CN115140729A - Preparation method of high-purity carbon material - Google Patents
Preparation method of high-purity carbon material Download PDFInfo
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- CN115140729A CN115140729A CN202210843645.6A CN202210843645A CN115140729A CN 115140729 A CN115140729 A CN 115140729A CN 202210843645 A CN202210843645 A CN 202210843645A CN 115140729 A CN115140729 A CN 115140729A
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Abstract
The invention discloses a preparation method of a high-purity carbon material, which adopts vacuum induction furnace equipment to carry out high-temperature chemical purification on the carbon material, adopts the process sequence of high-temperature purification firstly and high-temperature chemical purification secondly, can remove most impurities after the high-temperature purification in the early stage, can achieve the high purity of 5N grade, can greatly reduce the consumption of purified gas in the subsequent high-temperature chemical purification process, and adopts multiple vacuum-normal pressure oscillation in the high-temperature chemical purification process, thereby being beneficial to improving the purification effect, improving the utilization rate of the purified gas, reducing the consumption of the purified gas and reducing the discharge amount of harmful gas; and multiple vacuum-micro positive pressure circulation is adopted, so that the impurities of chlorine and fluorine in the purified gas can be removed.
Description
Technical Field
The invention relates to the field of carbon material preparation, and particularly relates to a preparation method of a high-purity carbon material.
Background
The carbon material has multiple excellent characteristics of corrosion resistance, radiation protection, heat conduction, electric conduction, high temperature resistance, self-lubrication and the like, and is widely applied to multiple fields. The carbon material can be used for preparing carbon material alkene, and the carbon material can drive the technical revolution in the fields of new energy, new materials and the like. The purity of the carbon material determines its use value, and the higher the purity, the greater its use value.
The high-purity carbon material means that the carbon content of the carbon material is more than 99.99 percent, and the high-purity carbon material product has the characteristics of high strength, high density, high purity, high chemical stability, compact and uniform structure, high temperature resistance, high conductivity, good wear resistance, self-lubrication and the like; the high-purity light carbon material has the characteristics of good thermal insulation performance, high temperature resistance, corrosion resistance and the like. Both of them can be widely used in the field of thermal field materials in thermal equipment such as semiconductor single crystal furnaces, epitaxial furnaces and the like. At present, the high-purity carbon material purified by the existing purification technology can not fully meet the requirements of the semiconductor furnace thermal field material in the aspects of purity and stability.
The Chinese patent with publication number CN105347337B discloses a method for purifying natural graphite by using Freon at high temperature, which comprises the following steps: loading natural graphite powder into a high-temperature graphite purification furnace; vacuumizing the high-temperature graphite purifying furnace until the pressure is 100Pa or below; filling protective gas into the high-temperature graphite purification furnace, wherein the pressure is 100-1000 Pa higher than atmospheric pressure; heating a high-temperature graphite purification furnace to 1600-3000 ℃ at a heating rate of 4-20 ℃/min; introducing Freon gas, and keeping the time for 20-120 min; and after keeping, stopping introducing the Freon gas, cooling the high-temperature graphite purification furnace at the cooling rate of 4-20 ℃/min, and cooling to room temperature to obtain the purified graphite powder. The technical scheme can only obtain high-purity graphite powder with the purity of 90.0-99.99 percent by purifying the natural graphite at high temperature by using Freon, and the high-end requirement of the existing industrial production is difficult to meet.
