CN218621128U - A graphite device for high-purity graphite powder nitrogen discharging - Google Patents
A graphite device for high-purity graphite powder nitrogen discharging Download PDFInfo
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- CN218621128U CN218621128U CN202223114406.1U CN202223114406U CN218621128U CN 218621128 U CN218621128 U CN 218621128U CN 202223114406 U CN202223114406 U CN 202223114406U CN 218621128 U CN218621128 U CN 218621128U
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Abstract
The utility model discloses a graphite device for discharging nitrogen from high-purity graphite powder, which comprises a graphite crucible base, a graphite crucible cylinder, a graphite cover, a graphite air pipe, an upper graphite baffle plate and a lower graphite baffle plate; the graphite crucible base and the graphite cover are respectively arranged at the bottom and the top of the graphite crucible cylinder, and the graphite cover and the graphite crucible base are respectively provided with an upper air inlet and outlet hole and a lower air inlet and outlet hole; a plurality of air holes are distributed on the graphite air pipes, the graphite air pipes are arranged in the graphite crucible cylinder, two ends of each graphite air pipe are respectively sleeved and embedded on the upper graphite partition plate and the lower graphite partition plate, and two ends of each graphite air pipe are respectively communicated with the upper air inlet and outlet hole and the lower air inlet and outlet hole; graphite powder is filled in the inner cavity of the graphite crucible barrel at the periphery of each graphite gas pipe; use the utility model provides a graphite device for high-purity graphite powder nitrogen discharging carries out graphite powder nitrogen discharging technology, can show the nitrogen content who reduces in the graphite powder, and synthetic high-purity carborundum raw materials can be used for semi-insulating type carborundum single crystal to grow and use.
Description
Technical Field
The utility model relates to a semiconductor technology field especially relates to a graphite device that is used for high-purity graphite powder to arrange nitrogen.
Background
Graphite powder is usually purified to be more than 5N by adding halogen elements at high temperature, the requirement of synthesizing a third-generation semiconductor conductive silicon carbide raw material can be met, but the nitrogen content of the semi-insulating silicon carbide raw material needs to be strictly controlled, and the carbon powder needs to be subjected to nitrogen discharge treatment. The nitrogen content in the graphite powder mainly consists of combined nitrogen and adsorbed nitrogen. The nitrogen compounds are mainly AlN, BN and C 3 N 4 Etc., extremely difficult to remove; the adsorbed nitrogen can be divided into low-temperature adsorbed nitrogen and high-temperature adsorbed nitrogen, the low-temperature adsorbed nitrogen can be removed by repeatedly vacuumizing before use, but the high-temperature adsorbed nitrogen needs to be discharged by high temperature, high vacuum and small molecule gas replacement.
In summary, the synthesis of nitrogen-discharging from semi-insulating silicon carbide feedstock is a problem that needs to be solved by those skilled in the art.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing a graphite device for nitrogen is arranged to high-purity graphite powder to solve the problem that above-mentioned prior art exists, can show the nitrogen content who reduces in the graphite powder, synthetic high-purity carborundum raw materials can be used for semi-insulating type carborundum single crystal to grow and use.
In order to achieve the above purpose, the utility model provides a following scheme:
the utility model provides a graphite device for discharging nitrogen from high-purity graphite powder, which comprises a graphite crucible base, a graphite crucible cylinder, a graphite cover, a graphite air pipe, an upper graphite baffle plate and a lower graphite baffle plate; the graphite crucible base and the graphite cover are respectively arranged at the bottom and the top of the graphite crucible cylinder, and an upper air inlet and an upper air outlet and a lower air inlet and an air outlet are respectively arranged on the graphite cover and the graphite crucible base; the upper graphite partition plate is arranged at the bottom of the upper air inlet and outlet hole, and the lower graphite partition plate is arranged at the top of the lower air inlet and outlet hole; a plurality of air holes are distributed on the graphite air pipe, the graphite air pipe is provided with a plurality of air holes, the graphite air pipe is arranged in the graphite crucible cylinder, two ends of each graphite air pipe are respectively sleeved and embedded on the upper graphite clapboard and the lower graphite clapboard, and two ends of each graphite air pipe are respectively communicated with the upper air inlet and the lower air inlet and outlet; and the inner cavity of the graphite crucible cylinder at the periphery of each graphite air pipe is filled with graphite powder.
