JP2001114599A - Method of and device for producing single crystal - Google Patents

Abstract

PROBLEM TO BE SOLVED: To prevent the adhesion of a single crystal grown on the surface of a seed crystal to a polycrystal formed on the periphery of the single crystal. SOLUTION: A seed crystal-adhering member 12b is attached to the opening of a lid 12a so that the seed crystal-adhering member 12b is surrounded with the lid 12a, and the seed crystal-adhering member 12b is separated from the terminal surface of the lid 12a at a prescribed distance d. The seed crystal 5-attaching surface of the seed crystal-adhering member 12b is dented from the surface of the lid 12a so that the growth surface of the seed crystal 5 is the same as or slightly projected from the surface of the lid 12a, when the seed crystal 5 is disposed. Thus, the single crystal grows from the growth surface of the seed crystal 5, while the polycrystal grows from the surface of the lid 12a. The single crystal can grow in a state embedded in the polycrystal without adhering to the polycrystal.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a single crystal on a seed crystal attached to a seed crystal attaching member, a method for producing a high-quality single crystal with few defects, and a single crystal suitable for the method The present invention relates to a crystal manufacturing apparatus, and is particularly suitable for use in a silicon carbide single crystal manufacturing method for manufacturing a high-quality silicon carbide single crystal and a silicon carbide semi-crystal manufacturing apparatus.

[0002]

2. Description of the Related Art Silicon carbide single crystals are expected to be used as semiconductor substrates for power devices because of their characteristics of high breakdown voltage and high electron mobility. In general, a single crystal growth method called a sublimation method (improved Rayleigh method) is used for silicon carbide single crystal growth.

In the improved Rayleigh method, a silicon carbide raw material is inserted into a graphite crucible, and a seed crystal is mounted on the inner wall of the graphite crucible so as to face the raw material portion.
The substrate is heated to 0 to 2400 ° C. to generate a sublimation gas, and is recrystallized into a seed crystal whose temperature is lower by several tens to several hundreds degrees Celsius than a raw material part, thereby growing a silicon carbide single crystal.

Heretofore, conventionally, a graphite crucible 1 as shown in FIG.
The crystal growth was performed in a state where the seed crystal 5 was attached to the projection provided on the inner wall of the lid member 12. For this reason, FIG.
As shown in (b), with the growth of silicon carbide single crystal 7 on seed crystal 5, polycrystal 8 grows on the inner wall surface of graphite crucible 1 exposed in the crystal growth space, and polycrystal 8 grows.
However, there is a problem in that the silicon carbide single crystal 7 has a bad effect such that it adheres and fuses around the desired silicon carbide single crystal 7 and the periphery 7a of silicon carbide single crystal 7 is polycrystallized.

In order to solve the above-mentioned problem, Japanese Patent Laid-Open Publication No. Hei 6-48898 discloses a method in which single crystal growth is temporarily stopped before the surrounding polycrystal becomes larger than a desired single crystal, and a single crystal is removed from a graphite crucible. It has been proposed to repeat the process of restarting single crystal growth after removing the surrounding polycrystals many times.

[0006]

However, in this method, the above steps must be repeated a plurality of times in producing one single crystal ingot, which is complicated. Moreover, as in the production of silicon carbide single crystal, 200
When a single crystal must be grown at a high temperature of 0 ° C. or higher, it takes a long time to raise and lower the temperature. Furthermore, it is very difficult to find a timing at which the surrounding polycrystal does not exceed a desired single crystal, that is, a timing immediately before the polycrystal is attached to the single crystal, and to stably reproduce the timing.

The present invention has been made in view of the above problems, and prevents a single crystal grown on a seed crystal surface and a polycrystal formed around the single crystal from adhering to each other. It is intended to be able to be manufactured.

[0008]

According to the first or second aspect of the present invention, a crucible (1) is constituted by a seed crystal sticking member (12b) and containers (11, 12a). The container (1) that surrounds the seed crystal attaching member (12b) while the seed crystal attaching member is surrounded by the container.
1, 12a) are arranged such that a predetermined gap (d) is formed between the end face and the seed crystal attaching member, and the surface of the seed crystal attaching member on which the seed crystal is attached is the seed crystal. The sticking member is located so as to be recessed from one surface of the container in which the seed crystal is attached, and the surface of the seed crystal sticking member surrounded by the container is covered with the seed crystal and the container when the seed crystal is attached. It is characterized by being.

