CN108658596B - Graphite plate and manufacturing method thereof - Google Patents
Graphite plate and manufacturing method thereof Download PDFInfo
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- CN108658596B CN108658596B CN201810401836.0A CN201810401836A CN108658596B CN 108658596 B CN108658596 B CN 108658596B CN 201810401836 A CN201810401836 A CN 201810401836A CN 108658596 B CN108658596 B CN 108658596B
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- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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Abstract
The invention belongs to the field of powder metallurgy. Discloses a graphite plate and a manufacturing method thereof, which are prepared from the following raw materials in percentage by weight: the method comprises the following steps of using 80-92% of recrystallized graphite mixed asphalt coke powder, using a forming agent, using ferroalloy powder and recrystallized graphite mixed asphalt coke powder, wherein the grain size range of the recrystallized graphite mixed asphalt coke powder is 1-10 microns, enabling the recrystallized graphite mixed asphalt coke, the medium-temperature asphalt powder, the forming agent and the ferroalloy powder to react with each other at high temperature and high pressure, and enabling the added medium-temperature asphalt powder and the ferroalloy powder to play roles of a binder and a catalyst, so that the overall strength of the graphite plate can be improved, and the physical and chemical performance indexes of the graphite plate can meet the requirements of different fields.
Description
[ technical field ] A method for producing a semiconductor device
The invention belongs to the field of powder metallurgy, and particularly relates to a graphite plate and a manufacturing method thereof.
[ background of the invention ]
Graphite has excellent performances of high temperature resistance, electric conduction, good heat conduction performance, good lubricating performance, strong plasticity and good thermal shock resistance due to the special structure, and the graphite has wide application in industry and can be used in almost every industry.
Because graphite is often processed into graphite plates due to its excellent properties, the graphite plates are widely applied to various fields such as electronics, metallurgy, electroplating, chemical engineering, steel and environmental protection sewage treatment, but because the traditional graphite production needs to be subjected to a multi-dipping and baking process, the manufacturing process is complex, the production period is as high as 6 months generally, the production cost is high, and the environmental pollution in the production process is serious. The physical and chemical properties of graphite plates made of artificial graphite cannot meet the requirements of different fields.
In view of the above, it is necessary to provide a graphite sheet with better physical and chemical properties and a manufacturing method thereof.
[ summary of the invention ]
In order to solve the technical problems, embodiments of the present invention provide a graphite sheet with better physical and chemical properties and a manufacturing method thereof.
In order to solve the above technical problems, embodiments of the present invention provide the following technical solutions:
in a first aspect, an embodiment of the present invention provides a graphite plate, which is prepared from the following raw materials in percentage by weight: the composite material comprises medium-temperature asphalt powder, a forming agent, ferroalloy powder and recrystallized graphite mixed asphalt coke powder, wherein the percentage of the recrystallized graphite mixed asphalt coke powder is 80-92%, and the particle size range of the recrystallized graphite mixed asphalt coke powder is 1-10 microns.
Preferably, the percentage of the recrystallized graphite mixed asphalt coke powder is 85% -90%.
Preferably, the grain size of the recrystallized graphite mixed asphalt coke powder is 1 micron, and the weight ratio of the high-purity iron alloy powder to the medium-temperature asphalt powder is 1: 20.
Preferably, the grain size of the recrystallized graphite mixed asphalt coke powder is 1 micron, and the weight ratio of the high-purity iron alloy powder to the medium-temperature asphalt powder is 3: 8.
Preferably, the grain size of the recrystallized graphite mixed asphalt coke powder is 3 microns, and the weight ratio of the high-purity iron alloy powder to the medium-temperature asphalt powder is 1: 10.
Preferably, the grain size of the recrystallized graphite mixed asphalt coke powder is 3 microns, and the weight ratio of the high-purity iron alloy powder to the medium-temperature asphalt powder is 1: 20.
Preferably, the granularity of the recrystallized graphite mixed asphalt coke powder is 5 microns, and the weight ratio of the high-purity iron alloy powder to the medium-temperature asphalt powder is 1: 3.