Preferably, the upper graphite partition is arranged at the bottom of the graphite cover, the lower graphite partition is arranged in the graphite crucible base, an upper air passing cavity communicated with the upper air inlet and outlet holes is reserved between the upper graphite partition and the graphite cover, and a lower air passing cavity communicated with the lower air inlet and outlet holes is reserved between the lower graphite partition and the graphite crucible base.
Preferably, the upper graphite baffle plate and the lower graphite baffle plate are provided with sleeve holes for sleeving and embedding the graphite air pipes, and the sleeve holes are in clearance fit with the graphite air pipes.
Preferably, the plurality of air holes on the graphite air pipe are air holes processed on the pipe body or air holes of the pipe body made of graphite materials.
Preferably, at least 5 graphite gas pipes are arranged.
Preferably, the number of the upper air inlet and outlet holes and the number of the lower air inlet and outlet holes are more than 12, and the upper air inlet and outlet holes and the lower air inlet and outlet holes are uniformly distributed on the graphite cover and the graphite crucible base respectively.
Preferably, the graphite cover and the graphite crucible base are in threaded connection with the graphite crucible cylinder.
Preferably, the top of the graphite cover is provided with at least two bolt holes for connecting with external extraction equipment.
The utility model discloses following beneficial technological effect has been gained for prior art:
the utility model provides a graphite device for high-purity graphite powder nitrogen discharging adopts the structural style of graphite crucible cooperation porous graphite trachea, possesses the advantage of big capacity and high gas throughput rate, and during operation, the micromolecular gas is evenly filled in the graphite device, is favorable to the micromolecular gas to replace out the nitrogen molecule, reaches the purpose of nitrogen discharging; the nitrogen content in the graphite powder can be obviously reduced, and the synthesized high-purity silicon carbide raw material can be used for the growth of semi-insulating silicon carbide single crystals.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
Fig. 1 is a schematic structural view of a graphite device for discharging nitrogen from high-purity graphite powder according to the present invention;
FIG. 2 is a cross-sectional view of a graphite apparatus for discharging nitrogen from high purity graphite powder in accordance with the present invention;
in the figure: 11-upper air inlet and outlet holes, 12-lower air inlet and outlet holes, 21-upper graphite partition plate, 22-lower graphite partition plate, 3-graphite crucible base, 4-graphite crucible barrel, 5-graphite air pipe, 6-graphite powder, 7-graphite cover, 8-bolt hole, 9-upper air passing cavity and 10-lower air passing cavity.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative efforts all belong to the protection scope of the present invention.
The utility model aims at providing a graphite device for high-purity graphite powder row nitrogen to solve the problem that prior art exists.
In order to make the above objects, features and advantages of the present invention more comprehensible, the present invention is described in detail with reference to the accompanying drawings and the detailed description.
The graphite device for discharging nitrogen from high-purity graphite powder in the embodiment, as shown in fig. 1 and 2, includes a graphite crucible base 3, a graphite crucible cylinder 4, a graphite cover 7, a graphite gas pipe 5, an upper graphite partition plate 21 and a lower graphite partition plate 22; the graphite crucible base 3 and the graphite cover 7 are respectively arranged at the bottom and the top of the graphite crucible barrel 4, and the graphite cover 7 and the graphite crucible base 3 are respectively provided with an upper air inlet and outlet hole 11 and a lower air inlet and outlet hole 12; the upper graphite partition plate 21 is arranged at the bottom of the upper air inlet and outlet hole 11, and the lower graphite partition plate 22 is arranged at the top of the lower air inlet and outlet hole 12; a plurality of air holes are distributed on the graphite air pipe 5, the graphite air pipes 5 are provided with a plurality of air holes, the graphite air pipes 5 are arranged in the graphite crucible cylinder 4, two ends of each graphite air pipe 5 are respectively sleeved and embedded on the upper graphite partition plate 21 and the lower graphite partition plate 22, and two ends of each graphite air pipe 5 are respectively communicated with the upper air inlet and outlet hole 11 and the lower air inlet and outlet hole 12; the inner cavity of the graphite crucible cylinder 4 at the periphery of each graphite air pipe 5 is filled with graphite powder 6.