According to such a configuration, the surface of the seed crystal attaching member surrounded by the container is covered with the seed crystal and the container, that is, the surface of the seed crystal attaching member is not exposed in the growth space. Polycrystals can be prevented from growing from the surface of the seed crystal attachment member. Therefore, it is possible to prevent the polycrystal grown from the seed crystal attaching member from attaching to the single crystal grown on the seed crystal, and to grow a high-quality single crystal.

In the invention according to claim 2, a gap (d) having a predetermined interval is formed between the end face of the container (11, 12a) surrounding the seed crystal sticking member (12b) and the seed crystal sticking member. And the source gas in the growth space can be extracted through the gap.

If a predetermined gap is provided between the seed crystal sticking member and the end face of the container as described above, and the raw material gas can be extracted from this gap, the flow of the raw material gas causes Since no polycrystal is formed on the surface surrounded by the container, the single crystal and the polycrystal formed on one surface of the container can be prevented from adhering. Thereby, a high-quality single crystal can be grown.

For example, as set forth in claim 3, the distance between the seed crystal sticking member and the end face of the container surrounding the seed crystal sticking member is 0.1 mm or less along the shape of the seed crystal sticking member. Preferably, it is large and smaller than 1 mm. That is, if the interval is too short, the effect of separating the seed crystal affixing member and the end face of the container is lost, and if the interval is too long, the gap formed by the separation becomes substantially equal to the growth space. Is preferred. For example, claim 2
In the case of extracting the source gas as described above, if the interval is too long, the flow of the source gas becomes slow, and the effect of preventing the polycrystal from attaching to the single crystal due to the flow of the gas is weakened.

Further, as set forth in claim 4, a heat insulating member for suppressing heat transfer from the container to the seed crystal attaching member may be provided between the seed crystal attaching member and the container.

With this configuration, since heat transfer from the container to the seed crystal attaching member is suppressed, a temperature difference is provided between one surface of the container in which the seed crystal attaching member is disposed and the seed crystal attaching member. Can be.

In this case, as described in claim 5, if a material through which the raw material gas can pass is used as the heat insulating member, the effect described in claim 2 can be obtained. As such a heat insulating member, for example, the porous graphite described in claim 6 can be mentioned.

According to a seventh aspect of the present invention, the seed crystal surface is flush with, or slightly protrudes from, one surface of the container in which the seed crystal attaching member is disposed. I have.

When the surface of the seed crystal is depressed with respect to one surface of the container, the grown single unit is greatly affected by the container located at the periphery of the seed crystal (for example, the effect of the sublimation gas in the container). Defects may be formed at the periphery of the crystal. Therefore, with the above structure, a defect can be prevented from being formed on the periphery of the single crystal, and a high-quality single crystal can be obtained. In particular, when one surface of the container is coated in advance with a silicon carbide material or a high melting point metal carbide, the effect is enhanced.

In the invention according to claim 8, the shapes of the seed crystal sticking member and the container are such that the growth surface temperature of the seed crystal is:
It is characterized in that it is configured to be lower than the surface temperature of one surface of the container in which the seed crystal attaching member is disposed.

Thus, the crystal can be preferentially grown on the growth surface of the seed crystal. Specifically, by forming a counterbore on the side opposite to the surface on which the seed crystal is attached, of the seed crystal attaching member, the shapes of the seed crystal attaching member and the container are adjusted so that the seed crystal grows. The shape may be such that a temperature difference can be made between the surface temperature and the surface temperature of one surface of the container.

In addition, as shown in claim 10, claim 1
In the single crystal manufacturing apparatus according to any one of to 9, the crucible is formed of a carbon material, and when applied as a silicon carbide single crystal manufacturing apparatus for growing a silicon carbide single crystal on a seed crystal formed of silicon carbide, This is particularly preferable because crystal growth is performed at a high temperature.

In this case, when one surface of the container in which the seed crystal attaching member is disposed is coated with a high melting point metal carbide, impurities and defects are less likely to enter the single crystal to be further grown. I can do it. As the refractory metal, at least one of hafnium carbide (HfC), tantalum carbide (TaC), zirconium carbide (ZrC), and titanium carbide (TiC) can be used.

