrane, discharging surplus adhesive in the carbon fiber layer and bubbles dispersed in the adhesive by virtue of normal static pressure of the heavy object, and then heating and curing the adhesive under the condition of keeping the side face clamping and the top layer applying pressure;
and 4, step 4: and removing the heavy object and the clamping frame, polishing and ultrasonically cleaning the side surface of the composite layer structure, and finally obtaining the diamond carbon fiber composite material.
According to the preferable technical scheme, in the preparation method of the diamond carbon fiber composite material, in the step 2, the binder is barium-phenolic resin, epoxy resin or modified epoxy resin, and the mixing ratio of the binder to absolute ethyl alcohol is 1: 1-1: 5; in the step 3, the heating temperature of heating and curing is 200-300 ℃, and the temperature is kept for 3-8 hours; in the step 3, the clamping frame is made of loose materials or through holes for discharging the binder are processed on the clamping frame.
The second technical scheme provided by the invention is as follows:
a diamond carbon fiber composite material is formed by overlapping self-supporting diamond diaphragms and carbon fiber layers which are sequentially and alternately arranged in an up-down direction, and the top layer and the bottom layer of the diamond carbon fiber composite material are self-supporting diamond diaphragms; the carbon fiber layer is a carbon fiber-diamond micro powder-curing binder complex, the structure of the complex is a carbon fiber reinforced curing binder, and the diamond micro powder is dispersed and distributed in the complex, as shown in fig. 3.
According to a preferable technical scheme, in the diamond-carbon fiber composite material, the self-supporting diamond diaphragm is prepared by a CVD method, the thermal conductivity is more than or equal to 600W/(m.K), the flatness is less than or equal to 0.1mm, the parallelism is less than or equal to 0.1mm, and the roughness Ra is less than or equal to 0.05 mm; the thickness of the self-supporting diamond diaphragm is 0.3 mm-1 mm, and the thickness of the carbon fiber layer is 0.1 mm-0.3 mm; the curing binder is a cured body of barium phenolic resin, epoxy resin and modified epoxy resin; the particle size of the diamond micro powder is 100 nm-10 mu m.
Furthermore, the invention also provides a preparation method of the diamond-carbon fiber composite material, which solves the problems that diamond is difficult to deposit on the surface of carbon fiber in a film form, and the diamond and the carbon fiber are difficult to connect and compound. The preparation method specifically comprises the following steps:
step 1: selecting a self-supporting diamond film with proper diameter and thickness according to the size requirement of the diamond carbon fiber composite material on the self-supporting diamond film, cutting the self-supporting diamond film into a set shape by adopting a laser cutting machine, and then performing thickness trimming and surface smoothing treatment on the self-supporting diamond film by adopting a laser surface trimming machine to obtain the self-supporting diamond film meeting the composite requirement;
step 2: the diamond micro powder, the curing binder and the absolute ethyl alcohol are mixed according to a proportion, and a stirrer is adopted to uniformly disperse the diamond micro powder;
and step 3: soaking carbon fiber tows in a binder preparation containing diamond micropowder, taking out, spreading and bonding carbon fibers on a self-supporting diamond membrane, placing a layer of self-supporting diamond membrane on the carbon fiber layer, and repeating the process of alternately spreading the carbon fibers soaked with the binder and the self-supporting diamond membrane until the composite thickness meets the requirement to obtain a composite layer structure;
and 4, step 4: clamping the side face of the composite layer structure after the composite through a clamping frame to keep the flatness of the composite layer structure, meanwhile, placing a heavy object on the surface of the top layer self-supporting diamond membrane, discharging surplus adhesive in the carbon fiber layer and bubbles dispersed in the adhesive by virtue of normal static pressure of the heavy object, and then heating and curing the adhesive under the condition of keeping the side face clamping and the top layer applying pressure;
and 5: and removing the heavy object and the clamping frame, polishing and ultrasonically cleaning the side surface of the composite layer structure, and finally obtaining the diamond carbon fiber composite material.
As a preferred technical scheme, in the step 2, when the diamond micro powder, the curing binder and the absolute ethyl alcohol are prepared, the ratio of the diamond micro powder to the curing binder is 1: 1-1: 5, and the ratio of the whole diamond micro powder to the curing binder to the absolute ethyl alcohol is 1: 2-1: 10; in the step 4, the heating temperature for heating and curing is 200-300 ℃, and the temperature is kept for 3-8 hours; in the step 4, the clamping frame is made of loose materials or through holes for discharging the binder are processed on the clamping frame.