Preferably, the granularity of the recrystallized graphite mixed asphalt coke powder is 10 microns, and the weight ratio of the high-purity iron alloy powder to the medium-temperature asphalt powder is 1: 4.
In a second aspect, an embodiment of the present invention provides a method for manufacturing a graphite plate, including: fully mixing the asphalt powder, the forming agent, the ferroalloy powder and the recrystallized graphite mixed asphalt coke powder, pressing the mixture into a column shape in a die by using a four-column press, filling the column shape into the composite pyrophyllite after dewaxing, heating, boosting and sintering by using a cubic press, and taking out the powder after pressure relief.
Preferably, the temperature and pressure increasing sintering comprises: firstly, increasing the pressure of the pressure line to 60Mpa for 1-2 minutes, maintaining the pressure for 1-3 minutes, then starting heating, increasing the power of the heater to 10 kilowatts, preserving the heat for 2-30 minutes, then slowly increasing the power to 18 kilowatts for 2-25 minutes, keeping the temperature for 5-35 minutes, stopping heating, recovering the power line to 0, then releasing the pressure after 5-10 minutes, recovering the pressure line to 0, and the whole sintering process is calculated according to the heating time for 9-90 minutes.
The embodiment of the invention has the beneficial effects that: different from the situation of the prior art, the raw materials for preparing the graphite plate in the embodiment of the invention comprise medium-temperature asphalt powder, a forming agent, iron alloy powder and recrystallized graphite mixed asphalt coke powder, the recrystallized graphite mixed asphalt coke, the medium-temperature asphalt powder, the forming agent and the iron alloy powder are mutually reacted under high temperature and high pressure, the added medium-temperature asphalt powder and the iron alloy powder play roles of a binder and a catalyst, the overall strength of the graphite plate can be improved, and the physical and chemical performance indexes of the graphite plate can meet the requirements of different fields.
[ description of the drawings ]
Fig. 1 is a process diagram of sintering under elevated temperature and pressure in the method for manufacturing graphite plates according to the embodiment of the present invention.
[ detailed description ] embodiments
In order to make the objects, methods, schemes and advantages of the present invention more apparent, the present invention will be described in detail with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The carbon material used in the invention is the recrystallized graphite mixed asphalt coke, the bending strength of the recrystallized graphite mixed asphalt coke is more than 70Mpa, the compressive strength is more than 100Mpa, the Shore hardness is 60-80, and the thermal expansion coefficient is 4.47EX10-6/° C, the thermal conductivity is 100W/m. The physical and chemical properties of the prepared graphite plate are superior to those of the traditional artificial graphite (three-dipping four-baking). The production period is shortened to a few days from about 6 months, the environmental pollution and the time cost are greatly reduced, and the economic benefit is obvious.
The embodiment of the invention provides a graphite plate which is prepared from the following raw materials: medium-temperature asphalt powder, a forming agent, ferroalloy powder and recrystallized graphite mixed asphalt coke.
The raw materials described below are all used in percentages by weight.
The asphalt powder is formed by the chemical treatment of sulfonation, emulsification and the like on asphalt substances, is an anionic high polymer, has a molecular structure of carbon-carbon bonds and carbon-sulfur bonds, and has stronger bond energy, so the temperature resistance is higher; the asphalt powder is divided into low-temperature asphalt powder, medium-temperature asphalt powder and high-temperature asphalt powder, the medium-temperature asphalt powder is adopted in the embodiment of the invention, the purity of the medium-temperature asphalt powder is 98%, the medium-temperature asphalt powder is used as a binder in the manufacturing process of the graphite plate, and the medium-temperature asphalt powder is 80-100 meshes.
Optionally, the amount of the medium-temperature asphalt powder is 2-10%, preferably 4-7%, and the amount of asphalt in the conventional method for manufacturing graphite plates is usually more than 25%, so that the energy consumption of high-temperature graphitization is avoided.