According to the thirteenth aspect of the present invention, on one surface of the crucible on which the seed crystal is disposed, a depression is formed in a portion where the seed crystal is disposed, and the seed crystal is disposed on the bottom surface of the depression. Sometimes, the bottom surface of the dent is covered with a seed crystal.

In the invention according to claim 14, the seed crystal sticking member (12a) is surrounded by containers (11, 12a),
When the surface on which the seed crystal is attached of the seed crystal attaching member is positioned so as to be recessed from one surface of the container in which the seed crystal attaching member is disposed, and the seed crystal (5) is attached to the seed crystal attaching member. Furthermore, a surface of the seed crystal attaching member surrounded by the container is covered with the seed crystal and the container, and a single crystal is grown on the seed crystal.

[0024] Thereby, since no polycrystal is formed from the seed crystal attaching member around the seed crystal, the polycrystal grown from the periphery adheres to the single crystal grown on the growth surface of the seed crystal. Can be prevented. Thereby, a high-quality single crystal can be grown.

In the invention according to claim 15, a predetermined gap (d) is provided between the seed crystal sticking member (12b) and the end faces of the containers (11, 12a) surrounding the seed crystal sticking member.
And growing a single crystal on the growth surface of the seed crystal while extracting the source gas in the growth space through the gap.

As described above, by providing a gap at a predetermined interval between the seed crystal sticking member and the end face of the container, the raw material gas can be extracted from this gap. Since the crystal growth can be suppressed in the region where the gas flows, the polycrystal formed on one surface of the container adheres to the single crystal formed on the seed crystal growth surface. Can be prevented.
Thereby, a high-quality single crystal can be grown.

According to a sixteenth aspect of the present invention, when the growth surface temperature of the seed crystal is lower than the surface temperature of one surface of the container in which the seed crystal attaching member is provided, the crystal is preferentially formed on the growth surface of the seed crystal. Growth can take place.

For example, by spraying a low-temperature gas on a side of the seed crystal attaching member opposite to the surface on which the seed crystal is attached, the growth surface temperature of the seed crystal can be reduced to one side of the container. It can be lower than the surface temperature.

In this case, as the low-temperature gas, the same inert gas as the inert gas introduced into the growth space of the crucible can be used as the low-temperature gas. Further, as described in claim 19, by mixing an element serving as a single crystal impurity into the same inert gas as the inert gas introduced into the growth space of the crucible as a low-temperature gas, the desired impurity can be added to the single crystal. Can also be doped. For example, as an element serving as an impurity, at least one of N (nitrogen), B (boron), Al (aluminum), P (phosphorus), and As (arsenic) may be used. it can.

The reference numerals in the parentheses of the above-mentioned means indicate the correspondence with the concrete means described in the embodiments described later.

[0031]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The embodiment shown in the drawings will be described below.

FIG. 1 shows a graphite crucible 1 as a crystal growth apparatus used in the present embodiment. This figure shows graphite when silicon carbide raw material 2 provided in graphite crucible 1 is sublimated by heat treatment, and silicon carbide single crystal 7 is grown on seed crystal 5 formed of a silicon carbide single crystal layer. It is sectional drawing of the crucible 1 made.

The graphite crucible 1 comprises a crucible body 11 having an open upper surface, and a lid member 12 for closing the opening of the crucible body 11. In the crucible 1 made of graphite, the lid 12 serves as a pedestal for supporting the seed crystal 5.

The lid member 12 includes a lid portion 12a and a seed crystal sticking member 12b. The lid 12a
It forms the outer shape of the lid member 12 and has a shape in which the center portion is opened in a circular shape. Seed crystal sticking member 12b
Is detachably formed at the opening of the lid 12a, and has a surface for attaching the seed crystal 5. The seed crystal sticking member 12b has a substantially cylindrical shape, and has a flange shape at the end opposite to the side where the seed crystal 5 is stuck. And
When the seed crystal attaching member 12b is arranged at the center opening of the lid member 12a, the flange portion is caught and the seed crystal attaching member 12b is fixed at a predetermined position of the lid member 12a.

