CN116813348A - Reduction treatment method and process for high-yield graphite column - Google Patents

Reduction treatment method and process for high-yield graphite column Download PDF

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Publication number
CN116813348A
CN116813348A CN202310843720.3A CN202310843720A CN116813348A CN 116813348 A CN116813348 A CN 116813348A CN 202310843720 A CN202310843720 A CN 202310843720A CN 116813348 A CN116813348 A CN 116813348A
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Prior art keywords
graphite
graphite column
reduction treatment
treatment method
column
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Inventor
李洪现
贾风中
王涛
朱华民
常洪菊
王新
杜冠新
王延平
张巧霞
刘小凤
李东敖
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Liaocheng Guanxian Shangao Superhard Material Co ltd
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Liaocheng Guanxian Shangao Superhard Material Co ltd
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Priority to CN202310843720.3A priority Critical patent/CN116813348A/en
Publication of CN116813348A publication Critical patent/CN116813348A/en
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped 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
    • C04B35/52Shaped 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
    • C04B35/522Graphite
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6567Treatment time
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/658Atmosphere during thermal treatment
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/66Specific sintering techniques, e.g. centrifugal sintering
    • C04B2235/667Sintering using wave energy, e.g. microwave sintering
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency
    • Y02P20/129Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines

Abstract

The invention discloses a high-yield graphite column reduction treatment method and a high-yield graphite column reduction treatment process, wherein the high-yield graphite column reduction treatment method comprises the following steps: s1: detecting graphite column raw materials, namely detecting compactness and components of the graphite column materials; s2: pre-pressing the graphite column, namely placing the graphite column into a compression mold, and compressing the graphite column; s3: cleaning the graphite column to remove the powdered ink on the surface of the graphite column; s4: microwave heating, namely placing the graphite column in a microwave heating furnace path for continuous heating; s5: regulating and controlling the heating atmosphere, regulating the contents of hydrogen, nitrogen and argon in the heating atmosphere, and regulating the pulse pressure and the pulse times; s6: and (5) finishing heating, and finishing the reduction treatment of the graphite column. The invention adopts the mode of ensuring the application effect of the graphite column and microwave heating, so that the temperature inside and outside the graphite column is consistent, and the reduction treatment efficiency is effectively improved and the energy consumption is reduced by matching with the mode of positive pressure atmosphere sintering.