The ferroalloy powder is an intermediate alloy consisting of iron and one or more elements, is mainly used for steel smelting, and can also be used as a deoxidizer and a catalyst, the purity of the ferroalloy powder in the embodiment of the invention is 99%, and the particle size range of the ferroalloy powder is 10-50 microns; wherein, the dosage of the ferroalloy powder is 0.1 to 3 percent, and the dosage of the ferroalloy powder is preferably 0.2 to 2 percent.
The recrystallized graphite mixed asphalt coke is used as a raw material for manufacturing graphite plates, the particle size range of the recrystallized graphite mixed asphalt coke powder is 1-10 microns, and the preferred particle size range of the recrystallized graphite mixed asphalt coke powder is 1-3 microns.
Adding recrystallized graphite mixed asphalt coke powder with different granularities into asphalt powder and iron alloy powder according to a certain weight ratio, wherein the recrystallized graphite mixed asphalt coke accounts for the total weight of raw materials used for manufacturing the graphite plate and comprises the following components in percentage by weight: 80-92 percent of the total weight of the graphite-graphite mixed asphalt coke powder, wherein the percentage of the recrystallized graphite mixed asphalt coke powder is preferably 85-90 percent.
The forming agent can be one or more of polyethylene, paraffin, phenolic resin, stearic acid and water; wherein, the dosage of the forming agent is 3-10 percent, and the dosage of the forming agent is preferably 4-7 percent.
The embodiment of the invention also provides a manufacturing method of the graphite plate, which comprises the following steps: and fully mixing the medium-temperature asphalt powder, the forming agent, the ferroalloy powder and the recrystallized graphite mixed asphalt coke powder, pressing the mixture into blocks in a die by using a four-column press, and taking out the carbon test block after pressure relief to obtain the graphite plate disclosed by the embodiment of the invention.
The cubic press is a 6X 3000T press produced by Shaoguangsu super hard material science and technology Limited.
The graphite plate of the embodiment of the invention is manufactured by hot pressing sintering of a cubic press, and the performance of the graphite plate is superior to that of the traditional artificial graphite (three-dipping four-baking).
In this embodiment, the sintering under elevated temperature and pressure includes: firstly, increasing the pressure of a pressure line to 60Mpa for 1-5 minutes, maintaining the pressure for 1-3 minutes, then starting heating, increasing the power of a heater to 10 kilowatts, keeping the temperature for 2-30 minutes, then slowly increasing the power to 18 kilowatts for 2-25 minutes, keeping the temperature for 5-35 minutes, stopping heating, recovering the power line to 0, and calculating the total sintering process according to the heating time for 9-90 minutes. And then the pressure is released after 5 to 10 minutes, the pressure line is restored to 0, the carbon test block is taken out after the pressure is released, the carbon test block is placed in an electric furnace and heated to 1600-2200 ℃ for tempering treatment, and the density of the test block is 1.70g/cm2The bending strength is not lower than 60Mpa, and the compressive strength is not lower than 90 Mpa; the Shore hardness is more than 65, and the coefficient of thermal expansion is 4.34EX10-6/° C, the thermal conductivity is 100W/m. Examples of the present invention are illustrated below by way of specific examples and comparative examples.
The graphite plate with better performance can not be manufactured by adopting the four raw materials through the conventional process, the particle size of the raw material powder for manufacturing the graphite plate by using the conventional process is not higher than 400 meshes, and the hot pressing process in the embodiment can be used for manufacturing the graphite plate by adopting the raw materials with more than 800 meshes.