The inner diameter of the opening at the center of the lid 12a is substantially equal to the outer diameter of the seed crystal sticking part 12b. When the seed crystal sticking part 12b is attached to the lid 12a, the inner diameter of the lid 12a is reduced. The distance d is set between the inner peripheral wall (end surface) of the opening and the outer peripheral wall of the seed crystal attaching member 12b. At this time, the interval d is larger than 0.1 mm.
It is set to be smaller than 0 mm. This is because if the distance d is too small, it becomes substantially the same as when no space is left, and if it is too large, it acts like a growth space.

Further, the thickness (length in the axial direction) of the seed crystal attaching member 12b is substantially equal to the thickness of the seed crystal 5
Is thinner to the extent of or slightly smaller than the thickness of.
In other words, when the single crystal 5 is not attached when the cover material 12 is viewed as a whole, the portion where the seed crystal 5 is attached is configured to be concave, and when the seed crystal 5 is attached, the seed crystal 5 is attached. Is formed to be flush with or slightly project from the surface of the lid 12a.

As described above, since the inner diameter of the central opening portion of the lid portion 12a is substantially equal to the outer diameter of the seed crystal attaching portion 12b, the surface of the seed crystal attaching member 12b on which the seed crystal 5 is disposed. When the seed crystal 5 is disposed, the bottom surface of the dent of the cover member 12 is almost completely covered by the seed crystal 5 and is not exposed to the outside.

Further, since the growth surface of the seed crystal 5 is not located at a position depressed from the adjacent lid portion 12a, the carbon gas sublimated from the end portion of the lid portion 12a adjacent to the seed crystal 5 is seeded. The growth surface of the crystal 5 can be prevented from being affected.

The silicon carbide sticking member 12b is
a and the thickness of the seed crystal 5 can be made slightly lower than the surface temperature of the lid 12a due to heat conduction due to the thermal conductivity. Therefore, crystal growth can be preferentially generated on the growth surface of seed crystal 5.

The graphite crucible 1 can be heated by a heater in a vacuum vessel (heating furnace) into which an argon gas can be introduced. By adjusting the power of the heater, the temperature of the seed crystal 5 can be reduced. It can be maintained at a temperature lower by about 10 to 100 ° C. than the temperature of silicon carbide raw material powder 2.

When the silicon carbide single crystal 7 is grown on the growth surface of the seed crystal 5 using the graphite crucible 1 thus configured, as shown in FIG. The growth proceeds while being expanded in the radial direction, and after the diameter has expanded to some extent, the growth proceeds with substantially the same diameter thereafter. At this time, polycrystal 8 similarly grows from the surface of lid portion 12a along with the growth of silicon carbide single crystal 7,
Was found to grow so as to surround silicon carbide single crystal 7 at a predetermined distance from silicon carbide single crystal 7. In other words, buried growth is performed in which silicon carbide single crystal 7 grows in a state of being buried in polycrystal 8.

As described above, when the single crystal and the polycrystal are grown on adjacent different growth surfaces having substantially the same height (in the case of the present embodiment, the surface of the seed crystal 5 and the surface of the lid 12a). The single crystal and the polycrystal can be grown so as not to be fused at a predetermined interval.

As a result, it is possible to prevent the occurrence of crystal defects caused by the attachment of the polycrystal to the single crystal, and to manufacture a high-quality, large-diameter silicon carbide single crystal 7.

Next, a description will be given of the results of an experiment in which a silicon carbide single crystal 7 was actually formed on the surface of a seed crystal 5 using the graphite crucible 1 having the above configuration.

The growth of silicon carbide single crystal 7 was performed as follows.

First, as a seed crystal 5, a silicon carbide single crystal produced by the Acheson method was used to obtain a diameter of 10 mm and a thickness of 1 mm.
And the mirror-finished surface was used. At this time, the crystal orientation was determined so that the growth plane of the seed crystal 5 became the (000-1) just plane.

Then, the seed crystal 5 is attached to the seed crystal attaching member 1.
After attaching to 2a, it attached to lid part 12a. At this time, the seed crystal sticking member 12b and the lid 12
The gap d between the gap a and the gap a was 0.5 mm.

The lid 12a and the seed crystal attaching member 12
b was mounted on the crucible body 11 in which the silicon carbide raw material powder 2 was previously placed. Then, the graphite crucible 1 is placed in a heating furnace, and the temperature of the silicon carbide raw material powder 2 is set to 2290 ° C.
The growth surface temperature of the seed crystal 5 is 2230 ° C. and the atmospheric pressure is 1
Under the condition of Torr, silicon carbide single crystal 7 was grown by a sublimation method for 24 hours.

