The tungsten crucible trimming device of long crystal furnace use and method
Technical field
The present invention relates to the technical field of quasiconductor and LED, especially and the tungsten crucible trimming device of long crystal furnace use and method.
Background technology
At present, during artificial gem produces, the crucible material being used for carrying raw material is mainly tungsten, fusing point high (more than 3400 DEG C) due to tungsten, there is good elevated temperature strength, molten alkali metal and steam there are is good corrosion resisting property, is used for the raw material carrier as artificial gem produces and is quite suitable for.
The manufacturing process of tungsten crucible mainly uses tungsten powder charging pressing mold molding, and through high temperature sintering, this kind of processing procedure is in Material Manufacturing Process and non-fusible material, just it is not afraid of and is mixed into the impurity brought by crucible and deoxidizer etc. yet, and sinter and be typically in vacuum and reducing atmosphere to carry out, it is not afraid of oxidation, without to any pollution of material, and can guarantee that correctness and the uniformity of material composition proportioning.
But due in use procedure, tungsten there will be oxide volatilization more than 1000 DEG C, this can cause tungsten wall thinning because of access times gradually, and be thinned to after to a certain degree, its heat insulation effect can be deteriorated, affect again the ability of heater material, cause that heater must provide for higher power, and this part can cause the loss of energy consumption. And tungsten crucible is after repeated, due to the hole problem that volatilization causes, can cause that it is brittle, the problem easily causing tungsten crucible cracking, and then cause that life cycle shortens, and production cost increases.
Summary of the invention
For above-mentioned problem, the present invention provides a kind of tungsten crucible trimming device and the method for long crystal furnace use, to repair because reusing thinning tungsten crucible, allows thinning sidewall of crucible thicken, replys the heat insulation effect of its script, the problem reducing energy consumption.
In order to reach above-mentioned purpose, the solution of the present invention is:
The tungsten crucible trimming device of long crystal furnace use, including reative cell, heater and reaction trachea; Reative cell tool CVD (chemicalvapordeposition chemical vapour desposition) cavity, the reaction trachea installed above of reative cell, one end of reaction trachea stretches at CVD cavity outer for connecting air supply pipe, and the other end reacting trachea stretches in CVD cavity and offers some pores on this end, waste discharge mouth is offered in the lower section of reative cell, and waste discharge mouth is connected to pump by pipeline; Heater is placed in CVD cavity, and heater is arranged on the pillar rotated by driven by motor, and heater has the articles holding table for crucible rotation.
The other end of described reaction trachea is inverted T shape, and the transverse tube of inverted T shape and vertical tube are all offered some pores.
Described reative cell is also installed RF power generator.
The tungsten crucible method for trimming of long crystal furnace use, its step is as follows:
The first step, puts into the crucible that need to repair in the CVD cavity of reative cell, and is placed on the articles holding table of heater;
Second step, contains WF at the crucible that need to repair6, and the other end of reaction trachea is stretched into WF6In, make the pore on reaction trachea be immersed in WF6In;
3rd step, by CVD cavity evacuation, to 100Pa P 0.1MPa;
4th step, heats heater to 600~800 DEG C;
5th step, is supplied SiH by reaction trachea to CVD cavity4, make gas SiH4With WF6Reaction, produces tungsten deposition thin film and repairs tungsten crucible;
6th step, takes unreacted gas and side-product away by vacuum pump, cleans CVD cavity;
7th step, delivers to annealing furnace by the tungsten crucible after repairing, and launches high temperature (> 2100 DEG C) annealing, namely completes finishing.
Described 6th step, uses Ar and N2It is filled with CVD cavity, relends and help vacuum pump to take unreacted gas and side-product away.
After adopting such scheme, the present invention repairs because reusing thinning tungsten crucible by chemical vapour deposition (CVD) (CVD), it is possible not only to allow W atom enter crucible and fills up the hole because volatilization causes, reduce the chance of sidewall of crucible cracking, substantially prolongs life cycle, simultaneously, thinning sidewall of crucible is allowed to thicken, replying its heat insulation effect originally, the problem reducing energy consumption, production cost reduces.
Accompanying drawing explanation
Fig. 1 is the structural representation of apparatus of the present invention.
Detailed description of the invention
As it is shown in figure 1, present invention is disclosed the tungsten crucible trimming device of long crystal furnace use, including reative cell 1, heater 2 and reaction trachea 3.
Reative cell 1 has CVD (chemicalvapordeposition chemical vapour desposition) cavity.
The reaction trachea 3 installed above of reative cell 1, one end of reaction trachea 3 stretches at CVD cavity outer for connecting air supply pipe (ordinary elements, not shown), and the other end reacting trachea 3 stretches in CVD cavity and offers some pores 31 on this end. In order to reach optimum response effect, the other end of reaction trachea 3 is inverted T shape, and the transverse tube of inverted T shape and vertical tube are all offered some pores 31. Waste discharge mouth 11 is offered in the lower section of reative cell 1, and waste discharge mouth 11 is connected to pump (ordinary elements, not shown) by pipeline.
Heater 2 is placed in CVD cavity, and heater 2 is arranged on the pillar 21 being rotated by motor (ordinary elements, not shown), and heater 2 has the articles holding table rotated for crucible 5. Rotated by heater 2, the surface of crucible when making tungsten grow up, can be deposited on uniformly, promote the tungsten chemical vapor deposition uniformity.
Can also installing RF power generator 4 on reative cell 1 further, this RF power generator 4 is prior art device, so, forms alternating electric field in cavity, and under the effect of alternating electric field, gaseous volatilization electric discharge is in plasma state, promotes finishing effect.
The tungsten crucible method for trimming of long crystal furnace use, its step is as follows:
The first step, puts into the crucible that need to repair in the CVD cavity of reative cell, and is placed on the articles holding table of heater;
Second step, contains WF at the crucible that need to repair6, and the other end of reaction trachea is stretched into WF6In, make the pore on reaction trachea be immersed in WF6In;
3rd step, by CVD cavity evacuation, to 100Pa P 0.1MPa;
4th step, heats heater to 600~800 DEG C;
5th step, is supplied SiH by reaction trachea to CVD cavity4, make gas SiH4With WF6Reaction, produces tungsten deposition thin film and repairs tungsten crucible;
Concrete reaction is as follows:
SiH4Reaction during immersion: SiH4→Si+H2
During nucleation: SiH4+WF6→W+SiH4+HF
Si+WF6→W+SiH4
During large quantities of deposit: WF6+H2→W+HF
6th step, uses Ar and N2It is filled with CVD cavity, relends and help vacuum pump to take unreacted gas and side-product away, clean CVD cavity;
7th step, delivers to annealing furnace by the tungsten crucible after repairing, and launches high temperature (> 2100 DEG C) annealing, namely completes finishing.