The two technical schemes provided by the invention have the following beneficial effects:
1) the diamond carbon fiber composite material has the advantages that the thermal conductivity of diamond is high, the heat dissipation performance is excellent, the carbon fiber has high tensile strength and high toughness, the two technical schemes of the invention utilize adhesives such as barium phenolic resin, epoxy resin, modified epoxy resin and the like, the invention combines two carbon materials with excellent performance of a CVD self-supporting diamond membrane and the carbon fiber, the performance complementation of the two carbon materials is realized, the diamond carbon fiber composite material is prepared, the material can have the high thermal conductivity of diamond and the high tensile strength and high toughness of the carbon fiber, and can be used as a thermal management material with high thermal conductivity, high strength, high toughness and low density, and the mechanical impact and thermal impact can be effectively resisted.
2) The composite material surface of the two technical schemes has excellent thermal conductivity, the self-supporting diamond membranes are used as the composite material, and the plurality of self-supporting diamond membranes in the horizontal direction can be used as efficient heat dissipation channels to quickly transfer contact heat, so that the horizontal direction has higher thermal conductivity which can reach about 90% of diamond; considering the problems that the thermal conductivity of the resin binder is not high, the normal thermal conductivity is influenced due to the existence of interface thermal resistance and the like, the normal thermal conductivity of the first technical scheme of the invention is lower, and the invention is suitable for being applied to occasions only requiring high thermal conductivity in the horizontal direction; in the second technical scheme provided by the invention, the diamond micro powder is added into the binder, and the existence of the diamond micro powder enables the resin binder to be changed into a diamond/resin binder composite material, so that the thermal conductivity of the resin binder is greatly improved, and the diamond carbon fiber composite material is ensured to have higher thermal conductivity in the upward direction, and the diamond carbon fiber composite material is particularly suitable for being used as a heat dissipation bracket in thermal control systems in the fields of aerospace, nuclear industry and the like.
3) The diamond carbon fiber composite material is formed by bonding two materials through an adhesive, and the shapes and the thicknesses of the two materials are adjustable, so that the overall shape and the thickness of the composite material can be flexibly adjusted according to the space of a thermal control system, and the thermal conductivity can be regulated and controlled according to the cost and the actual requirement.
Drawings
The schematic drawings in the present application are only for the purpose of further understanding the present application and do not constitute an undue limitation of the present application.
Fig. 1 is a schematic structural diagram of a diamond carbon fiber composite material according to a first technical scheme of the invention.
Fig. 2 is a schematic diagram of the preparation of the diamond carbon fiber composite material according to the first technical scheme of the invention.
Fig. 3 is a schematic structural diagram of a diamond carbon fiber composite material according to a second technical scheme of the invention.
Fig. 4 is a schematic diagram of the preparation of the diamond carbon fiber composite material according to the second technical scheme of the invention.
Fig. 5 is a schematic structural view of the diamond carbon fiber composite material prepared in example 1.
Fig. 6 is a schematic structural view of the diamond carbon fiber composite material prepared in example 2.
Fig. 7 is a schematic structural view of the diamond carbon fiber composite material prepared in example 3.
Fig. 8 is a schematic structural view of the diamond carbon fiber composite material prepared in example 4.
Fig. 9 is a schematic structural view of the diamond carbon fiber composite material prepared in example 5.
Fig. 10 is a schematic structural view of the diamond carbon fiber composite material prepared in example 6.
In the figure: 1-self-supporting diamond membrane, 2-carbon fiber layer, 3-diamond micro powder, 4-clamping frame and 5-weight.
Detailed Description
The present invention will be further described with reference to the following examples, but is not limited to the following examples. All other embodiments obtained by a person skilled in the art without making any inventive step are within the scope of protection of the present invention.
Example 1:
a diamond carbon fiber composite material comprises an upper self-supporting diamond diaphragm 1, a lower self-supporting diamond diaphragm 1 and a carbon fiber layer 2 sandwiched between the upper self-supporting diamond diaphragm 1 and the lower self-supporting diamond diaphragm 2, wherein the length, the width and the thickness of the self-supporting diamond diaphragm 1 are 30 mm multiplied by 20 mm multiplied by 1.0 mm, and the length, the width and the thickness of the carbon fiber layer 2 are 30 mm multiplied by 20 mm multiplied by 0.3 mm, as shown in figure 5.