The silicon carbide single crystal 7 thus obtained is
The growth height was about 12 mm and the maximum diameter was about 15 mm. Further, polycrystal was hardly generated from seed crystal sticking member 12b, and polycrystal 8 generated from the surface of the single crystal manufacturing apparatus around seed crystal 5 and silicon carbide single crystal 6 grown were completely separated. At the peripheral portion of the silicon carbide single crystal substrate cut out of silicon carbide single crystal 7, there were almost no polycrystals, cracks or subgrain-like defects caused by fusion with the polycrystal.

(Second Embodiment) The graphite crucible 1 of the present embodiment is different from the first embodiment only in the configuration of the lid member 12, and therefore only different portions from the first embodiment will be described.

FIG. 2 is a cross-sectional view of the lid material 12 of the graphite crucible 1 as a crystal growth apparatus in the present embodiment. 3 (a) and 3 (b) show a front view and a back view of the lid member 12 shown in FIG. 2, respectively.

In the present embodiment, the lid 12 is formed of one member, and a substantially circular recess 13 is formed at the center of the lid 12.
The recess 13 constitutes the seed crystal attaching member 12b in the first embodiment, and the seed crystal 5 is arranged in the recess 13.

A notch 14 is formed on the outer periphery of the dent 13 of the cover member 12 to a position at a predetermined depth of the cover member 12, and the back side of the cover member 12 (the surface on which the seed crystal 5 is disposed). The gas vent hole 15 communicating with the notch 14
Are formed at a plurality of locations (six locations in FIG. 3).

The gas in the graphite crucible 1 is released through the notch 14 and the gas vent hole 15. The depth of the recess 13 is equal to or slightly smaller than the thickness of the seed crystal 5, and the width of the notch 14 is the same as the lid 12 a and the seed crystal attaching member 12 b in the first embodiment.
The distance d is set in the same way as the distance d.

Next, a description will be given of an experimental result in which a silicon carbide single crystal 7 is actually formed on the surface of the seed crystal 5 using the graphite crucible 1 having the above configuration.

First, a seed crystal 5 similar to the one used in the experiment of the first embodiment is prepared, this seed crystal 5 is stuck in the recess 13, and the crucible body 11 in which the silicon carbide raw material powder 2 has been previously placed is covered with a lid. Material 12 was attached.

Then, the graphite crucible 1 is placed in a heating furnace, the temperature of the silicon carbide raw material powder 2 is 2300 ° C., the growth surface temperature of the seed crystal 15 is 2230 ° C., and the atmospheric pressure is 1 To.
Under the condition of rr, silicon carbide single crystal 7 was grown by sublimation for 24 hours.

The silicon carbide single crystal 7 thus obtained is
The growth height was about 15 mm and the maximum diameter was about 15 mm. Part of the sublimation gas that passed through the gas vent hole 15 was attached to another part of the graphite crucible 1 and was polycrystallized.

Polycrystal is hardly generated from seed crystal sticking member 2, and is completely separated from polycrystal 8 generated from the surface of cover material 12 around seed crystal 5 and grown silicon carbide single crystal 6. Was.

At the peripheral portion of the silicon carbide single crystal substrate cut out of silicon carbide single crystal 7, there were almost no polycrystals, cracks or subgrain-like defects caused by fusion with the polycrystal.

(Third Embodiment) The graphite crucible 1 of the present embodiment is different from the first embodiment only in the configuration of the lid member 12, and therefore only different portions from the first embodiment will be described.

FIG. 4 is a cross-sectional view of the lid member 12 of the graphite crucible 1 as a crystal growth apparatus in the present embodiment.

In the present embodiment, the lid member 12 is composed of the lid portion 12a and the seed crystal sticking member 12b as in the first embodiment, but the amount of protrusion of the flange portion of the seed crystal sticking member 12b is increased. Together with the lid part 12a and the seed crystal sticking part 12
b is widened, and porous graphite is filled between them. This porous graphite has heat insulation properties, can suppress heat conduction from the lid portion 12a to the seed crystal attaching member 12b, and has pores large enough to allow a raw material gas in the graphite crucible 1 to pass therethrough. Material.