Example 1
Weighing 4000 g of 1 micron recrystallized graphite mixed asphalt coke powder; weighing 200 g of 80-mesh medium-temperature asphalt powder (purity 98.0%); weighing 300 g of forming agent; weighing 10 g of 10-micron high-purity ferroalloy powder (99.0%); the four materials are fully mixed, pressed into blocks in a die by a four-column press, degummed at 600 ℃, then put into 3000 tons of compound pyrophyllite specially made by a double-sided pressure full-automatic hot press, hot-pressed and sintered by the 3000 tons of double-sided pressure full-automatic hot press, and hot-pressed and sintered according to the method shown in figure 1, wherein the abscissa is time, and the ordinate is pressure and heating power, which are all represented qualitatively. Firstly, increasing the pressure of a pressure line to 60Mpa for 1 minute, maintaining the pressure for 2 minutes, then starting heating, increasing the power of a heater to 10 kilowatts, keeping the temperature for 10 minutes, then slowly increasing the power to 18 kilowatts for 5 minutes, keeping the temperature for 15 minutes, stopping heating, recovering the power line to 0, then releasing the pressure after 5 minutes, recovering the pressure line to 0, and calculating the whole sintering process according to the heating time for 30 minutes. And taking out the carbon test block after pressure relief, and putting the carbon test block into an electric furnace to heat to 1800 ℃ for tempering treatment.
After cooling, the density of the test piece was measured to be 1.70g/cm2The bending strength is not lower than 60MPa, and the compressive strength is not lower than 90 MPa; the Shore hardness is more than 65, and the coefficient of thermal expansion is 4.45EX10-6/° C, the thermal conductivity is 100W/m.
Example 2
Weighing 4000 g of 3-micron recrystallized graphite mixed asphalt coke powder; weighing 200 g of 100-mesh medium-temperature asphalt powder (purity 98.0%); weighing 300 g of forming agent; weighing 20 g of 50-micron high-purity ferroalloy powder (99.0%); the four materials are fully mixed, pressed into blocks in a die by a four-column press, degummed at 600 ℃, then filled into the specially-made composite pyrophyllite of a 3000-ton double-sided full-automatic hot press, and hot-pressed and sintered by the 3000-ton double-sided full-automatic hot press, and the process is the same as that of the example 1. And (4) taking out the carbon test block after pressure relief, and putting the carbon test block into an electric furnace to heat to 2000 ℃ for tempering treatment.
After cooling, the density of the test piece was measured to be 1.71g/cm2The bending strength is not lower than 60MPa, and the compressive strength is not lower than 90 MPa; the Shore hardness is more than 60, and the coefficient of thermal expansion is 4.36EX10-6/° C, the thermal conductivity is 100W/m.
Example 3
10000 g of 1 micron recrystallized graphite mixed asphalt coke powder is weighed; weighing 800 g of 80-mesh medium-temperature asphalt powder (purity 98.0%); weighing 600 g of forming agent; weighing 30 g of 10-micron high-purity ferroalloy powder (99.0%); the four materials are fully mixed, pressed into blocks in a die by a four-column press, degummed at 800 ℃, then loaded into the specially-made composite pyrophyllite of a 3000-ton double-sided full-automatic hot press, and hot-pressed and sintered by the 3000-ton double-sided full-automatic hot press, the process is the same as the example 1, the difference is that the whole sintering process is 60 minutes, the carbon test block is taken out after pressure relief, and the carbon test block is placed in an electric furnace to be heated to 2100 ℃ for tempering treatment.
After cooling, the density of the test piece was measured to be 1.78g/cm2The bending strength is not lower than 60MPa, and the compressive strength is not lower than 90 MPa; the Shore hardness is more than 65, and the coefficient of thermal expansion is 4.36EX10-6/° C, the thermal conductivity is 100W/m.
Example 4
10000 g of 3 micron recrystallized graphite mixed asphalt coke powder is weighed; weighing 600 g of 100-mesh medium-temperature asphalt powder (purity 98.0%); weighing 600 g of forming agent; weighing 30 g of 50-micron high-purity ferroalloy powder (99.0%); the four materials are fully mixed, pressed into blocks in a die by a four-column press, degummed at 800 ℃, then loaded into the specially-made composite pyrophyllite of a 3000-ton double-sided full-automatic hot press, and hot-pressed and sintered by the 3000-ton double-sided full-automatic hot press, the process is the same as the example 1, the difference is that the whole sintering process is 60 minutes, the carbon test block is taken out after pressure relief, and the carbon test block is placed in an electric furnace to be heated to 2200 ℃ for tempering treatment.