The specific preparation method of the diamond carbon fiber composite material comprises the following steps:
step 1: selecting a CVD self-supporting diamond film with the diameter of 52 mm, the thickness of 1.2 mm, the tensile strength of 1000 MPa and the thermal conductivity of 600W/(m.K), designing an array of 30 mm multiplied by 20 mm by considering the cutting loss, and cutting by adopting a laser cutting machine, wherein the laser power is 12W and the frequency is 6 Hz; then, a laser face trimming machine is adopted to carry out thickness trimming and surface smoothing treatment on the self-supporting diamond film obtained by cutting, the laser power is 1000W during the thickness trimming, the trimming speed in the thickness direction is 0.02 mu m/d, the laser power is 450W during the surface smoothing treatment, the surface flatness of the self-supporting diamond film after the surface trimming treatment is 0.1mm, the parallelism is 0.1mm, and the roughness is 0.05mm, so that a self-supporting diamond film 1 is obtained;
and 2, step: uniformly blending barium phenolic resin and absolute ethyl alcohol according to a ratio of 1:5, soaking a 12K carbon fiber bundle with tensile strength of 5000 Mpa and elastic modulus of 230 GPa in the solution for 5 minutes, taking out the carbon fiber bundle, standing the carbon fiber bundle in the air for 30 minutes, and then flatly paving and bonding the carbon fiber bundle between two layers of self-supporting diamond membranes 1 to obtain a composite layer structure;
and 3, step 3: a clamping frame 4 made of loose materials is adopted, 5N clamping force is applied to four side faces of the composite layer structure after the composite layer structure is compounded to enable the composite layer structure to be flat, meanwhile, a weight 5 with the mass of 0.5 Kg is placed on the surface of the upper layer self-supporting diamond membrane 1, and the surplus resin in the carbon fibers and a small amount of bubbles dispersed in the resin are discharged by means of normal static pressure of the weight; heating and curing the barium phenolic resin under the condition of keeping side clamping and applying pressure on the upper surface layer, slowly heating to 300 ℃, and preserving heat for 8 hours;
and 4, step 4: and (3) removing the weight 5 and the clamping frame 4, grinding and ultrasonically cleaning four side surfaces of the composite layer structure, removing the end parts of the side-surface-cured barium phenolic resin and the carbon fiber leakage, grinding with 320-800 # SiC carborundum paper, ultrasonically cleaning with acetone for 15 minutes, and finally preparing the diamond-carbon fiber composite material, wherein the step is shown in figure 5.
The diamond carbon fiber composite material prepared by the steps has the in-plane thermal conductivity of about 500W/(m.K) and the tensile strength of about 2500 MPa, and is improved by 2.5 times compared with the tensile strength of diamond.
Example 2:
a diamond carbon fiber composite material is formed by overlapping self-supporting diamond diaphragms 1 and carbon fiber layers 2 which are sequentially and alternately arranged in an up-down direction, and the top layer and the bottom layer of the diamond carbon fiber composite material are both self-supporting diamond diaphragms 1; the self-supporting diamond diaphragm 1 has ten layers in total, the carbon fiber layer 2 has nine layers in total, the length, width and thickness of the self-supporting diamond diaphragm 1 are 15 mm multiplied by 0.6 mm, and the length, width and thickness of the carbon fiber layer 2 are 15 mm multiplied by 0.2 mm, as shown in fig. 6;
the specific preparation method of the diamond carbon fiber composite material comprises the following steps:
step 1: selecting a CVD self-supporting diamond film with the diameter of 55 mm, the thickness of about 0.8 mm, the tensile strength of 600 MPa and the thermal conductivity of 1000W/(m.K), designing an array of 15 mm multiplied by 15 mm by considering the cutting loss, and cutting by adopting a laser cutting machine, wherein the laser power is 11W and the frequency is 7 Hz; then, a laser faceting machine is adopted to carry out thickness trimming and surface smoothing treatment on the self-supporting diamond film obtained by cutting, the laser power is 900W when the thickness is trimmed, the trimming speed along the thickness direction is 0.02 mu m/d, the laser power is 400W when the surface is smoothed, the surface flatness of the self-supporting diamond film after the faceting treatment is 0.08mm, the parallelism is 0.08mm, and the roughness is 0.03 mm, so that the self-supporting diamond film 1 is obtained;
step 2: uniformly blending epoxy resin and absolute ethyl alcohol according to a ratio of 1:3, soaking 12K carbon fiber bundles with the tensile strength of 4500 MPa and the elastic modulus of 230 GPa in the solution for 3 minutes, taking out the carbon fiber bundles, placing the carbon fiber bundles in the air for 20 minutes, then flatly paving and bonding the carbon fiber bundles between two layers of self-supporting diamond membranes 1, and alternately flatly paving the carbon fiber bundles soaked with the epoxy resin and the self-supporting diamond membranes 1 until the composite thickness meets the requirement, and orthogonally paving adjacent carbon fiber bundle layers to improve the composite strength to obtain a composite layer structure;
and step 3: a clamping frame 4 made of loose materials is adopted, 5N clamping force is applied to four side faces of the composite layer structure to enable the composite layer structure to be flat, meanwhile, a weight 5 with the mass of 0.8 Kg is placed on the surface of the self-supporting diamond membrane 1 on the uppermost layer, and surplus resin in carbon fibers and a small amount of bubbles dispersed in the resin are discharged by means of normal static pressure; heating and curing the epoxy resin under the state of keeping the side clamping and the upper surface layer to apply pressure, slowly heating to 260 ℃, and preserving heat for 6 hours;
and 4, step 4: and (3) removing the clamping frame 4 and the weight 5, polishing and ultrasonically cleaning four side surfaces of the composite layer structure, removing the epoxy resin solidified on the side surfaces and the end part of the carbon fiber which leaks, polishing by using 320 to 800# SiC carborundum paper, ultrasonically cleaning by using acetone for 15 minutes, and finally preparing the diamond-carbon fiber composite material as shown in figure 6.