The other components such as the thickness of the seed crystal attaching member 12b are the same as those of the first embodiment.

Next, a description will be given of the results of an experiment in which a silicon carbide single crystal 7 was actually formed on the surface of a seed crystal 5 using the graphite crucible 1 having the above configuration.

First, a seed crystal 5 similar to that used in the experiment of the first embodiment is prepared. Subsequently, the seed crystal attaching member 12b is attached to the central opening of the lid 12a with the porous graphite sandwiched therebetween, and then the seed crystal 15 is attached to the seed crystal attaching member 12b.

Then, the lid member 12 was attached to the crucible main body 1 in which the silicon carbide raw material powder 2 was previously placed.

Then, the graphite crucible 1 was placed in a heating furnace, the temperature of the silicon carbide raw material powder 2 was 2290 ° C., the growth surface temperature of the seed crystal 5 was 2230 ° C., and the atmospheric pressure was 1 Torr.
Under the condition of r, silicon carbide single crystal 7 was grown by sublimation for 24 hours.

Silicon carbide single crystal 7 thus obtained
Had a growth height of about 13 mm and a maximum diameter of about 18 mm. The diameter of silicon carbide single crystal 7 was larger than the experimental result in the first embodiment. Similarly to the first embodiment, the peripheral portion of the silicon carbide single crystal substrate cut out of silicon carbide single crystal 7 had almost no polycrystal, crack or subgrain-like defect caused by fusion with polycrystal. .

(Comparative Example) As a reference, an experimental result when a silicon carbide single crystal was grown using the graphite crucible 1 having the conventional structure shown in FIG. 5 is shown.

First, a seed crystal 5 having the same configuration as in the first embodiment was prepared. Then, the seed crystal 5 was attached to the projection of the lid portion 12 of the graphite crucible 1 as shown in FIG. 5 and mounted on the crucible body 1 in which the silicon carbide raw material powder 2 was previously put.

Then, the graphite crucible 1 was placed in a heating furnace, the temperature of the silicon carbide raw material powder 2 was 2290 ° C., the growth surface temperature of the seed crystal 5 was 2230 ° C., and the atmospheric pressure was 1 Torr.
Under the condition of r, silicon carbide single crystal 7 was grown by sublimation for 24 hours.

The silicon carbide single crystal 7 thus obtained is
The growth height was about 12 mm and the maximum diameter was about 15 mm.

However, polycrystals 8 were generated around the protrusions, and polycrystals 8 grew from these around the periphery of silicon carbide single crystal 7. At the peripheral portion 7a of the silicon carbide single crystal substrate cut out from silicon carbide single crystal 7, polycrystals, cracks or subgrain-like defects caused by fusion with the polycrystal were observed.

(Other Embodiments) In each of the above embodiments, the case where the present invention is used for crystal growth of a silicon carbide single crystal has been described. However, the present invention can be used for other crystal growth.

In the above embodiment, the crucible 1 made of graphite is used.
This was used for a single crystal growth apparatus, but the graphite crucible 1
May be coated with a high melting point metal and its carbide. By coating the inner wall of the graphite crucible 1 with the high melting point metal as described above, the Si / C ratio becomes uniform, and it is possible to form the silicon carbide single crystal 7 having no crystal defects. As the refractory metal carbide, for example, any one of hafnium carbide (HfC), tantalum carbide (TaC), zirconium carbide (ZrC), and titanium carbide (TiC) can be used.

In the third embodiment, porous graphite is used, but other materials may be used as long as they allow gas to pass therethrough.

Further, in the above embodiment, the porous graphite is arranged between the lid 12a and the seed crystal sticking member 12b in order to make it difficult for heat to be transferred to the seed crystal sticking member 12b. Lid 1 where growth surface temperature of crystal 5 is adjacent
2a, so that the temperature is lower than the surface temperature of
A counterbore may be provided on the side opposite to the side on which the seed crystal 5 is arranged (hereinafter, referred to as a back surface) in 2b. Alternatively, a low-temperature gas may be blown onto the back surface of the seed crystal attaching member 12b so that the growth surface of the seed crystal 5 is lower in temperature than the surface of the lid 12a. At this time, the same low-temperature gas as the inert gas introduced into the graphite crucible 1 during crystal growth may be used. When it is desired to form a desired doped single crystal as silicon carbide single crystal 7, an element necessary for doping may be included in an inert gas sprayed on seed crystal attaching member 12b. For example, as an element to be doped, any of N (nitrogen), B (boron), Al (aluminum), P (phosphorus), As (arsenic), or the like is included in the inert gas.