After cooling, the test piece density was 1.75g/cm2The bending strength is not lower than 60MPa, and the compressive strength is not lower than 90 MPa; the Shore hardness is more than 65, and the coefficient of thermal expansion is 4.35EX10-6/° C, the thermal conductivity is 100W/m.
Example 5
Weighing 1000 g of 5-micron recrystallized graphite mixed asphalt coke powder; weighing 60 g of 80-mesh medium-temperature asphalt powder (purity 98.0%); weighing 50 g of forming agent; weighing 20 g of 10-micron high-purity ferroalloy powder (99.0%); the four materials are fully mixed, pressed into blocks in a die by a four-column press, degummed at 600 ℃, then put into the specially-made composite pyrophyllite of a 3000-ton double-sided full-automatic hot press, and hot-pressed and sintered by the 3000-ton double-sided full-automatic hot press, the process is the same as the example 1, except that the whole sintering process is 10 minutes, the carbon test block is taken out after pressure relief, and the carbon test block is placed in an electric furnace to be heated to 2200 ℃ for tempering treatment.
After cooling, the density of the test block was measured to be 1.83g/cm2The bending strength is not lower than 80MPa, and the compressive strength is not lower than 100 MPa; the Shore hardness is more than 70, and the coefficient of thermal expansion is 4.48EX10-6/° C, the thermal conductivity is 100W/m.
Example 6
Weighing 1000 g of 10-micron recrystallized graphite mixed asphalt coke powder; weighing 80g of 100-mesh medium-temperature asphalt powder (purity 98.0%); weighing 50 g of forming agent; weighing 20 g of 50-micron high-purity ferroalloy powder (99.0%); the four materials are fully mixed, pressed into blocks in a die by a four-column press, degummed at 600 ℃, then loaded into the specially-made composite pyrophyllite of a 3000-ton double-sided full-automatic hot press, and the hot-pressing sintering process is carried out by adopting the 3000-ton double-sided full-automatic hot press as in example 1, except that the whole sintering process is 10 minutes, the carbon test block is taken out after pressure relief, and the carbon test block is placed in an electric furnace to be heated to 2200 ℃ for tempering treatment.
After cooling, the density of the test piece was measured to be 1.85g/cm2The bending strength is not lower than 80MPa, and the compressive strength is not lower than 100 MPa; the Shore hardness is more than 70, and the coefficient of thermal expansion is 4.47EX10-6/° C, the thermal conductivity is 100W/m.
Comparative example 1
Weighing 4000 g of 1 micron artificial graphite powder; weighing 200 g of 80-mesh medium-temperature asphalt powder (purity 98.0%); weighing 300 g of forming agent; weighing 10 g of 10-micron high-purity ferroalloy powder (99.0%); the four materials were mixed thoroughly and hot pressed and sintered by a cubic press, the procedure was the same as in example 1.
Taking out the carbon test block after pressure relief, and testing the density of the test block to be 1.84g/cm2The bending strength is lower than 50MPa, and the compressive strength is lower than 60 MPa; the Shore hardness is less than 50, the coefficient of thermal expansion is not measurable, and the thermal conductivity is not measurable.
Comparative example 2
Weighing 4000 g of 3-micron artificial graphite powder; weighing 200 g of 100-mesh asphalt; weighing 300 g of forming agent; weighing 20 g of 50-micron high-purity ferroalloy powder (99.0%); the four materials were mixed thoroughly and hot pressed and sintered by a cubic press, the procedure was the same as in example 1.
Taking out the carbon material after pressure relief, and testing the density of the test block to be 1.80g/cm2The bending strength is lower than 50MPa, and the compressive strength is lower than 60 MPa; the Shore hardness is less than 50, the coefficient of thermal expansion is not measurable, and the thermal conductivity is not measurable.
In addition, the production cost and the production period of the graphite plate prepared by adopting the artificial graphite are both higher than those of the examples 1-6, and the pollution of the graphite plate prepared by adopting the artificial graphite to the environment is also obviously higher than that of the examples 1-6.
