Growing technique of single-crystal silicon from melt

FIELD: metallurgy, crystals.

SUBSTANCE: invention concerns field of semiconducting materials metallurgy and can be used mainly at receiving of substances crystals with fusion temperature, increasing quartz softening temperature, for instance at growing of single-crystal silicon by means of Czochralski growth technique. Method includes location of quartz crucible in compound support, formed by cylinder course and disk, feed stock charging into quartz crucible, mounting of crucible with support into furnace, charging melting, single-crystal seed introduction and single crystal withdrawal from the melt. In particular technique cylinder course is implemented in the form of glass, bottom of which is formed by means of location at support disk layer of the same material, from which it is made cylinder part of course, crucible is located in course with ability of sliding, crucible is installed into furnace in a way that crucible bottom is in area of maximal heating. Melting mode is specified, providing reliable softening of spherical bottom-most part of quartz crucible, crucible is held till melting of charging material, then it is pulled down inside of furnace in position of growing process start and there is fixed single crystal growing mode.

EFFECT: decreasing of cost price of single-crystal silicon at the expense of crucible durability increasing and ability of it multiple additional charging by initial raw materials.

4 cl, 3 dwg

 

The invention relates to the metallurgy of semiconductor materials and can be used mainly in obtaining crystals of substances with a melting point higher than the softening temperature of quartz, for example, when growing silicon single crystals by the Czochralski method.

Typically, the single crystal growth of silicon is performed with the use of quartz crucibles. Today in installations for growing silicon single crystals they found the widest application. A common shortcoming of quartz crucibles is that at the melting temperature of silicon they are softened, the material enters into the chemical reaction between silicon and graphite stand. It violates the integrity of the structure of the quartz crucible, the crucible is destroyed, it crumbles the inner surface of the crucible loses its shape and quickly becomes unusable in the process of growing. Violation of the integrity of the crucible in the presence of molten silicon can lead to an emergency situation. Therefore, to maintain the shape of the quartz crucible during crystal growing, preserving the integrity of the melting device with the crucible during cooling after the process of cultivation and to increase the service life of the crucibles used RA is personal devices.

A method of obtaining single-crystal silicon that is implemented using a device in which to provide rigid fixation of the shape of the quartz crucible using a grid of carbon fiber, hardened by pyrocarbon (see A.S. USSR №1424379, op. 05.09.1990, IPC5SW 15/10). The crucible is placed inside a grid in the form of reinforcement, fixing the form of the crucible. However, the presence of the grid does not prevent changing the geometrical shape of the crucible and its destruction in the process of growing the single crystal due to the fact that the softened material of the crucible under the action of the melt is extruded into the voids of the mesh, which ultimately leads to the destruction of the crucible and the possible loss of the molten silicon.

A method of obtaining single-crystal silicon using complex crucible in which to avoid destruction on its inner wall cause the protective coating, produced from grain synthetic crystalline quartz (see France application No. 2461028, IPC SW 15/10). However, such a protective coating is a source of contamination of the material melt and negatively affects the quality of grown crystals.

A known method of growing silicon single crystals from the melt using a quartz crucible placed inside a graphite base, rigidly fixed on the rod (see RF patent is the 2114938, op. 10.07.1998, IPC6SW 15/10). To eliminate deformation of the quartz crucible and the graphite base, the crucible is placed with the formation of a gap between them which is filled with a layer of filling of the powder of silicon carbide thickness, locally changing in accordance with the height of the crucible.

This solution does not fully ensures the integrity of the crucible during cooling after the process because of the uncertainty of the magnitude of the gap between the quartz crucible and the graphite support.

Closest to the claimed technical solution is the method of growing silicon single crystals from the melt, in which the quartz crucible is placed in a graphite base that perform compound in the form of upper and lower disks and shells (see RF patent №2241080, op. 27.11.2004, IPC7SW 15/10). In the crucible download source raw materials, establish the crucible with stand in thermal unit, carry out the fusion download, introduction crystal seed and pulling the crystal from the melt. After completion of the process of growing produce uploading crucible, and the growing process is repeated.

This method due to the melting device ensures high performance of growing single crystals of silicon. Shell ensures the preservation of the geometric dimensions of the quartz TIG is I am in the process of growing, the integrity of the crucible during cooling after the process of growing, easy disassembly when replacing the quartz crucible with residue of silicon on a new crucible and used repeatedly. This method allows for the uploading of the crucible to 2-3 times, but no more. In the process disrupted the integrity of the structure of the quartz crucible, the crucible is destroyed, crumbling its inner surface, and the crucible becomes unusable in the process of cultivation.

The objective of the invention is to increase the service life of the crucible, the possibility of repeated loading and, consequently, reducing the cost of silicon single crystals, and the technical result is the elimination of voids between the outer surface of the crucible and the inner surface of the base due to more complete mating surfaces of the quartz crucible and shell, as well as the reduction of destructive chemical reactions between the material of the crucible and the material of the stand.