[Brief description of the drawings]

FIG. 1 is a graphite crucible 1 according to a first embodiment of the present invention.
FIG. 3 is a diagram showing a cross-sectional configuration of FIG.

FIG. 2 is a diagram illustrating a cross-sectional configuration of a lid member 12 according to a second embodiment of the present invention.

FIG. 3A is a front view of the lid member 12 shown in FIG. 2,
FIG. 3B is a back view of the lid 12 shown in FIG. 2.

FIG. 4 is a diagram showing a cross-sectional configuration of a lid member 12 according to a third embodiment of the present invention.

FIG. 5A is a diagram showing a cross-sectional configuration of a conventional graphite crucible 1, and FIG. 5B is an enlarged view of the vicinity of a lid member 12 of the graphite crucible 1 shown in FIG.

[Explanation of symbols]

DESCRIPTION OF SYMBOLS 1 ... Graphite crucible, 2 ... Silicon carbide raw material, 5 ... Seed crystal, 7
... Silicon carbide single crystal, 8 ... Polycrystal, 12 ... Lid material, 12a ...
Lid, 12b: seed crystal sticking member, 13: recess, 14: notch, 15: vent hole.

 ────────────────────────────────────────────────── ─── Continuing from the front page (72) Inventor Ichito Hara 1-1-1, Showa-cho, Kariya-shi, Aichi Prefecture Inside Denso Co., Ltd. (72) Inventor Atsuto Okamoto 41, Yakumichi, Yakumichi, Nagakute-cho, Aichi-gun, Aichi Prefecture -1 F-term in Toyota Central Research Laboratory, Inc. (reference) 4G077 BE08 DA02 ED04 SA11

Claims (21)