In this embodiment, the upper graphite partition 21 is disposed at the bottom of the graphite cover 7, the lower graphite partition 22 is disposed in the graphite crucible base 3, an upper air-passing cavity 9 communicating with the upper air inlet and outlet hole 11 is left between the upper graphite partition 21 and the graphite cover 7, and a lower air-passing cavity 10 communicating with the lower air inlet and outlet hole 12 is left between the lower graphite partition 22 and the graphite crucible base 3. Go up graphite baffle 21 and be provided with the trepanning that is used for the cover to inlay graphite trachea 5 on the graphite baffle 22 down, clearance fit between trepanning and the graphite trachea 5, the nested gap of leaving makes the material can have sufficient expansion space in the heating process, goes up graphite baffle 21, graphite baffle 22 down and not only plays the effect of fixed graphite trachea 5, simultaneously under quick evacuation, can protect high-purity graphite powder 6 not taken out.
In this embodiment, the pores of the graphite gas tube 5 are pores processed on the tube body or pores of the tube body made of graphite (porosity > 30%).
In this embodiment, at least 5 graphite gas pipes 5 are provided, and when 5 graphite gas pipes are provided, 1 graphite gas pipe 5 is located at the center of the graphite crucible barrel 4, and the other 4 graphite gas pipes 5 are uniformly distributed circumferentially around the axis of the graphite crucible barrel 4. The number of the upper air inlet and outlet holes 11 and the number of the lower air inlet and outlet holes 12 are all larger than 12 and are uniformly distributed on the graphite cover 7 and the graphite crucible base 3 respectively. The upper air inlet and outlet holes 11 and the lower air inlet and outlet holes 12 can be distributed in a circumferential outward diffusion mode or in a rectangular array mode by taking the center of the graphite cover 7 as a center.
In the embodiment, the graphite cover 7 and the graphite crucible base 3 are both in threaded connection with the graphite crucible cylinder 4, and mainly play roles of supporting the upper graphite partition plate 21 and the lower graphite partition plate 22 and containing the high-purity graphite powder 6.
In this embodiment, at least two bolt holes 8 are formed in the top of the graphite cover 7 for connecting an external extraction device, so that the whole device can be conveniently extracted and used.
The purity of the graphite material used in this example was greater than 5N.
The utility model provides a graphite device for high-purity graphite powder nitrogen extraction, the theory of operation as follows:
after high-purity graphite powder is placed in the graphite crucible device, the device filled with the high-purity graphite powder is placed in a thermal field and then is placed in a PVT furnace, the limit vacuum is pumped to be below 10-6mbar and is kept for 4-10 hours, and N adsorbed at low temperature in the high-purity graphite powder is interpreted and discharged and is pumped out through a vacuum system; then heating the carbon powder to 1000-1200 ℃ by induction heating and filling with small molecule gas (H) 2 、He、H 2 +He、H 2 + Ar, the purity is more than 6N) to the pressure in the furnace of 300-800mbar, the vacuum pumping is carried out to 10-6mbar after the pressure is maintained for 1-4 hours, 3-5 cycles are repeated, replacement is carried out through micromolecule gas and nitrogen molecules, and the nitrogen absorbed in the deep layer is pumped out through high vacuum to achieve the effect of nitrogen exhaust; then subsequently adding by inductionHeating the hot graphite crucible to 2000-2300 deg.C, introducing mixed gas of small molecule gas and inert gas, and performing high temperature nitrogen discharge treatment. The gas enters the graphite gas pipe 5 through the gas holes on the graphite gas pipe 5 and is pumped out through the upper gas inlet and outlet hole 11 on the graphite cover 7 and the lower gas inlet and outlet hole 12 on the graphite crucible base 3.