The diamond carbon fiber composite material prepared by the steps has the in-plane thermal conductivity of about 900W/(m.K) and the tensile strength of about 1600 MPa, and is improved by 2.7 times compared with the tensile strength of diamond.
Example 3:
a diamond carbon fiber composite material is formed by overlapping self-supporting diamond diaphragms 1 and carbon fiber layers 2 which are sequentially and alternately arranged along the up-down direction, and the top layer and the bottom layer of the composite material are both self-supporting diamond diaphragms 1; twenty layers in total for the self-supporting diamond diaphragm 1 and nineteen layers in total for the carbon fiber layer 2, wherein the length, width and thickness of the self-supporting diamond diaphragm 1 are 10 mm × 5mm × 0.3 mm, and the length, width and thickness of the carbon fiber layer 2 are 10 mm × 5mm × 0.1mm, as shown in fig. 7;
the specific preparation method of the diamond carbon fiber composite material comprises the following steps:
step 1: selecting a CVD self-supporting diamond film with the diameter of 20 mm, the thickness of 0.5 mm, the tensile strength of 500 MPa and the thermal conductivity of 2000W/(m.K), designing an array of 10 mm multiplied by 5mm by considering the cutting loss, and cutting by adopting a laser cutting machine, wherein the laser power is 10W, and the frequency is 8 Hz; then, a laser faceting machine is adopted to carry out thickness trimming and surface smoothing treatment on the self-supporting diamond film obtained by cutting, the laser power is 850W when the thickness is trimmed, the trimming speed along the thickness direction is 0.02 mu m/d, the laser power is 350W when the surface is smoothed, the surface flatness of the diamond after the faceting treatment is 0.05mm, the parallelism is 0.05mm, and the roughness is 0.01mm, thus obtaining a self-supporting diamond film 1;
and 2, step: uniformly blending modified epoxy resin and absolute ethyl alcohol according to a ratio of 1:1, soaking 12K carbon fiber bundles with the tensile strength of 4000 Mpa and the elastic modulus of 200 GPa in the solution for 1 minute, taking out the carbon fiber bundles, placing the carbon fiber bundles in the air for 10 minutes, then flatly paving and bonding the carbon fiber bundles between two layers of self-supporting diamond membranes 1, alternately flatly paving the carbon fiber bundles soaked with the modified epoxy resin and the self-supporting diamond membranes 1 until the composite thickness meets the requirement, and orthogonally flatly paving adjacent carbon fiber bundle layers to improve the composite strength to obtain a composite layer structure;
and step 3: a clamping frame 4 with a through hole is adopted to apply 5N clamping force to four side surfaces of the composite layer structure to enable the composite layer structure to be flat, meanwhile, a weight 5 with the mass of 1 Kg is placed on the surface of the self-supporting diamond membrane 1 on the uppermost layer, and the surplus resin in the carbon fiber and a small amount of bubbles dispersed in the resin are discharged by means of the normal static pressure of the weight; heating and curing the modified epoxy resin under the condition of keeping the side clamping and the upper surface layer to apply pressure, slowly heating to 200 ℃, and preserving heat for 3 hours;
and 4, step 4: and (3) removing the clamping frame 4 and the weight 5, polishing and ultrasonically cleaning four side surfaces of the composite layer structure, removing the modified epoxy resin solidified on the side surfaces and the end part of the carbon fiber which leaks, wherein the polishing adopts 320 to 800# SiC carborundum paper, the ultrasonic cleaning selects acetone, the cleaning time is 15 minutes, and finally the diamond carbon fiber composite material is prepared, as shown in figure 7.