Disclosure of Invention
The invention aims to provide a preparation method of a high-purity carbon material, aiming at the defects in the prior art, the purification effect is improved through high-temperature purification, the purity of the carbon material can be improved to 6N grade, and the purification problem of the high-purity carbon material is effectively solved.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a high-purity carbon material adopts vacuum induction furnace equipment to carry out high-temperature chemical purification on the carbon material, and comprises the following steps:
s1, placing the carbon material in a vacuum induction furnace, closing a furnace cover, vacuumizing, and then inputting inert gas into the furnace to enable the pressure in the furnace to rise and keep at 600-900 torr;
s2, starting a heating power supply, raising the temperature of a working area of the induction furnace to 2200-3200 ℃, keeping the pressure in the induction furnace at 760-900 torr, preserving heat, and performing high-temperature purification and graphitization treatment on the material;
s3, when the heat preservation time is up, closing the heating power supply, reducing the furnace temperature to 2800-2200 ℃, closing the inert gas, vacuumizing again and keeping the vacuum degree for 5-30 minutes, and then adding working gas to increase the pressure in the furnace and keep the pressure at 600-900 torr;
s4, starting a heating power supply, raising the temperature of the furnace to 2200-3000 ℃, preserving the temperature, and carrying out high-temperature chemical purification on the materials;
s5, closing a heating power supply, reducing the furnace temperature to 2800-2000 ℃, closing working gas, vacuumizing the furnace body and keeping the vacuum degree, adding inert gas, increasing the furnace pressure and keeping the furnace pressure at 600-900 torr, detecting the content of impurity elements in the gas discharged by the vacuum induction furnace, starting a vacuum pump again and closing the inert gas if the content of the impurity elements exceeds the standard, increasing the furnace vacuum degree to 0.01-10 torr and keeping the vacuum degree, adding the inert gas again, increasing the furnace pressure and keeping the furnace pressure at 600-900 torr, detecting the content of the impurity elements in the gas in the furnace again, repeating the steps until the content of the impurity elements in the gas in the furnace is less than a process value, keeping the vacuum degree, waiting for the furnace temperature to decrease, adding protective gas to increase the furnace pressure to 760 torr after the furnace temperature decreases to 100 ℃, opening a furnace cover and taking out materials to obtain the high-purity carbon material.
Further, the carbon material comprises graphite and graphite products, carbon and carbon products, powdered graphite, graphene, carbon nanotubes, carbon nanosheets, carbon fibers and carbon fiber products, and carbon-carbon composite materials.
Further, the working gas is a purified gas or a mixed gas of the purified gas and an inert gas, and the purified gas is a chlorine-containing gas or/and a fluorine-containing gas, and comprises chlorine, freon, carbon tetrachloride and a combination thereof.
Further, the inert gas includes argon or helium.
Further, the shielding gas comprises argon or nitrogen.
Further, the vacuum induction furnace comprises a vertical vacuum induction furnace and a horizontal vacuum induction furnace.
Preferably, the vacuum induction furnace is a vertical vacuum induction furnace.
Further, steps S3 and S4 may be looped several times.
Further, in the circulation process, the furnace temperature, the heat preservation time and the vacuum degree are respectively adjustable.
Further, the vacuum degree of the vacuum induction furnace after vacuum pumping treatment is 0.01-10 torr.
Compared with the prior art, the invention has the following beneficial effects:
1. the vertical vacuum induction furnace is adopted to obtain high temperature of more than 3000 ℃, which is beneficial to improving the purification effect.
2. The process sequence of high-temperature purification and high-temperature chemical purification is adopted, most impurities can be removed after the early high-temperature purification, the material can reach 5N-grade high purity, and the purified gas consumption in the subsequent high-temperature chemical purification process can be greatly reduced.
3. In the high-temperature chemical purification process, multiple vacuum-normal pressure oscillations are adopted, which is beneficial to improving the purification effect, improving the utilization rate of the purified gas, reducing the consumption of the purified gas and reducing the discharge of harmful gas.
4. After purified gas is introduced, multiple vacuum-micro positive pressure circulation is adopted in a high-temperature environment, so that the impurities of chlorine and fluorine in the purified gas can be removed, the purity of the carbon material can be improved to 6N grade, and the problem of purification of the high-purity carbon material is effectively solved.
Drawings
Fig. 1 is a schematic structural view of a material holder in embodiment 1;
FIG. 2 is a schematic view showing the structure of a crucible in example 2;
FIG. 3 is a schematic view of the structure of the graphite felt of example 3;
wherein 11 is a tray, 21 is a crucible, 22 is powder graphite, 31 is a graphite sleeve, and 32 is a graphite felt.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive step based on the embodiments of the present invention, are within the scope of protection of the present invention.