The solution of the problem and the technical result is achieved by the fact that in the proposed method of growing silicon single crystals from the melt, including the placement of the quartz crucible in the composite base formed by a cylindrical shell made of a material allowing the formation and compatible with the process grow the Oia, and a disk mounted coaxially with each other, the loading raw material into a quartz crucible, the installation of the crucible with stand in thermal unit, the meltdown download, introduction monocrystalline seed crystal and the pulling of the single crystal from the melt, the sides are in the form of glass, the bottom of which is formed by placing the disk coasters layer of the same material, which is made cylindrical part of the shell. The crucible is placed in the ring slidable along the axis, then set the crucible with stand in thermal unit so that the bottom of the crucible was in the zone of maximum heating, set the melting operation, providing a strong softening of the spherical bottom of the quartz crucible can withstand the crucible to melt the material of the boot, then lower the heat inside of the node in the position of the beginning of the cultivation process and establish a regime of growing the single crystal.

In the proposed method the shell is fixed around the crucible through the rings of a composite material.

This ring features a round shell with the crucible in an elliptical circles, excluding their mutual intersection.

As the material of the shell using the foil of width of graphite.

Running shells in the form of a Cup, the bottom of which is formed by placing on the NEC stand layer of the same material, which is made cylindrical part of the shell, isolates from contacting the bottom of the quartz crucible and the graphite surface of the disc stand. This decreases the intensity of chemical reactions between the material of the crucible and the material of the base, destroying the structural integrity of the quartz crucible during repeated use of the crucible in the processes of cultivation.

The crucible is placed in the ring slidable along the axis to ensure that in the process of softening the spherical bottom of the quartz crucible and the shutter speed of the crucible to melt the material download the crucible without stress filled all the voids between the outer surface of the crucible and the inner surface of the base due to more complete mating surfaces of the quartz crucible and shell in the shape of the glass.

Installation of the crucible with stand in thermal unit so that the bottom of the crucible was in the zone of maximum heating, provides in the process of melting operation softening of the spherical bottom of the quartz crucible, resulting in under the weight of the crucible and melt the shape of the crucible is fully mated with the shape of the shell. Thus, when lowering of the crucible to heat the node at the position of the beginning of the growth process, the surface of the quartz crucible and shell in the shape of the glass is fully coupled, which allows you to keep multiple use is the use of the crucible integrity of its structure, transparency and the original smooth internal and external surfaces. The crucible remains usable in the process of growing during multiple uploading.

The shell is fixed around the crucible through the rings of composite material that is compatible with the growth process, to ensure structural integrity in the form of shells and the crucible with the melt. The arrangement of the rings around the shell with the crucible in an elliptical circles, excluding their mutual intersection, makes it easy to ensure when assembling placing the crucible in the ring with the possibility of sliding down along the axis under the action of gravity. This is achieved by the fact that the internal diameter of the rings is slightly greater than the external diameter of the shell with the crucible and the offset plane of the rings around the shell with a crucible provided with appropriate planting density of the crucible in the ring. Ring of composite material with this shift are arranged in an elliptical circles without overlap.

Using as the material of the shell, made in the form of glass, foil width of graphite provides compatibility of materials in the process of growing silicon single crystals, the necessary rigidity and good contact of the shell with the crucible.

These benefits before the its method can significantly increase the service life of the crucible, the possibility of repeated loading and, consequently, to reduce the cost of silicon single crystals by reducing the specific consumption of crucibles required for growing units suitable products, and reducing energy costs

The essence of the invention is illustrated by drawings.

1 schematically shows a General view of the camera to grow with the image of the elements of the device, the required disclosure of the nature of the proposed method.

Figure 2 shows an enlarged fragment of the mating surfaces of the crucible and shell at the time of installation of the crucible with stand in thermal unit, in which the bottom of the crucible is in the zone of maximum heating.

Figure 3 shows an enlarged fragment of the mating surfaces of the crucible and shell after carrying out the melting operation, providing a strong softening of the spherical bottom of the quartz crucible and melting of the material of the boot.

1 shows a quartz crucible 1 is placed inside a graphite composite coasters, made in the form of the upper disk 2, the lower disk 3 and the shell 4, installed coaxially to each other. The shell 4 is formed in the shape of the glass, the bottom of which 5 are formed by placing on the top disc 2 coasters layer of the same material, which is made cylindrical part of the shell 4 of the Cylindrical part of the shell 4 is fixed around the quartz crucible 1, for example, with three rings 6, which are evenly spaced along the height of the quartz crucible 1 in an elliptical circles. The ends of the rings 6 are connected by brackets (not shown). The lower disk 3 is rigidly fixed to the rod 7. The upper disk 2 having a larger diameter than the lower disk 3 made can be locked relative to the lower disk and the crucible with the cowling. Figure 1 also shows the heater 8. Arrows mark the zone of maximum heating. For placement in thermal unit and taking out the quartz crucible 1, together with the removable part of the graphite stand can be used lifting device 9 in the form of a ring, on which are mounted rotatably bars with bends.

The proposed method is as follows.