The diamond carbon fiber composite material prepared by the steps has the in-plane thermal conductivity of about 1800W/(m.K) and the tensile strength of about 1500 MPa, and is improved by 3 times compared with the tensile strength of diamond.
Example 4:
a kind of diamond carbon fiber composite material, it is made up of upper, lower two-layer self-supporting diamond diaphragm 1 and carbon fiber layer 2 that is inserted in it among them, the length, width, thickness of the self-supporting diamond diaphragm 1 are 35 mm x 25 mm x 0.8 mm, the length, width, thickness of the carbon fiber layer 2 are 35 mm x 25 mm x 0.3 mm; the carbon fiber layer 2 is a carbon fiber-diamond micro powder 3-curing adhesive composite, the structure of the composite is a carbon fiber reinforced curing adhesive, and the diamond micro powder 3 is dispersed in the composite, as shown in fig. 8.
The specific preparation method of the diamond carbon fiber composite material comprises the following steps:
step 1: selecting a CVD self-supporting diamond film with the diameter of 65 mm, the thickness of 1mm, the tensile strength of 1000 MPa and the thermal conductivity of 800W/(m.K), designing an array of 35 mm multiplied by 25 mm by considering the cutting loss, and cutting by adopting a laser cutting machine, wherein the laser power is 12W and the frequency is 6 Hz; then, a laser surface trimming machine is adopted to perform thickness trimming and surface smoothing treatment on the self-supporting diamond film, the laser power is 1000W during the thickness trimming, the trimming speed along the thickness direction is 0.02 mu m/d, the laser power is 450W during the surface smoothing treatment, the surface flatness of the self-supporting diamond film after the surface trimming treatment is 0.1mm, the parallelism is 0.1mm, and the roughness is 0.05mm, so that the self-supporting diamond film 1 is obtained;
and 2, step: selecting diamond micro powder 3 with the particle size of 10 microns, firstly blending the diamond micro powder and barium phenolic resin according to the proportion of 1:5, and then uniformly blending the whole diamond micro powder and barium phenolic resin with absolute ethyl alcohol according to the proportion of 1: 2;
and step 3: soaking 12K carbon fiber bundles with the tensile strength of 4500 MPa and the elastic modulus of 220 GPa in the solution for 5 minutes, taking out the carbon fiber bundles, placing the carbon fiber bundles in the air for 30 minutes, and then flatly paving and bonding the carbon fiber bundles between two layers of self-supporting diamond membranes 1 to obtain a composite layer structure;
and 4, step 4: a clamping frame 4 with a through hole is adopted to apply 5N clamping force to four side faces of the composite layer structure to enable the composite layer structure to be flat, meanwhile, a weight 5 with the mass of 0.5 Kg is placed on the surface of the upper self-supporting diamond membrane 1, and surplus resin in the carbon fiber and a small amount of bubbles dispersed in the resin are discharged by means of normal static pressure; heating and curing the barium phenolic resin under the condition of keeping side clamping and applying pressure on the upper surface layer, slowly heating to 300 ℃, and preserving heat for 8 hours;
and 5: and (3) removing the weight 5 and the clamping frame 4, polishing and ultrasonically cleaning four side surfaces of the composite layer structure, removing the end parts of the barium-phenolic resin cured on the side surfaces and the carbon fiber leakage, polishing by using 320# -800 # SiC carborundum paper, ultrasonically cleaning by using acetone for 15 minutes, and finally preparing the diamond-carbon fiber composite material, wherein the step is shown in figure 8.
The diamond carbon fiber composite material prepared by the steps has the in-plane thermal conductivity of about 700W/(m.K), the normal thermal conductivity of about 550W/(m.K) and the tensile strength of about 2200 MPa, and is improved by 2.2 times compared with the tensile strength of diamond.
Example 5:
a diamond carbon fiber composite material is formed by overlapping self-supporting diamond diaphragms 1 and carbon fiber layers 2 which are sequentially and alternately arranged along the up-down direction, and the top layer and the bottom layer of the composite material are both self-supporting diamond diaphragms 1; the self-supporting diamond diaphragm 1 has five layers in total, and the length, width and thickness of each layer of self-supporting diamond diaphragm 1 are 20 mm multiplied by 0.6 mm; the carbon fiber layers 2 are four layers in total, and the length, width and thickness of each carbon fiber layer 2 are 20 mm multiplied by 0.2 mm; the carbon fiber layer 2 is a carbon fiber-diamond micro powder 3-curing adhesive composite, the structure of the composite is a carbon fiber reinforced curing adhesive, and the diamond micro powder 3 is dispersed in the composite, as shown in fig. 9.