Example 1
As shown in fig. 1, the present embodiment provides a method for manufacturing a graphite tray for epitaxial wafers of semiconductor wafers, which uses isostatic pressing graphite as a material, and includes the following steps:
s1, placing a tray 11 on material racks uniformly arranged up and down, placing the material racks and the tray in a vacuum induction furnace, closing a furnace cover, starting a vacuum pump to raise the vacuum degree in the furnace to 0.02 torr, closing the vacuum pump, inputting argon into the furnace, and raising the pressure in the furnace to 750-800 torr;
s2, starting a heating power supply to enable the temperature of a working area of the induction furnace to reach 3200 ℃, keeping the pressure in the induction furnace at 750-800 torr, preserving the heat for 60 minutes, and carrying out high-temperature purification and graphitization treatment on the tray;
and S3, when the heat preservation time is up, closing the heating power supply, reducing the furnace temperature to 2600 ℃, closing the inert gas, starting the vacuum pump again, increasing the vacuum degree in the furnace to 0.01 torr, keeping the vacuum degree for 30 minutes, closing the vacuum pump, adding mixed gas of Freon 22 and argon, wherein the volume mixing ratio of Freon 22 to argon is 1:1, raising the pressure in the furnace to 780 torr;
s4, starting a heating power supply, keeping the furnace temperature at 3000 ℃ for 60 minutes, and performing high-temperature chemical purification on the material;
s5, repeating the steps S3 and S4 for two times, wherein the purity can be higher by repeating the steps for two times;
s6, turning off a heating power supply, reducing the furnace temperature to 2500 ℃, turning off working gas in the step S4, turning on a vacuum pump, increasing the vacuum degree in the furnace to 0.01 torr and keeping the vacuum degree for 10 minutes, turning off the vacuum pump, adding argon gas, increasing the pressure in the furnace and keeping the pressure at 780 torr, detecting the contents of chlorine and fluorine in the gas discharged by the vacuum induction furnace, turning on the vacuum pump again if the element content is not less than 1ppm, increasing the vacuum degree in the furnace to 0.01 torr and keeping the vacuum degree, adding inert gas again, increasing the pressure in the furnace and keeping the pressure at 800 torr, detecting the contents of chlorine and fluorine in the gas in the furnace again, repeatedly vacuumizing, adding argon gas, detecting the contents of chlorine and fluorine in the gas in the furnace until the contents of chlorine and fluorine in the gas in the furnace are less than 1ppm, keeping the vacuum degree at 0.01 torr, waiting for the reduction of the furnace temperature, adding protective gas nitrogen gas to increase the pressure in the furnace to 760 torr, opening a furnace cover, taking out the material, and obtaining a high-purity graphite tray with the carbon content of more than 99.9999%. Because absolute vacuum is difficult to reach, this embodiment makes argon gas produce "washing" effect through filling into argon gas repeatedly, goes out the gas replacement that contains fluorine, chlorine in the stove, finally reaches the material of high-purity.
The performance of the semiconductor is affected by the presence of sensitive impurities such as phosphorus, boron, aluminum, etc. in the tray. This embodiment adopts the high temperature purification of 3200 ℃ above, makes most impurity gasification, to a small amount of stubborn impurity, through the chemical purification under the 3000 ℃ condition, makes impurity and chlorine, fluorine take place chemical reaction. Because the high temperature of more than 3000 ℃ makes the impurity activity stronger, more fully reacts with chemical gas, and the purity that can reach is higher. The embodiment can lead the phosphorus, the boron and the aluminum to be less than 0.1ppm, and can even lead the boron and the aluminum to be less than 0.01ppm under the laboratory condition.
Example 2
As shown in fig. 2, this embodiment provides a method for preparing high purity carbon graphite powder, in which the raw material is natural graphite powder or artificial graphite powder, and the specific steps are as follows:
s1, placing powder graphite 22 in a crucible 21, then arranging the crucible 21 in a vacuum induction furnace up and down, closing a furnace cover, starting a vacuum pump to enable the vacuum degree in the furnace to rise to 0.1 torr, closing the vacuum pump, inputting argon into the furnace, and enabling the pressure in the furnace to rise and keep at 760 torr;
s2, starting a heating power supply to enable the temperature of a working area of the induction furnace to reach 3100 ℃, keeping the pressure in the induction furnace at 750-800 torr, keeping the temperature for 90 minutes, and performing high-temperature purification and graphitization treatment on the powder graphite;
and S3, when the heat preservation time is up, closing the heating power supply, reducing the furnace temperature to 2600 ℃, closing the inert gas, starting the vacuum pump again, increasing the vacuum degree in the furnace to 0.01 torr, keeping the vacuum degree for 30 minutes, closing the vacuum pump, adding mixed gas of chlorine, freon 22 and argon, wherein the volume mixing ratio of the chlorine, the Freon 22 and the argon is 1:1:1, raising the pressure in the furnace to 780 torr and keeping the pressure;
s4, starting a heating power supply, keeping the furnace temperature at 3000 ℃ for 60 minutes, and performing high-temperature chemical purification on the material;
s5, repeating the steps S3 and S4 for one time;
s6, turning off a heating power supply, reducing the furnace temperature to 2500 ℃, turning off working gas in the step S4, turning on a vacuum pump, increasing the vacuum degree in the furnace to 0.01 torr and keeping the vacuum degree for 30 minutes, turning off the vacuum pump, adding argon gas, increasing the pressure in the furnace to 780 torr, detecting the contents of chlorine and fluorine in the gas discharged from the vacuum induction furnace, turning on the vacuum pump again if the contents of the elements are not less than 0.5ppm, increasing the vacuum degree in the furnace to 0.01 torr and keeping the vacuum degree, adding inert gas again, increasing the pressure in the furnace to 800 torr, detecting the contents of chlorine and fluorine in the gas in the furnace again, repeatedly vacuumizing, adding argon gas, detecting the contents of chlorine and fluorine in the gas in the furnace until the contents of chlorine and fluorine in the gas in the furnace are less than 0.5ppm, keeping the vacuum degree at 0.01 torr, waiting for the furnace temperature reduction, adding protective gas to increase the pressure in the furnace to 760 torr after the furnace temperature is reduced to 100 ℃, opening a furnace cover, taking out the material 21, and obtaining high-purity graphite powder with the carbon content of more than 99.99 percent.
