CN111560604A - Vertical spraying device for spraying type gas inlet CVD - Google Patents

Vertical spraying device for spraying type gas inlet CVD Download PDF

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Publication number
CN111560604A
CN111560604A CN202010542458.5A CN202010542458A CN111560604A CN 111560604 A CN111560604 A CN 111560604A CN 202010542458 A CN202010542458 A CN 202010542458A CN 111560604 A CN111560604 A CN 111560604A
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CN
China
Prior art keywords
spray
pipe
gas
cvd
spraying
Prior art date
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Pending
Application number
CN202010542458.5A
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Chinese (zh)
Inventor
于葛亮
张锦
刘伟铭
康斯坦丁·诺沃舍洛夫
孙正乾
杨金东
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Wuxi Flexsemi Semiconductor Technology Co ltd
Peking University
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Wuxi Flexsemi Semiconductor Technology Co ltd
Peking University
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Application filed by Wuxi Flexsemi Semiconductor Technology Co ltd, Peking University filed Critical Wuxi Flexsemi Semiconductor Technology Co ltd
Priority to CN202010542458.5A priority Critical patent/CN111560604A/en
Publication of CN111560604A publication Critical patent/CN111560604A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/455Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45563Gas nozzles
    • C23C16/45565Shower nozzles
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/455Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45502Flow conditions in reaction chamber
    • C23C16/4551Jet streams
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/455Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45557Pulsed pressure or control pressure

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Vapour Deposition (AREA)

Abstract

The invention relates to a spray type gas inlet CVD vertical spray device, which comprises a spray pipe and a spray head, wherein the lower end part of the spray pipe is fixed with the spray head, the middle section of the spray pipe is a preheating zone with a spiral pipe structure, and a bottom plate of the spray head is provided with spray holes. After the device is installed and used, the gas is fully preheated, and the gas-phase carbon source is fully preheated in the spraying device vertically, so that the reaction is more full. The gas source sprays and jets out, has a burst pressure when making gaseous phase carbon source act on the basement, and pressure can be adjusted through adjusting spray time and jet pressure, makes the better reaction of two-dimensional material.

Description

Vertical spraying device for spraying type gas inlet CVD
Technical Field
The invention relates to a device for two-dimensional material growth, in particular to a vertical spraying device for spraying type gas inlet CVD.
Background
The conventional method for growing two-dimensional materials on the market is as follows: the system comprises two temperature zones, wherein the low temperature zone is 800 ℃, the high temperature zone is 850 ℃, a catalyst and a substrate silicon wafer are placed in a quartz boat of the high temperature zone, then the catalyst and the substrate silicon wafer are mixed and preheated in the low temperature zone by controlling the flow rate of each gas, and the gas is diffused to the high temperature zone to react under the action of the catalyst and then deposited on the surface of the silicon wafer. The growth structure has the advantages of simple structure and convenient growth operation. The defects are that the repeatability of the two-dimensional material grown by practice is poor and not high, the quality of the grown two-dimensional material is also poor, and the single layer and the multiple layers are not controllable. Insufficient stability. The carbon source molecules enter the substrate airflow viscous layer in a diffusion mode, and the carbon source concentration and the gas phase near the catalyst have deviation, so that the utilization rate of the catalyst is not high.
The existing two-dimensional material growth carbon source can not be deposited on the silicon chip well, and the main analysis is as follows: the preheating of the gas source is insufficient, the flow direction of the gas-phase carbon source is not guided and is uncontrollable, carbon source molecules can only enter a substrate airflow viscous layer in a diffusion mode, and the concentration of the carbon source near the catalyst and the gas phase have deviation, so that the utilization rate of the catalyst is not high.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a vertical spraying device for spraying type gas inlet CVD, which has the advantages of full preheating of a gas source and controllable flow direction of a gas-phase carbon source during the growth of a two-dimensional material.
According to the technical scheme provided by the invention, the spray type gas inlet CVD vertical spray device comprises a spray pipe and a spray head, wherein the spray head is fixed at the lower end part of the spray pipe, the middle section of the spray pipe is a preheating zone with a spiral pipe structure, and a spray hole is formed in a bottom plate of the spray head.
Preferably, the inner diameter of the preheating zone is smaller than the inner diameter of the upper section of the spray pipe, the inner diameter of the preheating zone is smaller than the inner diameter of the lower section of the spray pipe, and the inner diameters of the upper section and the lower section of the spray pipe are equal.
Preferably, a mounting plate is fixed to an outer circumference of the upper stage of the shower pipe.
Preferably, the inner diameter of the shower head is gradually increased in a direction from top to bottom.
Preferably, the sum of the cross-sectional areas of the spray holes is smaller than the area of the inlet end of the spray pipe.
The invention has the following advantages:
1. the gas is fully preheated, and the gas phase carbon source is fully preheated in the spraying device vertically, so that the reaction is more full.
2. The gas source sprays and jets out, has a burst pressure when making gaseous phase carbon source act on the basement, and pressure can be adjusted through adjusting spray time and jet pressure, makes the better reaction of two-dimensional material.
Drawings
Fig. 1 is a schematic structural view of the present invention.
Fig. 2 is an enlarged sectional view of the showerhead of the present invention.
Detailed Description
The present invention will be further described with reference to the following specific examples.
The invention relates to a spray type gas inlet CVD vertical spray device, which comprises a spray pipe 1 and a spray head 2, wherein the spray head 2 is fixed at the lower end part of the spray pipe 1, the middle section of the spray pipe 1 is a preheating zone 11 with a spiral pipe structure, the upper section and the lower section of the spray pipe 1 are cylindrical straight pipes, and a spray hole 21 is arranged on a bottom plate of the spray head 2.
The inner diameter of the preheating zone 11 is smaller than that of the upper section of the spray pipe 1, the inner diameter of the preheating zone 11 is smaller than that of the lower section of the spray pipe 1, and the inner diameters of the upper section and the lower section of the spray pipe 1 are equal.
An installation disc 3 is fixed on the excircle of the upper section of the spray pipe 1.
In the direction from top to bottom, the inner diameter of the spray header 2 is gradually increased.
The sum of the cross-sectional areas of the spray holes 21 is smaller than the area of the inlet end of the spray pipe 1.
When the two-dimensional material preheating device works, mixed gas enters the preheating zone 11 adopting the spiral structure, the preheating zone 11 adopting the spiral structure increases the distance of the mixed gas, increases the heating area, fully preheats the mixed gas through time, and the fully preheated mixed gas is sprayed to the surface of a substrate through the spraying holes 21 to form certain spraying pressure, so that the gas phase concentration is consistent, the utilization rate of a catalyst is improved, and the growth efficiency and the quality of the two-dimensional material are improved. The number, size and density of the spray holes 21 can be changed according to the process requirements.
The invention is different from the horizontal air inlet of the traditional CVD equipment, the invention adopts the vertical spraying mode to feed air, and the following points are mainly considered:
1) the gas uniformity is further improved. When the reaction gas passes through the spray holes 21 of the spray header 2, the gas can be further mixed, so that the uniformity of the gas is further improved;
2) the gas flow rate is faster. When passing through the spray header 2, the gas has an obvious speed increase after passing through the spray header 2 due to the sudden reduction of the pipe diameter. By controlling the size and number of the apertures 21 of the shower head 2, different speed differences can be achieved. When the velocity difference is large, the gas to be reacted is "sprayed" vertically directly onto the growth substrate.
3) The gas viscosity state changes near the substrate. In conventional CVD, the predominant diffusion flow that typically participates in vapor deposition is diffusion of vapor phase molecules into the viscous layer near the substrate by diffusion, while reaction products and some partially reacted products such as ∙ CH3 are also in the viscous layer and may re-adsorb onto the catalyst causing catalyst poisoning. The invention uses the 'spraying' mode and is matched with the low-pressure environment, so that the thickness of the viscous layer can be greatly reduced, incomplete reaction products can be quickly separated from the substrate, and the activity time of the catalyst is prolonged.