The specific preparation method of the diamond carbon fiber composite material comprises the following steps:
step 1: selecting a CVD self-supporting diamond film with the diameter of 65 mm, the thickness of 0.8 mm, the tensile strength of 800 MPa and the thermal conductivity of 1200W/(m.K), designing an array of 20 mm multiplied by 20 mm by considering the cutting loss, and cutting by adopting a laser cutting machine, wherein the laser power is 11W and the frequency is 7 Hz; then, a laser surface trimming machine is adopted to perform thickness trimming and surface smoothing treatment on the self-supporting diamond film, the laser power is 900W when the thickness is trimmed, the trimming speed along the thickness direction is 0.02 mu m/d, the laser power is 400W when the surface is smoothed, the surface flatness of the self-supporting diamond film after the surface trimming treatment is 0.08mm, the parallelism is 0.08mm, and the roughness is 0.03 mm, so that the self-supporting diamond film 1 is obtained;
and 2, step: selecting diamond micro powder 3 with the particle size of 2.5 microns, firstly blending the diamond micro powder and epoxy resin according to the proportion of 1:2, and then uniformly blending the whole diamond micro powder and the epoxy resin with absolute ethyl alcohol according to the proportion of 1: 8;
and 3, step 3: placing 12K carbon fiber bundles with the tensile strength of 4000 MPa and the elastic modulus of 200 GPa in the solution for soaking for 3 minutes, taking out the carbon fiber bundles, placing the carbon fiber bundles in the air for 20 minutes, then flatly paving and bonding the carbon fiber bundles on a self-supporting diamond membrane 1, placing a layer of self-supporting diamond membrane 1 on the self-supporting diamond membrane, and alternately flatly paving the carbon fiber bundles soaked with the bonding agent and the self-supporting diamond membrane 1 until the composite thickness meets the requirement, wherein adjacent carbon fiber bundle layers are orthogonally flatly paved to improve the composite strength to obtain a composite layer structure;
and 4, step 4: a clamping frame 4 made of loose materials is adopted, 5N clamping force is applied to four side surfaces of the composite layer structure to enable the composite layer structure to be flat, meanwhile, a weight 5 with the mass of 0.8 Kg is placed on the surface of the self-supporting diamond membrane 1 on the uppermost layer, and the surplus resin in the carbon fiber and a small amount of bubbles dispersed in the resin are discharged by means of normal static pressure; heating and curing the epoxy resin under the state of keeping side clamping and applying pressure on the upper surface layer, slowly heating to 260 ℃, and preserving heat for 6 hours;
and 5: and (3) removing the weight 5 and the clamping frame 4, grinding and ultrasonically cleaning four side surfaces of the composite layer structure, removing the epoxy resin solidified on the side surfaces and the end part of the carbon fiber which leaks, grinding with 320-800 # SiC carborundum paper, ultrasonically cleaning with acetone for 15 minutes, and finally preparing the diamond-carbon fiber composite material, wherein the step is shown in figure 9.
The diamond carbon fiber composite material prepared by the steps has the in-plane thermal conductivity of about 1100W/(m.K), the normal thermal conductivity of about 900W/(m.K), and the tensile strength of about 1900 MPa, which is improved by 2.4 times compared with the tensile strength of diamond.
Example 6:
a diamond carbon fiber composite material is formed by overlapping self-supporting diamond diaphragms 1 and carbon fiber layers 2 which are sequentially and alternately arranged in an up-down direction, and the top layer and the bottom layer of the diamond carbon fiber composite material are both self-supporting diamond diaphragms 1; the self-supporting diamond diaphragm 1 has nine layers, and the length, the width and the thickness of each layer of self-supporting diamond diaphragm 1 are 15 mm multiplied by 10 mm multiplied by 0.4 mm; the carbon fiber layers 2 are eight layers in total, and the length, width and thickness of each carbon fiber layer 2 are 20 mm multiplied by 0.1 mm; the carbon fiber layer 2 is a carbon fiber-diamond micro powder 3-curing adhesive composite, the structure of the composite is a carbon fiber reinforced curing adhesive, and the diamond micro powder 3 is dispersed in the composite, as shown in fig. 10.
