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High-purity graphite powder and preparation method thereof

A technology of high-purity graphite powder and graphite powder, applied in chemical instruments and methods, inorganic chemistry, non-metallic elements, etc., can solve problems such as inability to remove high melting point carbides, and achieve high practical value and significant effects

Inactive Publication Date: 2019-02-01
ADVANCED FOR MATERIALS & EQUIP
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Based on this, it is necessary to provide a high-purity graphite powder and a preparation method thereof for the technical problem that carbides with high melting point and high boiling point cannot be removed in the prior art, which can increase the purity of graphite powder from 99% to more than 99.9999%, effectively Solve the purification problem of high-purity graphite

Method used

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  • High-purity graphite powder and preparation method thereof
  • High-purity graphite powder and preparation method thereof
  • High-purity graphite powder and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A preparation method of high-purity graphite powder, comprising the steps of:

[0029] S1. Take petroleum coke (purity: 99.85%) with a particle size D50 of 0.5-0.8mm in a graphite boat with a size of φ52×360mm, and put it into GP-0512 graphite with an inner cavity size of φ60×1200mm for purification In the equipment, feed Ar (purity ≥ 99.999%) to purge for 10 minutes, with a flow rate of 20L / h, so that the pressure in the purification equipment is 1.5KPa;

[0030] S2. When the temperature rises to 1600°C, CCl is introduced 4 , the heating rate is 10°C / min, the flow rate is 150L / h, the heat preservation is 2h, and the Ar flow rate is increased to 200L / h;

[0031] S3. Heat up to 2200°C and start feeding CHClF 2 , the heating rate is 1°C / min, the flow rate is 100L / h, the heat preservation is 2h, and the CCl in step S2 is maintained 4 and Ar flow constant;

[0032] S4, heating up to 2800°C to stop feeding CCl 4 and CHClF 2 , the heating rate was 1°C / min, the temperatu...

Embodiment 2

[0035] A preparation method of high-purity graphite powder, comprising the steps of:

[0036] S1. Take flake graphite (purity: 99.5%) with a particle size D50 of 0.5-1.0mm in a graphite boat with a size of φ52×360mm, and put it into the graphite purification equipment GP-0512 with an inner cavity size of φ60×1200mm after loading. , feed Ar (purity ≥ 99.999%) to purge for 5 minutes, flow rate 20L / h, so that the pressure in the purification equipment is 1.7KPa;

[0037] S2. Raise the temperature to 1650°C and start to feed CCl 4 , the heating rate is 15°C / min, the flow rate is 100L / h, the heat preservation time is 0.5h, and the Ar flow rate is increased to 200L / h;

[0038] S3. Heat up to 2300°C and start feeding CHClF 2 , heating rate 3°C / min, flow rate 100L / h, heat preservation 2h, maintain CCl in step S2 4 and Ar flow constant;

[0039] S4. Heating up to 2850°C and stopping the introduction of CCl 4 and CHClF 2 , the heating rate was 3°C / min, the temperature was kept for...

Embodiment 3

[0042] S1. Take microcrystalline graphite (purity: 99.7%) with a particle size D50 of 0.5-1.0mm in a graphite boat with a size of φ52×360mm, and put it into a graphite purification equipment with an inner cavity size of φ60×1200mm after loading. In 0512, pass Ar (purity ≥ 99.999%) to purge for 10 minutes, with a flow rate of 20L / h, so that the pressure in the purification equipment is 1.8KPa;

[0043] S2. When the temperature rises to 1700°C, CCl is introduced 4 , the heating rate is 13°C / min, the flow rate is 200L / h, the heat preservation is 1h, and the Ar flow rate is increased to 200L / h;

[0044] S3. Heat up to 2300°C and start feeding CHClF 2 , heating rate 2°C / min, flow rate 75L / h, heat preservation 1.5h, maintain CCl in step S2 4 and Ar flow constant;

[0045] S4. Heating up to 2850°C and stopping the introduction of CCl 4 and CHClF 2 , the heating rate was 2°C / min, the temperature was kept for 0.8h, the Ar flow rate was reduced to 25L / h, and the temperature was low...

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Abstract

The invention relates to high-purity graphite powder and a preparation method thereof. The preparation method comprises the following steps: adding graphite powder raw materials in a graphite boat, mounting the graphite boat in graphite purification equipment, and feeding argon for blowing; feeding purified gas A at the temperature of 1200-1800 DEG C, and insulating for 0.5-2 h; when heating to the temperature of 2000-2400 DEG C, feeding purified gas B and keeping feeding purified gas A; when heating to the temperature of 2600-3000 DEG C, stopping feeding the purified gas A and the purified gas B, insulating for 0.5-2 h, and cooling to the room temperature to obtain the high-purity graphite powder. In a whole preparation process, argon needs to be fed continuously for protection. Gas heatpurification and high-temperature purification are combined scientifically, key impurities such as B, Al and V in the graphite powder raw materials are removed thoroughly, therefore, the high-purity graphite powder with the purity greater than or equal to 99.9999% is obtained, conditions are created for industrialized production of the high-purity graphite powder with the carbon content of 99.9999% or above, and a certain scientific basis is provided.

Description

technical field [0001] The invention relates to the technical field of graphite powder materials, in particular to a high-purity graphite powder and a preparation method thereof. Background technique [0002] In recent years, graphite users in the semiconductor and electronics industries have placed very stringent requirements on the purity of graphite. In order to meet the needs of special materials used in the semiconductor and electronics industries, the content of certain impurity elements in graphite must be controlled within 10 -8 order of magnitude, which puts forward higher requirements on the purity of graphite powder. [0003] The main impurity components contained in graphite powder raw materials are silicate minerals such as K, Na, Mg, Fe, Ca, etc. These impurities can be effectively removed by high temperature method, but a single high temperature method can only produce 99.99% purity Graphite powder between ~99.999%. The reason is that the high temperature m...

Claims

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Application Information

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IPC IPC(8): C01B32/215
CPCC01B32/215
Inventor 戴煜邓军旺许鹏谢煜明
Owner ADVANCED FOR MATERIALS & EQUIP
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