Description

Reduction treatment method and process for high-yield graphite column
Technical Field
The invention relates to the technical field of diamond manufacturing, in particular to a high-yield graphite column reduction treatment method and a high-yield graphite column reduction treatment process.
Background
The diamond has high hardness, so that the diamond is widely applied in industry and can be used for cutting, grinding and drilling; the heat spreader has high heat conductivity and good electrical insulation, and can be used as a heat spreader of a semiconductor device; the synthetic diamond has excellent light transmittance and corrosion resistance, is widely applied in the electronic industry, and is unfavorable for saving industrial production cost because the natural diamond is less in natural environment and has high price, so people start to adopt the synthetic diamond, and the requirements of practical application can be met because the properties of the synthetic diamond and the natural diamond are different.
After massive search, the prior art is found that: the invention discloses a preparation process of a graphite column for diamond synthesis, which comprises the steps of firstly adding a nucleating agent and metal powder into a mixer, continuously mixing the mixture after adding a dispersing agent in the mixing process, then continuously mixing the graphite powder and the dispersing agent, granulating the mixture twice, performing primary compression molding, heating on an intermediate frequency heater after molding, rapidly performing secondary compression molding, repeatedly carrying out reheating and repressing on the graphite column, and finally carrying out microwave reduction treatment on the graphite column.
In summary, in the diamond manufacturing field, a powder catalyst method is generally adopted to produce diamond, and the produced diamond presents black particles due to oxidation of the surface of catalyst powder, so that the diamond cannot be applied commercially, and a common solution in practical industrial production is high-temperature vacuum reduction treatment.
Disclosure of Invention
The invention aims to provide a high-yield graphite column reduction treatment method and a high-yield graphite column reduction treatment process, so as to solve the problems in the background technology.
In order to achieve the above purpose, the present invention provides the following technical solutions: a high-yield graphite column reduction treatment method and process, the graphite column reduction treatment method is as follows:
s1: detecting graphite column raw materials, namely detecting compactness and components of the graphite column materials;
s2: pre-pressing the graphite column, namely placing the graphite column into a compression mold, and compressing the graphite column;
s3: cleaning the graphite column to remove the powdered ink on the surface of the graphite column;
s4: microwave heating, namely placing the graphite column in a microwave heating furnace path for continuous heating;
s5: regulating and controlling the heating atmosphere, regulating the contents of hydrogen, nitrogen and argon in the heating atmosphere, and regulating the pulse pressure and the pulse times;
s6: and (5) finishing heating, and finishing the reduction treatment of the graphite column.
Preferably, in S1 based on the graphite column reduction treatment method:
and (3) inspecting the graphite columns serving as raw materials, respectively inspecting the graphite columns with the same batch and specification, respectively sampling and detecting the surface, the inside, the upper end, the middle end and the lower end of the graphite columns, and detecting the density and the components of the whole graphite columns and sampling parts of the graphite columns for reflecting the quality and the impurity content of the graphite columns.
Preferably, in S2 based on the graphite column reduction treatment method:
placing the graphite columns which are qualified in inspection in a pre-pressing die, wherein synchronous compression members are arranged at the two ends of the pre-pressing die, respectively applying pressure to the two ends of the graphite columns, and compressing the graphite columns for improving the density of the graphite columns.
Preferably, in S3 based on the graphite column reduction treatment method:
and placing the pre-pressed graphite column in an air purging channel, and purging the surface of the graphite column with compressed air at a high speed for removing residual toner on the surface of the graphite column, so as to keep the surface of the graphite column clean.
Preferably, in S4 based on the graphite column reduction treatment method:
the graphite columns are arranged linearly and enter a microwave heating furnace path, the graphite columns are heated in a microwave heating mode, the graphite columns are uniformly heated from inside to outside, and a servo driving system is arranged in the microwave heating furnace path and used for regulating and controlling the advancing speed of the graphite columns.
Preferably, in S5 based on the graphite column reduction treatment method:
the computer control system is adopted to regulate the input flow and the input proportion of the hydrogen, the nitrogen and the argon respectively, and is used for regulating the mixed atmosphere in the microwave heating furnace path and controlling the output pulse, the pulse pressure and the frequency.
Preferably, in S6 based on the graphite column reduction treatment method:
the graphite column passing through the microwave heating furnace is subjected to a natural cooling stage, and the residual temperature of 200-300 ℃ is kept for subsequent use.
Preferably, the temperature in the microwave heating furnace is controlled between 800 and 950 ℃, and the input speed of the graphite column is 1cm/min.
Preferably, the mixing atmosphere is: 25% of hydrogen, 60% of nitrogen and 15% of argon; pulse pressure: the pressure is 0.3MPa higher, the pressure is 0.01MPa lower, and the pulse times are 10 times.
Preferably, the heating range in the microwave heating tunnel is three stages: the first stage is a preheating stage, and the preheating temperature is 30-250 ℃; the second stage is a high temperature stage, and the temperature is 500-1000 ℃; the third stage is waste heat stage with temperature of 950-600deg.C and high temperature stage time of 2-4h.
Compared with the prior art, the invention has the beneficial effects that: the invention adopts a microwave heating mode, can effectively ensure the heating comprehensiveness of the graphite column, avoids the problem of uneven distribution of traditional resistance heating heat, combines positive pressure mixed atmosphere for sintering, has more comprehensive and efficient reduction treatment of the graphite column, and performs detection and pre-pressing treatment of the graphite column before the reduction treatment of the graphite column, keeps the internal structure of the graphite column compact, is beneficial to microwave heating, and can reduce the energy consumption of sintering.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Two embodiments provided by the present invention:
embodiment one:
a high-yield graphite column reduction treatment method comprises the following steps:
s1: detecting graphite column raw materials, namely detecting compactness and components of the graphite column materials; and (3) inspecting the graphite columns serving as raw materials, respectively inspecting the graphite columns with the same batch and specification, respectively sampling and detecting the surface, the inside, the upper end, the middle end and the lower end of the graphite columns, and detecting the density and the components of the whole graphite columns and sampling parts of the graphite columns for reflecting the quality and the impurity content of the graphite columns.
S2: pre-pressing the graphite column, namely placing the graphite column into a compression mold, and compressing the graphite column; placing the graphite columns which are qualified in inspection in a pre-pressing die, wherein synchronous compression members are arranged at the two ends of the pre-pressing die, respectively applying pressure to the two ends of the graphite columns, and compressing the graphite columns for improving the density of the graphite columns.
S3: cleaning the graphite column to remove the powdered ink on the surface of the graphite column; and placing the pre-pressed graphite column in an air purging channel, and purging the surface of the graphite column with compressed air at a high speed for removing residual toner on the surface of the graphite column, so as to keep the surface of the graphite column clean.
S4: microwave heating, namely placing the graphite column in a microwave heating furnace path for continuous heating; the graphite columns are arranged linearly and enter a microwave heating furnace path, the graphite columns are heated in a microwave heating mode, the graphite columns are uniformly heated from inside to outside, and a servo driving system is arranged in the microwave heating furnace path and used for regulating and controlling the advancing speed of the graphite columns.
S5: regulating and controlling the heating atmosphere, regulating the contents of hydrogen, nitrogen and argon in the heating atmosphere, and regulating the pulse pressure and the pulse times; the computer control system is adopted to regulate the input flow and the input proportion of the hydrogen, the nitrogen and the argon respectively, and is used for regulating the mixed atmosphere in the microwave heating furnace path and controlling the output pulse, the pulse pressure and the frequency.
S6: and after heating, finishing the reduction treatment of the graphite column, and naturally cooling the graphite column passing through the microwave heating furnace channel, and maintaining the residual temperature of 200-300 ℃ for subsequent use.
Embodiment two:
the temperature in the microwave heating furnace is controlled at 800-950 ℃, and the input speed of the graphite column is 1cm/min.
The mixed atmosphere is as follows: 25% of hydrogen, 60% of nitrogen and 15% of argon; pulse pressure: the method is characterized in that the method is 0.3MPa high, 0.01MPa low and 10 times of pulse times, and a computer control system is adopted to respectively regulate and control the input flow and the input proportion of hydrogen, nitrogen and argon, and is used for regulating the mixed atmosphere in a microwave heating furnace path and controlling the output pulse, the pulse pressure and the pulse times.
Heating range in the microwave heating oven channel is three stages: the first stage is a preheating stage, and the preheating temperature is 30-250 ℃; the second stage is a high temperature stage, and the temperature is 500-1000 ℃; the third stage is waste heat stage with temperature of 950-600deg.C and high temperature stage time of 2-4h.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.

