Narrow flow induction coupling chemical vapor deposition (CVD) densification method for rapidly preparing carbon/carbon composite material crucible

A carbon composite material and inductively coupled technology, applied in the field of narrow-flow inductively coupled CVD densification, can solve the problems of low densification efficiency, long preparation cycle, and high manufacturing cost

Active Publication Date: 2013-07-10
山东道普安制动材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the existing CVD technology has the disadvantages of low densification efficiency and long production cycle, or a single furnace can only process a single product, resulting in high manufacturing costs, which limits the applic...

Method used

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  • Narrow flow induction coupling chemical vapor deposition (CVD) densification method for rapidly preparing carbon/carbon composite material crucible

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] A carbon / carbon composite crucible for pulling silicon single crystal material was prepared, the crucible size was Φ500×450mm.

[0039] (1) Put the carbon fiber braided crucible preform, inductive coupling tooling, and airflow tool in the reaction chamber of the vacuum induction deposition furnace. The crucible preform is sleeved on the inductive coupling tooling, and then covered with the airflow tooling, the preform and the inductive coupling tooling, The gas flow tooling is matched to form a 50mm wide gas flow channel and the whole inner surface of the crucible preform cylinder section is inductively coupled;

[0040] The inductive coupling tool is a coupling graphite core, and the air flow tool is made of electrode graphite.

[0041] (2) Increase the temperature and vacuum, when the temperature reaches 950℃, the vacuum degree is 1000Pa, and the temperature is kept for 20min;

[0042] (3) Then use nitrogen as the protective dilution gas, press propylene: N 2 =1:1 volume rati...

Embodiment 2

[0045] Example 2. Preparation of a carbon / carbon composite crucible for purifying and smelting polysilicon, the crucible size is Φ600×600mm.

[0046] (1) Place the carbon fiber cloth mesh needle-punched crucible preform and tooling in the reaction chamber of the vacuum induction deposition furnace. The preform is matched with the induction coupling tooling and airflow tooling to form a 30mm wide gas flow channel and the crucible barrel section for inductive coupling on the entire inner surface ;

[0047] (2) Increase the temperature and vacuum, when the temperature reaches 1250℃, the vacuum degree is 2000Pa, and the temperature is kept for 30min;

[0048] (3) Then use nitrogen as the protective diluent gas, press methane: N 2 =2:1 volume ratio of methane and N 2 The gas flows into the reaction chamber of step (1), N 2 The air flow is 1000ml / min, the aeration infiltration reaction is 120h, and the carbon matrix is ​​formed by in-situ pyrolysis and deposition;

[0049] (4) After cooling...

Embodiment 3

[0051] Example 3. A carbon / carbon composite crucible for polycrystalline silicon ingots was prepared, the crucible size was 800×800×600 mm.

[0052] (1) Place the carbon fiber cloth laminated crucible preform and tooling in the reaction chamber of the vacuum induction deposition furnace. The preform is matched with the inductive coupling tooling and airflow tooling to form a 10mm wide gas flow channel and the crucible barrel section for inductive coupling on the entire inner surface;

[0053] (2) Heat up and vacuum, when the temperature reaches 1150℃, keep the temperature for 30min under the condition of 4000Pa vacuum;

[0054] (3) Then use nitrogen as the protective dilution gas, press liquefied petroleum gas: N 2 =1:2 volume ratio will be liquefied petroleum gas and N 2 The gas flows into the reaction chamber of step (1), N 2 The air flow is 3000ml / min, the aeration permeation reaction is 180h, and the carbon matrix is ​​formed by in-situ pyrolysis and deposition;

[0055] (4) After...

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Abstract

The invention relates to a narrow flow induction coupling chemical vapor deposition (CVD) densification method for rapidly preparing a carbon/carbon composite material crucible. The method comprises the steps of: adopting a chemical vapor deposition technology, under the synergistic effect of narrow slit airflow and inductive coupling, leading mixed gas of small-molecule hydrocarbon and N2 gas to a high-temperature reaction chamber, adsorbing the small-molecule hydrocarbon at the surface of an inner hole of a carbon fiber crucible precast body or a low-density carbon/carbon composite material crucible billet body, and releasing pyrolytic carbon at a high temperature, depositing the pyrolytic carbon at the surface of a hot carbon fiber, continuously improving the density of the billet body, and rapidly obtaining the compact carbon/carbon composite material crucible. By adopting the method disclosed by the invention, the crusting phenomenon of the surface is effectively restrained under the synergistic effect of narrow slit airflow and inductive coupling measures; high deposition temperature and reaction gas furnace pressure are permitted; inner and outer balanced densification is more rapidly carried out; the quality is improved; the cycle is shortened; and the cost is also reduced.

Description

Technical field [0001] The invention relates to a narrow-flow induction coupling CVD densification method for rapidly preparing a carbon / carbon composite material crucible, belonging to the field of chemical vapor deposition. technical background [0002] Carbon fiber reinforced carbon-based composite material (referred to as carbon / carbon, C / C) is a composite material made of carbon or graphite fiber as the reinforcement and carbon or graphite as the matrix. It has special properties such as high temperature resistance, good thermal conductivity, thermal shock resistance, low ablation rate, high strength at high temperature, and certain chemical inertness. It is an ideal high-temperature structure, high-temperature friction, high-temperature electrical heating and anti-ablation material. In recent years, with the reduction of carbon fiber raw materials and manufacturing costs, the application of C / C composite materials is gradually entering the industrial field from the aerospac...

Claims

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Application Information

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IPC IPC(8): C04B35/83C04B35/622
Inventor 刘汝萃刘汝强
Owner 山东道普安制动材料有限公司
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