Claims (5)

1. A vertical spraying device for spraying type gas inlet CVD is characterized in that: the device comprises a spray pipe (1) and a spray head (2), wherein the spray head (2) is fixed at the lower end part of the spray pipe (1), the middle section of the spray pipe (1) is a preheating zone (11) with a spiral pipe structure, and a spray hole (21) is formed in a bottom plate of the spray head (2).
2. The vertical shower apparatus for spray-type inlet gas CVD as claimed in claim 1, wherein: the inner diameter of the preheating zone (11) is smaller than the inner diameter of the upper section of the spray pipe (1), the inner diameter of the preheating zone (11) is smaller than the inner diameter of the lower section of the spray pipe (1), and the inner diameters of the upper section and the lower section of the spray pipe (1) are equal.
3. The vertical shower apparatus for spray-type inlet gas CVD as claimed in claim 2, wherein: an installation disc (3) is fixed on the excircle of the upper section of the spray pipe (1).
4. The vertical shower apparatus for spray-type inlet gas CVD as claimed in claim 1, wherein: in the direction from top to bottom, the inner diameter of the spray header (2) is gradually increased.
5. The vertical shower apparatus for spray-type inlet gas CVD as claimed in claim 1, wherein: the sum of the cross sectional areas of the spraying holes (21) is smaller than the area of the inlet end of the spraying pipe (1).
CN202010542458.5A 2020-06-15 2020-06-15 Vertical spraying device for spraying type gas inlet CVD Pending CN111560604A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010542458.5A CN111560604A (en) 2020-06-15 2020-06-15 Vertical spraying device for spraying type gas inlet CVD

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010542458.5A CN111560604A (en) 2020-06-15 2020-06-15 Vertical spraying device for spraying type gas inlet CVD

Publications (1)

Publication Number Publication Date
CN111560604A true CN111560604A (en) 2020-08-21

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115676805A (en) * 2021-07-26 2023-02-03 北京大学 Single-walled carbon nanotube horizontal array and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1904136A (en) * 2005-07-25 2007-01-31 精工爱普生株式会社 Method of forming film, patterning and method of manufacturing electronic device using thereof
CN101560650A (en) * 2009-05-15 2009-10-21 江苏大学 Multiple spray header chemical vapor deposition reaction chamber structure
US20110277681A1 (en) * 2009-03-03 2011-11-17 Chantal Arena Gas injectors for cvd systems with the same
CN212713746U (en) * 2020-06-15 2021-03-16 无锡盈芯半导体科技有限公司 Vertical spraying device for spraying type gas inlet CVD

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1904136A (en) * 2005-07-25 2007-01-31 精工爱普生株式会社 Method of forming film, patterning and method of manufacturing electronic device using thereof
US20110277681A1 (en) * 2009-03-03 2011-11-17 Chantal Arena Gas injectors for cvd systems with the same
CN101560650A (en) * 2009-05-15 2009-10-21 江苏大学 Multiple spray header chemical vapor deposition reaction chamber structure
CN212713746U (en) * 2020-06-15 2021-03-16 无锡盈芯半导体科技有限公司 Vertical spraying device for spraying type gas inlet CVD

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115676805A (en) * 2021-07-26 2023-02-03 北京大学 Single-walled carbon nanotube horizontal array and preparation method thereof

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