Claims (10)

1. A high-yield graphite column reduction treatment method is characterized in that: the reduction treatment method of the graphite column comprises the following steps:
s1: detecting graphite column raw materials, namely detecting compactness and components of the graphite column materials;
s2: pre-pressing the graphite column, namely placing the graphite column into a compression mold, and compressing the graphite column;
s3: cleaning the graphite column to remove the powdered ink on the surface of the graphite column;
s4: microwave heating, namely placing the graphite column in a microwave heating furnace path for continuous heating;
s5: regulating and controlling the heating atmosphere, regulating the contents of hydrogen, nitrogen and argon in the heating atmosphere, and regulating the pulse pressure and the pulse times;
s6: and (5) finishing heating, and finishing the reduction treatment of the graphite column.
2. The high-yield graphite column reduction treatment method according to claim 1, wherein the method comprises the following steps: in S1 based on the graphite column reduction treatment method:
and (3) inspecting the graphite columns serving as raw materials, respectively inspecting the graphite columns with the same batch and specification, respectively sampling and detecting the surface, the inside, the upper end, the middle end and the lower end of the graphite columns, and detecting the density and the components of the whole graphite columns and sampling parts of the graphite columns for reflecting the quality and the impurity content of the graphite columns.
3. The high-yield graphite column reduction treatment method according to claim 1, wherein the method comprises the following steps: in S2 based on the graphite column reduction treatment method:
placing the graphite columns which are qualified in inspection in a pre-pressing die, wherein synchronous compression members are arranged at the two ends of the pre-pressing die, respectively applying pressure to the two ends of the graphite columns, and compressing the graphite columns for improving the density of the graphite columns.
4. The high-yield graphite column reduction treatment method according to claim 1, wherein the method comprises the following steps: in S3 based on the graphite column reduction treatment method:
and placing the pre-pressed graphite column in an air purging channel, and purging the surface of the graphite column with compressed air at a high speed for removing residual toner on the surface of the graphite column, so as to keep the surface of the graphite column clean.
5. The high-yield graphite column reduction treatment method according to claim 1, wherein the method comprises the following steps: in S4 based on the graphite column reduction treatment method:
the graphite columns are arranged linearly and enter a microwave heating furnace path, the graphite columns are heated in a microwave heating mode, the graphite columns are uniformly heated from inside to outside, and a servo driving system is arranged in the microwave heating furnace path and used for regulating and controlling the advancing speed of the graphite columns.
6. The high-yield graphite column reduction treatment method according to claim 1, wherein the method comprises the following steps: in S5 based on the graphite column reduction treatment method:
the computer control system is adopted to regulate the input flow and the input proportion of the hydrogen, the nitrogen and the argon respectively, and is used for regulating the mixed atmosphere in the microwave heating furnace path and controlling the output pulse, the pulse pressure and the frequency.
7. The high-yield graphite column reduction treatment method according to claim 1, wherein the method comprises the following steps: in S6 based on the graphite column reduction treatment method:
the graphite column passing through the microwave heating furnace is subjected to a natural cooling stage, and the residual temperature of 200-300 ℃ is kept for subsequent use.
8. The high-yield graphite column reduction treatment process according to claim 1, wherein: the temperature in the microwave heating furnace is controlled at 800-950 ℃, and the input speed of the graphite column is 1cm/min.
9. The high-yield graphite column reduction treatment process according to claim 1, wherein: the mixed atmosphere is as follows: 25% of hydrogen, 60% of nitrogen and 15% of argon; pulse pressure: the pressure is 0.3MPa higher, the pressure is 0.01MPa lower, and the pulse times are 10 times.
10. The high-yield graphite column reduction treatment process according to claim 1, wherein: heating range in the microwave heating oven channel is three stages: the first stage is a preheating stage, and the preheating temperature is 30-250 ℃; the second stage is a high temperature stage, and the temperature is 500-1000 ℃; the third stage is waste heat stage with temperature of 950-600deg.C and high temperature stage time of 2-4h.
CN202310843720.3A 2023-07-11 2023-07-11 Reduction treatment method and process for high-yield graphite column Pending CN116813348A (en)