The specific preparation method of the diamond carbon fiber composite material comprises the following steps:
step 1: selecting a CVD self-supporting diamond film with the diameter of 32 mm, the thickness of 0.6 mm, the tensile strength of 600 MPa and the thermal conductivity of 1800W/(m.K), designing an array of 15 mm multiplied by 10 mm by considering the cutting loss, and cutting by adopting a laser cutting machine, wherein the laser power is 10W and the frequency is 8 Hz; then, a laser trimming machine is adopted to carry out thickness trimming and surface smoothing treatment on the diamond diaphragm, the laser power is 850W during the thickness trimming, the trimming speed in the thickness direction is 0.02 mu m/d, the laser power is 350W during the surface smoothing treatment, the flatness of the diamond surface is 0.05mm, the parallelism is 0.05mm, and the roughness is 0.01mm after the surface trimming treatment, so that the self-supporting diamond diaphragm 1 is obtained;
and 2, step: selecting diamond micro powder 3 with the particle size of 100 nm, firstly blending the diamond micro powder and the modified epoxy resin according to the proportion of 1:3, and then uniformly blending the whole diamond micro powder and the modified epoxy resin with absolute ethyl alcohol according to the proportion of 1: 10;
and step 3: placing 12K carbon fiber bundles with tensile strength of 3800 MPa and elastic modulus of 190 GPa in the solution for soaking for 1 minute, taking out the carbon fiber bundles, placing the carbon fiber bundles in the air for 10 minutes, then flatly paving and bonding the carbon fiber bundles on a self-supporting diamond membrane 1, placing a layer of self-supporting diamond membrane 1 on the self-supporting diamond membrane, and alternately flatly paving the carbon fiber bundles soaked with the bonding agent and the self-supporting diamond membrane 1 until the composite thickness meets the requirement, wherein adjacent carbon fiber bundle layers are orthogonally flatly paved to improve the composite strength to obtain a composite layer structure;
and 4, step 4: a clamping frame 4 with a through hole is adopted to apply 5N clamping force to four side surfaces of the composite layer structure to enable the composite layer structure to be flat, meanwhile, a weight 5 with the mass of 1 Kg is placed on the surface of the self-supporting diamond membrane 1 on the uppermost layer, and the surplus resin in the carbon fiber and a small amount of bubbles dispersed in the resin are discharged by means of the normal static pressure of the weight; heating and curing the modified epoxy resin under the condition of keeping the side clamping and the upper surface layer to apply pressure, slowly heating to 200 ℃, and preserving heat for 3 hours;
and 5: and (3) removing the weight 5 and the clamping frame 4, grinding and ultrasonically cleaning four side surfaces of the composite layer structure, removing the modified epoxy resin solidified on the side surfaces and the end part of the carbon fiber which leaks, grinding with 320-800 # SiC carborundum paper, ultrasonically cleaning with acetone for 15 minutes, and finally preparing the diamond-carbon fiber composite material as shown in figure 10.
The diamond carbon fiber composite material prepared by the steps has the in-plane thermal conductivity of about 1650W/(m.K), the normal thermal conductivity of about 1400W/(m.K), and the tensile strength of about 1800 MPa, which is improved by about 3 times compared with the tensile strength of diamond.
Claims (8)
1. A diamond carbon fiber composite material is characterized in that: the self-supporting diamond diaphragm is formed by overlapping self-supporting diamond diaphragms and carbon fiber layers which are sequentially and alternately arranged in an up-down direction, and the top layer and the bottom layer of the self-supporting diamond diaphragm are self-supporting diamond diaphragms; the carbon fiber layer is a carbon fiber-cured binder complex, and the structure of the complex is a carbon fiber reinforced cured binder.
2. A diamond carbon fiber composite material is characterized in that: the self-supporting diamond diaphragm is formed by overlapping self-supporting diamond diaphragms and carbon fiber layers which are sequentially and alternately arranged in an up-down direction, and the top layer and the bottom layer of the self-supporting diamond diaphragm are self-supporting diamond diaphragms; the carbon fiber layer is a carbon fiber-diamond micro powder-curing binder complex, the structure of the complex is a carbon fiber reinforced curing binder, and the diamond micro powder is dispersed in the complex.
3. A diamond carbon fibre composite material according to claim 1 or 2 wherein: the self-supporting diamond diaphragm is prepared by adopting a CVD method, the thermal conductivity is more than or equal to 600W/(m.K), the flatness is less than or equal to 0.1mm, the parallelism is less than or equal to 0.1mm, and the roughness Ra is less than or equal to 0.05 mm; the thickness of the self-supporting diamond diaphragm is 0.3 mm-1 mm, and the thickness of the carbon fiber layer is 0.1 mm-0.3 mm.
