JP3640454B2 - Single crystal manufacturing method - Google Patents

Description

[0001]
[Industrial application fields]
The present invention relates to a manufacturing method for manufacturing a plate-shaped single crystal in a space in a partition body by installing a partition body including at least one partition plate in a crucible.
[0002]
[Prior art]
Conventionally, as a method for producing a single crystal of metal, oxide or semiconductor, a seed crystal (seed) is put in the raw material melt, and the Czochralski method of pulling up the single crystal attached to this seed crystal, In addition to the boat method in which the raw material is put into a cylindrical vertical or horizontal boat and melted to lower the temperature of the melt from the bottom of the boat to grow crystals in the boat, the horizontal or vertical Bridgman method In addition, a vertical and horizontal gradient freeze method called a VGF or HGF method is known.
[0003]
Most of the single crystals obtained by these production methods are bulk single crystals along the diameter of the crucible. By slicing the obtained single crystals, a plate-like body having a desired thickness can be obtained. Was the usual method.
[0004]
[Problems to be solved by the invention]
As described above, in the conventional method, since a plate material having a desired shape is sliced from the obtained bulk single crystal, a certain amount of time is required for the process, and depending on the object, for example, GaAs is used. There was a drawback that generation of residues such as harmful semiconductors was inevitable.
[0005]
An object of the present invention is to develop a novel manufacturing method and a manufacturing apparatus therefor, which can manufacture a plate-shaped single crystal having a target shape directly from a raw material, instead of the conventional method.
[0006]
[Means for Solving the Problems]
The inventors of the present invention have intensively studied to solve such a problem, and found that a single crystal having a desired thickness can be obtained by installing a partition having a specific shape in a crucible used in the conventional method. The headline and the present invention could be provided.
[0007]
That is, according to the present invention, firstly, a partition body composed of at least one partition plate is provided in a crucible , and the temperature is adjusted by a heater that is arranged around the crucible and can be changed in the heating region. A method for producing a single crystal, comprising melting , pouring the melt into a space in the partition , joining the bottom to a seed, and gradually cooling to produce a plate-like single crystal.
[0008]
In addition, the present invention secondly provides a compound semiconductor comprising at least one partition plate in a crucible and adjusting the temperature with a heater that is arranged around the crucible and capable of changing the heating region. Manufacturing a single crystal characterized by melting a raw material and a sealing material , pouring the compound semiconductor melt into a space in the partition , joining the bottom to a seed, and gradually cooling to produce a plate-shaped compound semiconductor single crystal Is the method. Further the present invention is a third, lateral shaped partition body formed of transversely parallel to each other a plurality of partition plates in the crucible is provided, and the temperature adjusted arranged heating zones variability heaters around the crucible The raw material at the upper part of the partition is melted, the melt is poured from the upper part of the crucible through a crystal connecting nozzle into the space in the partition, the bottom is joined to the seed, and cooled slowly to produce a plate-like single crystal. This is a method for producing a single crystal.
[0009]
[Action]
A conventionally known VGF method or vertical or horizontal Bridgman method can be used as means for growing a single crystal in the method of the present invention. As a crucible provided inside the apparatus, a crucible made of low-conductivity vitrocarbon (product name of glassy carbon material manufactured by Nippon Carbon Co., Ltd.) or graphite is used, and a plate-like partition made of the same material is contained in the crucible. A partition made of a partition plate is inserted vertically or horizontally.
[0010]
In this case, it suffices to have one or more partition plates, and the interval between the partition plates is set to a width of 1.5 mm in the first embodiment, but this may be adjusted to an arbitrary desired thickness. The vertical partition has a stacked structure in which a plurality of partition plates having a U-shaped cross section are stacked, and finally a flat plate is stacked, and the stacked body is installed inside the crucible.
[0011]
In addition, as shown in Example 4 as another embodiment of the partition, the partition plate is arranged in parallel in the crucible, and the molten metal is passed through the crystal communication nozzle from the upper part of the crucible and is obtained by each partition plate. The space is filled with melt.
[0012]
By using this partition, the melt obtained by melting the raw materials of copper, zinc, tin, bismuth metal and compound semiconductors such as GaAs and InAs is poured into the gap of the partition plate, and the bottom is joined to the seed. I tried to do it.
[0013]
Hereinafter, the method of the present invention and the device of the present invention will be described in detail with reference to the drawings, but the scope of the present invention is not limited thereto.
[0014]
[Example 1]
FIG. 1 shows an outline of an example of an apparatus used in the present invention. 1 is a raw material, 2 is a crucible, 3 is a seed, 4 is a sealing material, 5 is a vertical partition, 6 is an upper heater, 7 is a central heater, 8 is a lower heater, 9 is a water cooling jacket, and 10 is a heat insulating material Represents each. In a graphite crucible 2 provided in the apparatus, a vertical partition body 5 (shown in cross section in FIG. 2) formed by laminating three U-shaped partition plates and one flat plate is formed vertically. After the insertion, 100 g of 6N high-purity copper is put in the crucible 2 as the metal raw material 1, the raw material 1 on the upper part of the vertical partition 5 is melted at 1150 ° C., and the temperature of the common part between the lower part of the partition plate 5 and the seed 3 Was adjusted to 1083 ° C.
