Method of manufacturing silicon single crystal, apparatus for pulling silicon single crystal and vitreous silica crucible
Leakage of silicon melt is monitored and touch of a seed crystal at the silicon melt is detected, and in addition, reinforcement of a vitreous silica crucible to be endurable during pulling for a long time and decrease of impurity concentration of a silicon single crystal can be expected. A method for manufacturing a silicon single crystal is provided. The method includes: detecting touching status of a seed crystal at silicon melt by supplying voltage V 1 using a crucible side as a negative electrode and a wire side as a positive electrode and by monitoring change of the voltage, when the seed crystal provided at a front end of the wire touches the silicon melt inside a vitreous silica crucible; devitrifying an inner surface of the vitreous silica crucible as supplying voltage V 2 using the crucible side as a positive electrode and the wire side as a negative electrode during a temperature control period; and growing a silicon single crystal by slowly pulling the seed crystal as supplying voltage V 3 using the crucible side as a negative electrode and the wire side as a positive electrode after the temperature control period.
1. A method of manufacturing a silicon single crystal comprising:
detecting touching status of a seed crystal at silicon melt by supplying a first voltage using a vitreous silica crucible side as a negative electrode and a pulling shaft side as a positive electrode and by monitoring change of the first voltage, when the seed crystal provided at a front end of the pulling shaft touches the silicon melt inside a vitreous silica crucible;
devitrifying an inner surface of the vitreous silica crucible as supplying a second voltage greater than the first voltage using the vitreous silica crucible side as a positive electrode and the pulling shaft side as a negative electrode during a temperature control period of the silicon melt, the temperature control period being a certain period after the touch of the seed crystal at the silicon melt; and
growing a silicon single crystal by slowly pulling the seed crystal as supplying a third voltage smaller in absolute value than the second voltage using the vitreous silica crucible side as a negative electrode and the pulling shaft side as a positive electrode after the temperature control period.
2. The method of claim 1 , wherein the growing of the silicon single crystal further comprises reproducing a devitrified portion of the inner surface of the vitreous silica crucible by supplying a fourth voltage greater in absolute value than a third voltage for a certain period before the devitrified portion formed at the inner surface of the vitreous silica crucible disappears.
3. The method of claim 2 , wherein in the growing of the silicon single crystal, the supplying of the third voltage and the supplying of the fourth voltage are alternately repeated.
4. The method of claim 1 , wherein leakage of the silicon melt is detected by monitoring changes of the first to third voltages.
5. The method of claim 1 , wherein the vitreous silica crucible comprises one or at least two alkali metals selected from the group consisting of Na, K and Li, and a sum of concentrations of the alkali metals is equal to or greater than 0.05 ppm.
6. An apparatus for pulling a silicon single crystal, the apparatus comprising a pulling shaft, an elevator unit of the pulling shaft, a seed crystal provided at a front end of the pulling shaft, a vitreous silica crucible filled with silicon melt, a heater heating the silicon melt inside the vitreous silica crucible, a power supply supplying a voltage between the vitreous silica crucible and the pulling shaft, and a controller controlling the elevator unit, the heater and the power supply,
wherein the controller comprises:
a touch control part detecting touching status of the seed crystal at the silicon melt by supplying a first voltage using the vitreous silica crucible side as a negative electrode and the pulling shaft side as a positive electrode and by monitoring change of the first voltage, when the seed crystal touches the silicon melt by lowering the pulling shaft;
a devitrification control part devitrifying an inner surface of the vitreous silica crucible as supplying a second voltage greater than the first voltage using the vitreous silica crucible side as a positive electrode and the pulling shaft side as a negative electrode during a temperature control period of the silicon melt, the temperature control period being a certain period after the touch of the seed crystal; and
a single crystal control part growing a silicon single crystal by slowly pulling the seed crystal as supplying a third voltage smaller than the second voltage using the vitreous silica crucible side as a negative electrode and the pulling shaft side as a positive electrode after the temperature control period.
7. A vitreous silica crucible having a cylindrical sidewall part, a bottom part provided at a lower portion of the sidewall part, and a joining section provided between the sidewall part and the bottom part, the vitreous silica crucible being used for pulling a silicon single crystal in a state that a predetermined voltage is supplied with respect to a thickness direction of the crucible, the vitreous silica crucible comprising:
a transparent vitreous silica layer provided on an inner surface of the crucible; and
an opaque vitreous silica layer provided on an outer surface of the crucible, and including a plurality of bubbles,
wherein the opaque vitreous silica layer comprises one or at least two alkali metals selected from the group consisting of Na, K and Li, and a sum of concentrations of the alkali metals is equal to or greater than 0.05 ppm.
8. The vitreous silica crucible of claim 7 , wherein a sum of concentrations of the alkali metals comprised in the opaque vitreous silica layer is equal to or greater than 0.2 ppm.
9. The vitreous silica crucible of claim 7 , wherein the transparent vitreous silica layer comprises one or at least two alkali metals selected from the group consisting of Na, K and Li, and a sum of concentrations of the alkali metals is equal to or greater than 0.05 ppm and equal to or less than 5 ppm.
10. The method of claim 2 , wherein leakage of the silicon melt is detected by monitoring changes of the first to third voltages.
11. The method of claim 3 , wherein leakage of the silicon melt is detected by monitoring changes of the first to third voltages.
12. The method of claim 2 , wherein the vitreous silica crucible comprises one or at least two alkali metals selected from the group consisting of Na, K and Li, and a sum of concentrations of the alkali metals is equal to or greater than 0.05 ppm.
13. The method of claim 3 , wherein the vitreous silica crucible comprises one or at least two alkali metals selected from the group consisting of Na, K and Li, and a sum of concentrations of the alkali metals is equal to or greater than 0.05 ppm.
14. The method of claim 4 , wherein the vitreous silica crucible comprises one or at least two alkali metals selected from the group consisting of Na, K and Li, and a sum of concentrations of the alkali metals is equal to or greater than 0.05 ppm.
15. The method of claim 10 , wherein the vitreous silica crucible comprises one or at least two alkali metals selected from the group consisting of Na, K and Li, and a sum of concentrations of the alkali metals is equal to or greater than 0.05 ppm.
16. The method of claim 11 , wherein the vitreous silica crucible comprises one or at least two alkali metals selected from the group consisting of Na, K and Li, and a sum of concentrations of the alkali metals is equal to or greater than 0.05 ppm.
17. The vitreous silica crucible of claim 8 , wherein the transparent vitreous silica layer comprises one or at least two alkali metals selected from the group consisting of Na, K and Li, and a sum of concentrations of the alkali metals is equal to or greater than 0.05 ppm and equal to or less than 5 ppm.