The utility model discloses the principle and the implementation mode of the utility model are explained by applying the concrete examples, and the explanation of the above examples is only used for helping to understand the method and the core idea of the utility model; meanwhile, for those skilled in the art, the idea of the present invention may be changed in the specific embodiments and the application range. In summary, the content of the present description should not be construed as a limitation of the present invention.
Claims (8)
1. The utility model provides a graphite device that is used for high-purity graphite powder to arrange nitrogen which characterized in that: comprises a graphite crucible base, a graphite crucible cylinder, a graphite cover, a graphite gas pipe, an upper graphite clapboard and a lower graphite clapboard; the graphite crucible base and the graphite cover are respectively arranged at the bottom and the top of the graphite crucible cylinder, and the graphite cover and the graphite crucible base are respectively provided with an upper air inlet and an upper air outlet and a lower air inlet and an air outlet; the upper graphite partition plate is arranged at the bottom of the upper air inlet and outlet hole, and the lower graphite partition plate is arranged at the top of the lower air inlet and outlet hole; a plurality of air holes are distributed on the graphite air pipe, the graphite air pipes are provided with a plurality of air holes, the graphite air pipes are arranged in the graphite crucible cylinder, two ends of each graphite air pipe are respectively sleeved and embedded on the upper graphite partition plate and the lower graphite partition plate, and two ends of each graphite air pipe are respectively communicated with the upper air inlet hole and the lower air inlet hole; graphite powder is filled in the inner cavity of the graphite crucible cylinder at the periphery of each graphite air pipe.
2. The graphite apparatus for nitrogen rejection of high purity graphite powder of claim 1, wherein: the upper graphite partition plate is arranged at the bottom of the graphite cover, the lower graphite partition plate is arranged in the graphite crucible base, an upper air passing cavity communicated with the upper air inlet and outlet holes is reserved between the upper graphite partition plate and the graphite cover, and a lower air passing cavity communicated with the lower air inlet and outlet holes is reserved between the lower graphite partition plate and the graphite crucible base.
3. The graphite apparatus for nitrogen rejection of high purity graphite powder of claim 2, wherein: and the upper graphite clapboard and the lower graphite clapboard are provided with sleeve holes for sleeving and embedding the graphite air pipes, and the sleeve holes are in clearance fit with the graphite air pipes.
4. The graphite apparatus for nitrogen discharge of high purity graphite powder as claimed in claim 1, wherein: the plurality of air holes on the graphite air pipe are air holes processed on the pipe body or air holes which are made of graphite and are arranged on the pipe body.
5. The graphite apparatus for nitrogen discharge of high purity graphite powder as claimed in claim 1, wherein: the graphite trachea is provided with at least 5.
6. The graphite apparatus for nitrogen discharge of high purity graphite powder as claimed in claim 1, wherein: the number of the upper air inlet and outlet holes and the number of the lower air inlet and outlet holes are larger than 12, and the upper air inlet and outlet holes and the lower air inlet and outlet holes are uniformly distributed on the graphite cover and the graphite crucible base respectively.
7. The graphite apparatus for nitrogen rejection of high purity graphite powder of claim 1, wherein: the graphite cover and the graphite crucible base are in threaded connection with the graphite crucible cylinder.
8. The graphite apparatus for nitrogen discharge of high purity graphite powder as claimed in claim 1, wherein: the top of graphite lid is provided with two bolt holes at least for connect outside extraction equipment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202223114406.1U CN218621128U (en) | 2022-11-23 | 2022-11-23 | A graphite device for high-purity graphite powder nitrogen discharging |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202223114406.1U CN218621128U (en) | 2022-11-23 | 2022-11-23 | A graphite device for high-purity graphite powder nitrogen discharging |
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| CN218621128U true CN218621128U (en) | 2023-03-14 |
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| CN202223114406.1U Active CN218621128U (en) | 2022-11-23 | 2022-11-23 | A graphite device for high-purity graphite powder nitrogen discharging |
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