[0015]
Next, the whole crucible is gradually cooled at a rate of 50 ° C./hr, and the space inside the vertical partition 5 is 1.5 mm thick × 10 mm wide × 50 mm long as shown in FIG. 3 (partition plate not shown). Three single crystal copper plates were manufactured at the same time, and the common portion (polycrystalline portion) of the seed 3 was cut outside the crucible to obtain a desired single crystal copper plate.
[0016]
[Example 2]
As in Example 1, 100 g of 6N (99.9999%) high-purity copper as raw material 1 is put in the crucible 2, and the raw material 1 at the upper part of the vertical partition 5 is melted at 1150 ° C., and the lower part of the partition 5 is The temperature was adjusted to 1083 ° C.
[0017]
Subsequently, the crucible is pulled down at a speed of 60 mm / hr to cool down, and three single crystal copper plates of 1.5 mm thickness × 10 mm width × 50 mm length are simultaneously manufactured in the space inside the partition 5, as in Example 1. The common part (polycrystalline part) of the seed 3 was cut into a desired single crystal copper plate.
[0018]
[Example 3]
Instead of the graphite crucible in Example 1, a vitrocarbon crucible showing lower conductivity was prepared and installed in the apparatus, and 50 g of GaAs (purity 6N) and 10 g of B ₂ were used as the raw material 1 in the crucible _2. After charging O ₃ (sealing material 4), the upper part of the vertical partition 5 is set to 1280 ° C. and the lower part of the partition 5 is set to 1238 ° C. in an Ar atmosphere at a pressure 1 kg / cm ² higher than the normal pressure. Adjusted.
[0019]
Subsequently, the whole crucible was gradually cooled at a rate of 10 ° C./hr to simultaneously produce three single crystal GaAs plates 1.5 mm thick × 10 mm wide × 50 mm long in the gap of the vertical partition 5, as in Example 1. The common part (polycrystalline part) of the seed 3 was cut to obtain a desired single crystal GaAs plate.
[0020]
[Example 4]
As shown in FIG. 4, the raw material holder 11 in which a horizontal partition 13 made up of a plurality of partition plates parallel to each other in the lateral direction is placed in the crystallization apparatus used in Example 1 for crystallization. It was. In this case, 100 g of 6N high-purity copper is added as the metal raw material 1, the raw material 1 on the upper side of the horizontal partition plate 13 is melted at 1150 ° C., and the temperature of the space between the lower portion of the partition plate 13 and the seed 3 is 1083 ° C. It adjusted so that it might become.
[0021]
Next, the entire raw material holder 11 is gradually cooled at a rate of 50 ° C./hr to simultaneously produce six single crystal copper plates having a diameter of 20 mm and a thickness of 1.5 mm in a disk-shaped gap inside the horizontal partition 13, outside the holder. The desired portion (polycrystalline portion) with the seed 3 was cut to obtain a desired single crystal plate.
[0022]
【The invention's effect】
As described above, since the single crystal plate obtained by the present invention has a plate shape inside the partition body, the step of slicing the bulk crystal body into a desired shape as in the conventional method becomes unnecessary, and the present invention is The effect that contributes to cost reduction in operation is significant.
[Brief description of the drawings]
FIG. 1 is a schematic view showing a cross section of a device of the present invention.
FIG. 2 is a sectional view of a vertical partition installed in a crucible of the device of the present invention.
FIG. 3 is a perspective view of a crucible of the device of the present invention.
FIG. 4 is a transparent perspective view showing a horizontal partition installed in the crucible of the device of the present invention.
[Explanation of symbols]
1 Raw Material 2 Crucible 3 Seed 4 Sealing Material 5 Vertical Partition 6 Upper Heater 7 Center Heater 8 Lower Heater 9 Water Cooling Jacket 10 Heat Insulation Material 11 Material Holder 12 Crystal Contact Nozzle 13 Horizontal Partition 14 Seed Container

Claims (3)

A partition composed of at least one partition plate is provided in the crucible, the temperature is adjusted by a heater that is arranged around the crucible and the heating region can be changed, and the raw material in the upper part of the partition is melted to melt the melt in the partition. A method for producing a single crystal, which comprises pouring into a space and joining the bottom part to a seed and gradually cooling to produce a plate-like single crystal. A partition made of at least one partition plate is provided in the crucible , and the compound semiconductor raw material and the sealing material on the upper portion of the partition are melted by adjusting the temperature with a heater that is arranged around the crucible and capable of changing the heating region. A method for producing a single crystal, comprising: pouring the compound semiconductor melt into a space in the partition , joining the bottom to a seed, and gradually cooling to produce a plate-shaped compound semiconductor single crystal. A horizontal partition made up of a plurality of partition plates that are parallel to each other in the lateral direction is provided in the crucible , and the temperature is adjusted by a heater that is arranged around the crucible and that can change the heating region, so that the raw material at the top of the partition is melted. A method for producing a single crystal comprising producing a plate-like single crystal by pouring a melt from the upper part of the crucible through a crystal communication nozzle into a space in the partition body and joining the bottom part to a seed and gradually cooling .

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