Example 3
As shown in fig. 3, this embodiment provides a method for preparing an adhesive-based graphite felt, which includes the following steps:
s1, winding a viscose-based graphite felt 32 on a graphite sleeve 31, then placing the sleeve wound with the graphite felt in a vacuum induction furnace, closing a furnace cover, starting a vacuum pump to raise the vacuum degree in the furnace to 0.01 torr, closing the vacuum pump, inputting argon into the furnace to raise the pressure in the furnace and keep the pressure at 760 torr;
s2, starting a heating power supply to enable the temperature of a working area of the induction furnace to reach 2800 ℃, keeping the pressure in the induction furnace at 750-800 torr, preserving the temperature for 90 minutes, and performing high-temperature purification and graphitization treatment on the viscose-based graphite felt;
and S3, when the heat preservation time is up, closing the heating power supply, reducing the furnace temperature to 2550 ℃, closing the inert gas, starting the vacuum pump again, increasing the vacuum degree in the furnace to 0.01 torr, keeping the vacuum degree for 30 minutes, closing the vacuum pump, adding mixed gas of chlorine, freon 22 and argon, wherein the volume mixing ratio of the chlorine, the Freon 22 and the argon is 1:1:1, raising the pressure in the furnace to 780 torr;
s4, starting a heating power supply to keep the furnace temperature at 2800 ℃ for 60 minutes, and performing high-temperature chemical purification on the viscose base graphite felt;
s5, repeating the steps S3 and S4 for two times;
s6, turning off a heating power supply, reducing the furnace temperature to 2500 ℃, turning off working gas in the step S4, turning on a vacuum pump, increasing the vacuum degree in the furnace to 0.01 torr and keeping the vacuum degree for 30 minutes, turning off the vacuum pump, adding argon gas, increasing the pressure in the furnace and keeping the pressure at 780 torr, detecting the contents of chlorine and fluorine in the gas discharged by the vacuum induction furnace, if the element content is not less than 0.5ppm, turning on the vacuum pump again, increasing the vacuum degree in the furnace to 0.01 torr and keeping the vacuum degree, adding inert gas again, increasing the pressure in the furnace and keeping the pressure at 800 torr, detecting the contents of chlorine and fluorine in the gas in the furnace again, repeatedly vacuumizing, adding argon gas, detecting the contents of chlorine and fluorine in the gas in the furnace until the contents of chlorine and fluorine in the gas in the furnace are less than 0.5ppm, keeping the vacuum degree at 0.01 torr, waiting for the reduction of the furnace temperature, and adding protective gas after the furnace temperature is reduced to 100 ℃, increasing the pressure in the furnace to 760 torr and taking out the material, thereby obtaining a high-purity graphite felt with the carbon content of more than 99.9995% carbon.
It should be noted that, if directional indications (such as upper, lower, left, right, front, rear, 8230; \8230;) are involved in the embodiment of the present invention, the directional indications are only used to explain the relative positional relationship between the components in a specific posture (as shown in the figure), the motion situation, etc., and if the specific posture is changed, the directional indications are correspondingly changed.
In addition, if there is a description of "first", "second", etc. in an embodiment of the present invention, the description of "first", "second", etc. is for descriptive purposes only and is not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In addition, technical solutions between the embodiments may be combined with each other, but must be based on the realization of the technical solutions by a person skilled in the art, and when the technical solutions are contradictory to each other or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention.