4. A diamond carbon fibre composite material according to claim 2 wherein: the curing binder is a cured body of barium phenolic resin, epoxy resin and modified epoxy resin; the grain size of the diamond micro powder is 100 nm-10 mu m;
the preparation method of the diamond carbon fiber composite material according to claim 1, which is characterized by comprising the following steps:
step 1: selecting a self-supporting diamond film with proper diameter and thickness according to the size requirement of the diamond carbon fiber composite material on the self-supporting diamond film, cutting the self-supporting diamond film into a set shape by adopting a laser cutting machine, and then performing thickness trimming and surface smoothing treatment on the self-supporting diamond film obtained by cutting by adopting a laser trimming machine to obtain the self-supporting diamond film meeting the composite requirement;
step 2: uniformly blending a binder and absolute ethyl alcohol, soaking carbon fibers in a blending solution for 1-5 minutes, taking out the carbon fibers, placing the carbon fibers in the air for 10-30 minutes, then flatly paving and bonding the carbon fibers soaked with the binder on a self-supporting diamond membrane, placing a layer of self-supporting diamond membrane on a carbon fiber layer, and repeating the process of alternately flatly paving the carbon fibers soaked with the binder and the self-supporting diamond membrane until the composite thickness meets the requirement to obtain a composite layer structure;
and step 3: clamping the side face of the composite layer structure after the composite through a clamping frame to ensure the flatness of the composite layer structure, meanwhile, placing a heavy object on the surface of the top layer self-supporting diamond membrane, discharging surplus adhesive in the carbon fiber layer and bubbles dispersed in the adhesive by virtue of normal static pressure of the heavy object, and then heating and curing the adhesive under the condition of keeping the side face clamping and the top layer applying pressure;
and 4, step 4: and removing the heavy object and the clamping frame, polishing and ultrasonically cleaning the side surface of the composite layer structure, and finally obtaining the diamond carbon fiber composite material.
5. The method for preparing a diamond carbon fiber composite material according to claim 5, wherein: in the step 2, the binder is barium phenolic resin, epoxy resin or modified epoxy resin, and the mixing ratio of the binder to absolute ethyl alcohol is 1: 1-1: 5; in the step 3, the heating temperature for heating and curing is 200-300 ℃, and the temperature is kept for 3-8 hours.
6. The method for preparing the diamond carbon fiber composite material according to claim 2, which is characterized by comprising the following steps:
step 1: selecting a self-supporting diamond film with proper diameter and thickness according to the size requirement of the diamond carbon fiber composite material on the self-supporting diamond film, cutting the self-supporting diamond film into a set shape by adopting a laser cutting machine, and then performing thickness trimming and surface smoothing treatment on the self-supporting diamond film by adopting a laser trimming machine to obtain the self-supporting diamond film meeting the composite requirement;
and 2, step: proportionally mixing the diamond micro powder, the curing binder and the absolute ethyl alcohol, and uniformly dispersing the diamond micro powder by adopting a stirrer;
and 3, step 3: soaking carbon fiber tows in a binder formulation containing diamond micro powder, taking out the carbon fibers, flatly paving and bonding the carbon fibers on a self-supporting diamond membrane, placing a layer of self-supporting diamond membrane on the carbon fiber layer, and repeating the process of alternately flatly paving the carbon fibers soaked with the binder and the self-supporting diamond membrane until the composite thickness meets the requirement to obtain a composite layer structure;
and 4, step 4: clamping the side face of the composite layer structure after the composite through a clamping frame to keep the flatness of the composite layer structure, meanwhile, placing a heavy object on the surface of the top layer self-supporting diamond membrane, discharging surplus adhesive in the carbon fiber layer and bubbles dispersed in the adhesive by virtue of normal static pressure of the heavy object, and then heating and curing the adhesive under the condition of keeping the side face clamping and the top layer applying pressure;
and 5: and removing the heavy object and the clamping frame, polishing and ultrasonically cleaning the side surface of the composite layer structure, and finally obtaining the diamond carbon fiber composite material.
7. The method for preparing a diamond carbon fiber composite material according to claim 7, wherein: in the step 2, when the diamond micro powder, the curing binder and the absolute ethyl alcohol are prepared, the ratio of the diamond micro powder to the curing binder is 1: 1-1: 5, and the ratio of the whole diamond micro powder to the curing binder to the absolute ethyl alcohol is 1: 2-1: 10; in the step 4, the heating temperature of heating and curing is 200-300 ℃, and the temperature is kept for 3-8 hours.
8. The method for producing a diamond carbon fiber composite material according to claim 5 or 7, wherein: the clamping frame is made of loose materials or through holes for discharging the binder are processed on the clamping frame.
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