According to the embodiment, the physical and chemical properties of the graphite plate can be obviously improved by adding the recrystallized graphite mixed asphalt coke in the preparation process of the graphite plate, the recrystallized graphite mixed asphalt coke, the medium-temperature asphalt powder, the forming agent and the iron alloy powder react with each other at high temperature and high pressure, the added medium-temperature asphalt powder and the iron alloy powder play roles of a binder and a catalyst, the overall strength of the graphite plate can be improved, and the physical and chemical performance indexes of the graphite plate can meet the requirements of different fields.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (9)
1. A method for manufacturing a graphite plate is characterized by comprising the following steps of: fully mixing the medium-temperature asphalt powder, the forming agent, the high-purity ferroalloy powder and the recrystallized graphite mixed asphalt coke powder, pressing the mixture into a column shape in a die by using a four-column press, filling the column shape into composite pyrophyllite after dewaxing, heating, boosting and sintering by using a cubic press, and taking out the mixture after pressure relief;
wherein the using amount of the recrystallized graphite mixed asphalt coke powder is 80-92%, the granularity range of the recrystallized graphite mixed asphalt coke powder is 1-10 microns, and the using amount of the medium-temperature asphalt powder is 2-10%;
the heating and pressurizing sintering comprises the following steps: firstly, increasing the pressure line to 60Mpa for 1-5 minutes, maintaining the pressure for 1-3 minutes, then starting heating, increasing the power of a heater to 10 kilowatts, preserving the heat for 2-30 minutes, then slowly increasing the power to 18 kilowatts for 2-25 minutes, keeping the temperature for 5-35 minutes, stopping heating, recovering the power line to 0, then releasing the pressure after 5-10 minutes, recovering the pressure line to 0, and calculating the whole sintering process according to the heating time for 9-90 minutes.
2. A graphite sheet produced by the method for producing a graphite sheet according to claim 1.
3. The graphite sheet according to claim 2, wherein the amount of the recrystallized graphite mixed with the pitch coke powder is 85% to 90%.
4. The graphite plate according to claim 2, wherein the recrystallized graphite mixed asphalt coke powder has a particle size of 2 μm, and the weight ratio of the high-purity ferrous alloy powder to the medium-temperature asphalt powder is 1: 20.
5. The graphite plate according to claim 2, wherein the recrystallized graphite mixed asphalt coke powder has a particle size of 2 μm, and the weight ratio of the high-purity ferrous alloy powder to the medium-temperature asphalt powder is 3: 8.
6. The graphite plate according to claim 2, wherein the recrystallized graphite mixed asphalt coke powder has a particle size of 3 μm, and the weight ratio of the high-purity ferrous alloy powder to the medium-temperature asphalt powder is 1: 10.
7. The graphite plate according to claim 2, wherein the recrystallized graphite mixed asphalt coke powder has a particle size of 3 μm, and the weight ratio of the high-purity ferrous alloy powder to the medium-temperature asphalt powder is 1: 20.
8. The graphite plate according to claim 2, wherein the recrystallized graphite mixed asphalt coke powder has a particle size of 5 μm, and the weight ratio of the high-purity ferrous alloy powder to the medium-temperature asphalt powder is 1: 3.
9. The graphite sheet according to claim 2, wherein the recrystallized graphite mixed asphalt coke powder has a particle size of 10 μm, and the weight ratio of the high-purity iron alloy powder to the medium-temperature asphalt powder is 1: 4.
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| CN201810401836.0A CN108658596B (en) | 2018-04-28 | 2018-04-28 | Graphite plate and manufacturing method thereof |
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| CN201810401836.0A CN108658596B (en) | 2018-04-28 | 2018-04-28 | Graphite plate and manufacturing method thereof |
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| CN116425545A (en) * | 2023-03-20 | 2023-07-14 | 国家高速列车青岛技术创新中心 | Carbon sliding plate material without binder and preparation method thereof |
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