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Application Number Priority Date Filing Date Title
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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102557024A (en) * 2011-12-20 2012-07-11 湖南省中晟热能科技有限公司 Reduction method of composite material particles of graphite for synthetic diamond and contact agent
CN106348288A (en) * 2016-08-18 2017-01-25 中南钻石有限公司 Purifying process for synthesizing graphite core column for industrial diamonds
WO2018044762A1 (en) * 2016-08-31 2018-03-08 Rutgers, The State University Of New Jersey High-quality graphene and method of producing same via microwave reduction of graphene oxide
CN109292761A (en) * 2018-12-07 2019-02-01 四川聚创石墨烯科技有限公司 A kind of method of smooth microwave reduction graphene oxide
CN208800082U (en) * 2018-08-27 2019-04-30 河南省力量钻石股份有限公司 Diamond graphite column vacuum reduction cloth bracket and vacuum reduction device
CN111257385A (en) * 2020-01-20 2020-06-09 华侨大学 Oxygen reduction activity testing device and method based on gas diffusion electrode
CN112873972A (en) * 2021-02-23 2021-06-01 郑州华晶金刚石股份有限公司 Preparation process of graphite column for diamond synthesis

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102557024A (en) * 2011-12-20 2012-07-11 湖南省中晟热能科技有限公司 Reduction method of composite material particles of graphite for synthetic diamond and contact agent
CN106348288A (en) * 2016-08-18 2017-01-25 中南钻石有限公司 Purifying process for synthesizing graphite core column for industrial diamonds
WO2018044762A1 (en) * 2016-08-31 2018-03-08 Rutgers, The State University Of New Jersey High-quality graphene and method of producing same via microwave reduction of graphene oxide
CN208800082U (en) * 2018-08-27 2019-04-30 河南省力量钻石股份有限公司 Diamond graphite column vacuum reduction cloth bracket and vacuum reduction device
CN109292761A (en) * 2018-12-07 2019-02-01 四川聚创石墨烯科技有限公司 A kind of method of smooth microwave reduction graphene oxide
CN111257385A (en) * 2020-01-20 2020-06-09 华侨大学 Oxygen reduction activity testing device and method based on gas diffusion electrode
CN112873972A (en) * 2021-02-23 2021-06-01 郑州华晶金刚石股份有限公司 Preparation process of graphite column for diamond synthesis

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