When growing silicon single crystals with a given diameter dm=152.5 mm in its cylindrical part of the quartz crucible 1 of diameter D=356 mm and height H=240 mm set slidable in a graphite base. The removable part of the cradle perform compound, consisting of shell 4 and the disk 2. Shell is a nozzle of diameter d=356+1mm, a cylindrical portion 4 which is made of graphite foil, for example a foil of width of graphite (foil TWG), and the bottom 5 is formed by a layer of the same material from which made Qili the shape part of the shell, posted by on disk 2 of the graphite base. Foil width of graphite has good capacity for shaping and perfectly compatible with the process of growing single crystals. The shell is fixed around the crucible with three rings 6 of the composite material, reusable covering the crucible in an elliptical circles, excluding their mutual intersection. The cylindrical surface of the crucible is fixed sides and you can still slide the side surfaces of the crucible along the shell. Pot load of polycrystalline silicon (loading weight is 30 kg) with a ligature. Stand with a crucible installed inside the heater 8 using the tool 9 in the position corresponding to the initial position of the cultivation process. With the rod 7 raise the crucible to a height of h=135 mm relative to the original position of the cultivation process, the bottom of the quartz crucible is located in the zone of maximum heating. Carry out the sealing of the camera, install the supply of inert gas (argon) flow rate 20 l/min and the evacuation of the gas mixture (Ar, SiO) from the camera. Ask the melting operation, by setting the heating power corresponding to the current I=1800 A, which is 50-60% higher than the capacity for growing the single crystal. This power is here in 30 minutes provides a strong softening of the quartz, the melting of the load and the temperature of the melt 10% higher than the melting point of polycrystalline silicon.

This softened the spherical bottom part of the crucible under its own weight and the weight of the melt loading due to the sliding fit of the crucible in a cylindrical shell, completely fills all the emptiness before heating, between the crucible and shell.

After that, the crucible is lowered into thermal zone in the position of the beginning of the cultivation process and the process of growing the single crystal.

At the end of the process of growing produce uploading crucible, weighing 25-30 kg Newly loaded quartz crucible with a drum and a graphite disk is placed lifting fixture to its original position and the growing process is repeated.

Described is a method of growing single crystals can significantly increase the resource of the quartz crucible (200 hours) and allows multiple (5-10) uploading of the crucible.

Known methods of growing single crystals of silicon and the method adopted for the prototype, allow 2-3 times to make uploading of raw materials, and the proposed method due to the technological preparation of the crucible to the growth process increases the life of the quartz crucible and allows uploading of its raw materials 5-10 times. The crucible retains its robotos osobnosti within 150-250 hours.

The proposed method is used to obtain positive results for the typical range of diameters dmsingle crystals 100, 150, 200 mm and diameter D of the crucibles 270, 330, 356, 406, 457 615 mm Cost of obtaining suitable products (dislocation single crystal silicon with the specified technical characteristics) reduced compared to the prototype in average by 20%.

Thus, the proposed method of growing silicon single crystals from the melt allows to reduce the cost of silicon single crystals by increasing the service life of the crucible, the possibility of its repeated re-loading the raw material and lowering the unit cost of electricity.

1. The method of growing silicon single crystals from the melt, including the placement of the quartz crucible in the composite base formed by a cylindrical shell made of a material allowing the formation and compatible with the process of growing, and the disk, the loading raw material into a quartz crucible, the installation of the crucible with stand in thermal unit, the meltdown download, introduction monocrystalline seed crystal and the pulling of the single crystal from the melt, characterized in that the sides are in the form of glass, the bottom of which is formed by placing the disk coasters layer of the same material from which made cilindri the definition part of the shell, place the crucible in the ring with a slidable, set the crucible in the heating unit so that the bottom of the crucible was in the zone of maximum heating, set the melting operation, providing a strong softening of the spherical bottom of the quartz crucible can withstand the crucible to melt the material of the boot, then lower the heat inside of the node in the position of the beginning of the cultivation process and establish a regime of growing the single crystal.

2. The method of growing silicon single crystals from the melt according to claim 1, characterized in that the shell is fixed around the crucible through the rings of a composite material.

3. The method of growing silicon single crystals from the melt according to claim 2, characterized in that the rings have around the shell with the crucible in an elliptical circles, excluding their mutual intersection.

4. The method of growing silicon single crystals from the melt according to claim 1, characterized in that the material of the shell using the foil of width of graphite.



 

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1 dwg

The invention relates to methods of obtaining crystals of substances with a melting point higher than the softening temperature of quartz, for example silicon for the semiconductor industry by Czochralski method

The invention relates to the cultivation of the melt bulk single crystals of sapphire and are aimed at increasing the service life of structural elements

The invention relates to a device for growing crystals and method of growing crystals
The invention relates to the metallurgy of semiconductor materials and can be used in the design of the melting device for growing crystals from the melt, mainly silicon

The invention relates to single crystal growth by the Czochralski method

FIELD: devices for continuous grouped growing of the orientated layers of silicon on a carbonic fabric.

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EFFECT: the invention ensures growing of polycrystallic layers from a melt of silicon.

1 dwg

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