Claims (10)
1. A preparation method of a high-purity carbon material is characterized in that high-temperature chemical purification is carried out on the carbon material by adopting vacuum induction furnace equipment, and the preparation method comprises the following steps:
s1, placing the carbon material in a vacuum induction furnace, closing a furnace cover, vacuumizing, and then inputting inert gas into the furnace to increase the pressure in the furnace and keep the pressure at 600-900 torr;
s2, starting a heating power supply, raising the temperature of a working area of the induction furnace to 2200-3200 ℃, keeping the pressure in the induction furnace at 760-900 torr, preserving heat, and performing high-temperature purification and graphitization treatment on the material;
s3, when the heat preservation time is up, closing the heating power supply, reducing the furnace temperature to 2800-2200 ℃, closing the inert gas, vacuumizing again and keeping the vacuum degree for 5-30 minutes, and then adding working gas to increase the pressure in the furnace and keep the pressure at 600-900 torr;
s4, starting a heating power supply, raising the temperature of the furnace to 2200-3000 ℃, preserving the temperature, and carrying out high-temperature chemical purification on the materials;
s5, closing a heating power supply, reducing the furnace temperature to 2800-2000 ℃, closing working gas, vacuumizing the furnace body and keeping the vacuum degree, then adding inert gas, increasing the furnace pressure and keeping the furnace pressure at 600-900 torr, detecting the content of impurity elements in the gas discharged by the vacuum induction furnace, if the content of the impurity elements exceeds the standard, starting the vacuum pump again and closing the inert gas, increasing the furnace vacuum degree to 0.01-10 torr and keeping the vacuum degree, adding the inert gas again, increasing the furnace pressure and keeping the furnace pressure at 600-900 torr, detecting the content of the impurity elements in the gas in the furnace again, repeating the steps until the content of the impurity elements in the gas in the furnace is less than a process value, keeping the vacuum degree, waiting for the furnace temperature to decrease, adding protective gas to increase the furnace pressure to 760 torr after the furnace temperature decreases to 100 ℃, opening a furnace cover and taking out materials, thereby obtaining the high-purity carbon material.
2. The method for preparing a high-purity carbon material according to claim 1, wherein the carbon material comprises graphite and graphite products, carbon and carbon products, powdered graphite, graphene, carbon nanotubes, carbon nanosheets, carbon fibers and carbon fiber products, and carbon-carbon composites.
3. The method of claim 1, wherein the working gas is a purified gas or a mixture of a purified gas and an inert gas, and the purified gas is a chlorine-containing gas or/and a fluorine-containing gas, and comprises chlorine, freon, carbon tetrachloride and a combination thereof.
4. A method for producing a high purity carbon material as claimed in claim 3, wherein the inert gas comprises argon or helium.
5. The method for producing a high purity carbon material as claimed in claim 1, wherein the protective gas comprises argon or nitrogen.
6. The method for preparing a high purity carbon material according to claim 1, wherein the vacuum induction furnace comprises a vertical vacuum induction furnace and a horizontal vacuum induction furnace.
7. The method for producing a high purity carbon material according to claim 6, wherein the vacuum induction furnace is a vertical vacuum induction furnace.
8. The method for preparing a high purity carbon material as claimed in claim 1, wherein steps S3 and S4 are repeated several times.
9. The method for preparing a high purity carbon material as claimed in claim 8, wherein the furnace temperature, the holding time and the vacuum degree are respectively adjustable during the circulation process.
10. The method for preparing a high purity carbon material according to claim 1, wherein the degree of vacuum after the vacuum treatment in the vacuum induction furnace is 0.01 to 10 torr.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109553089A (en) * | 2018-12-29 | 2019-04-02 | 赛福纳米科技(徐州)有限公司 | Multi-purpose material heat treatment apparatus |
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| CN113772669A (en) * | 2020-06-10 | 2021-12-10 | 湖南红太阳新能源科技有限公司 | Method for removing residual fluorine gas in purified graphite material |
| CN113860299A (en) * | 2021-10-25 | 2021-12-31 | 世星科技股份有限公司 | Graphite purification process |
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| JPS6379759A (en) * | 1986-09-22 | 1988-04-09 | 東洋炭素株式会社 | Manufacture of high purity graphite material and manufacturing apparatus therefor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109553089A (en) * | 2018-12-29 | 2019-04-02 | 赛福纳米科技(徐州)有限公司 | Multi-purpose material heat treatment apparatus |
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