[Claims] 1. A crucible (1) comprising a container (11, 12a) provided with a seed crystal sticking member (12b) on one surface.
A seed crystal (5) is attached to the surface of the seed crystal attaching member, and a single crystal source gas to be grown into the growth space in the crucible is introduced, whereby the seed crystal growth surface A single crystal producing apparatus for growing a single crystal, wherein the seed crystal attaching member is surrounded by the container,
A predetermined gap is provided between the container and an end surface of a portion surrounding the seed crystal attaching member, and a surface of the seed crystal attaching member to which the seed crystal is attached is the seed crystal attached. The member is disposed so as to be recessed from one surface of the container, and when the seed crystal is attached, the surface of the seed crystal affixing member that is surrounded by the container includes the seed crystal and the container. A single crystal manufacturing apparatus characterized by being covered by: 2. A crucible (1) comprising a container (11, 12a) provided with a seed crystal sticking member (12b) on one surface.
A seed crystal (5) is attached to the surface of the seed crystal attaching member, and a single crystal source gas to be grown into the growth space in the crucible is introduced, whereby the seed crystal growth surface A single crystal producing apparatus for growing a single crystal, wherein the seed crystal attaching member is surrounded by the container,
A predetermined gap is provided between the container and an end surface of a portion surrounding the seed crystal attaching member, and the source gas in the growth space can be withdrawn through the gap. The surface of the seed crystal attachment member on which the seed crystal is attached is positioned so as to be recessed from one surface of the container in which the seed crystal attachment member is provided, and the seed crystal is attached when the seed crystal is attached. An apparatus for producing a single crystal, wherein the single crystal is not exposed to the growth space by a crystal and the container. 3. The distance between the seed crystal sticking member and the end surface of the container surrounding the seed crystal sticking member is larger than 0.1 mm and 1 mm along the shape of the seed crystal sticking member.
The single crystal manufacturing apparatus according to claim 1, wherein the size of the single crystal is smaller than that of the single crystal. 4. A heat insulating member for suppressing heat transfer from the container to the seed crystal attaching member is provided between the seed crystal attaching member and the container. 3. The single crystal production apparatus according to any one of 3. 5. The single crystal manufacturing apparatus according to claim 4, wherein the heat insulating member is made of a material through which the source gas can pass. 6. The apparatus according to claim 5, wherein the heat insulating member is made of porous graphite. 7. The seed crystal growth surface is flush with, or slightly protrudes from, one surface of the container in which the seed crystal sticking member is provided. The apparatus for producing a single crystal according to any one of 1 to 6. 8. The shape of the seed crystal sticking member and the container is configured such that a growth surface temperature of the seed crystal is lower than a surface temperature of one surface of the container in which the seed crystal sticking member is provided. 8. The method according to claim 1, wherein
The single crystal production apparatus according to any one of the above. 9. The single crystal manufacturing apparatus according to claim 8, wherein a counterbore is provided on a side of the seed crystal attaching member opposite to a surface on which the seed crystal is mounted. 10. The single crystal manufacturing apparatus according to claim 1, wherein the crucible is made of a carbon material, and the growth surface of the seed crystal made of silicon carbide is carbonized. An apparatus for producing a silicon carbide single crystal, wherein a silicon single crystal is grown. 11. The single crystal manufacturing apparatus according to claim 10, wherein one surface of the container on which the seed crystal attaching member is disposed is coated with a high melting point metal carbide. 12. The high melting point metal carbide is made of at least one of hafnium carbide (HfC), tantalum carbide (TaC), zirconium carbide (ZrC), and titanium carbide (TiC). Claim 1
2. The apparatus for producing a silicon carbide single crystal according to 1. 13. A seed crystal (5) is placed on one surface of a crucible (1), and a single crystal source gas to be grown on the seed crystal is supplied, whereby a single crystal is grown on the seed crystal growth surface. In a single crystal manufacturing apparatus for growing a crystal, a depression is formed in a portion of the crucible where the seed crystal is disposed, where the seed crystal is disposed, and the seed crystal is disposed on a bottom surface of the depression. Wherein the bottom surface of the recess is covered with the seed crystal when the single crystal is formed. 14. A crucible (1) comprising a container (11, 12a) having a seed crystal sticking member (12b) disposed on one surface thereof, and a seed crystal (5) attached to the surface of the seed crystal sticking member. Thereafter, a single crystal production method for growing a single crystal on a growth surface of the seed crystal by introducing a source gas and an inert gas of the single crystal to be grown into the growth space in the crucible, The seed crystal sticking member is surrounded by the container, and the surface of the seed crystal sticking member to which the seed crystal is attached is positioned so as to be recessed from one surface of the container in which the seed crystal sticking member is disposed, When the seed crystal is attached to the seed crystal attachment member, the surface of the seed crystal attachment member that is surrounded by the container is covered with the seed crystal and the container, and the seed crystal growth surface The single crystal Producing a single crystal wherein the to. 15. A crucible (1) comprising a container (11, 12a) having a seed crystal sticking member (12b) disposed on one surface thereof, and a seed crystal (5) attached to the surface of the seed crystal sticking member. Thereafter, a source gas and an inert gas of a single crystal to be grown in the growth space in the crucible are introduced, and the source gas is supplied to the seed crystal to grow the single crystal on the growth surface of the seed crystal. A method for producing a single crystal, wherein the seed crystal attachment member is surrounded by the container, and a predetermined space is provided between the seed crystal attachment member and an end surface of the container surrounding the seed crystal attachment member. Withdrawing the source gas of, and, of the seed crystal affixing member, the surface to which the seed crystal is attached is positioned so as to be recessed from one surface of the container provided with the seed crystal affixing member, Seed the seed crystal By to be entirely covered by the said container and seed crystals when attached to sticking member, a single crystal manufacturing method characterized by growing said single crystal on the seed crystal. 16. The method for producing a single crystal according to claim 15, wherein a growth surface temperature of the seed crystal is set lower than a temperature of one surface of the container in which the seed crystal attaching member is provided. 17. The method for producing a single crystal according to claim 16, wherein a low-temperature gas is sprayed on a side of the seed crystal attaching member opposite to a surface on which the seed crystal is attached. 18. The single crystal manufacturing method according to claim 17, wherein the same inert gas as the inert gas introduced into the growth space of the crucible is used as the low-temperature gas. 19. An inert gas which is the same as the inert gas introduced into the growth space of the crucible is used as the low-temperature gas, and an element serving as an impurity of the single crystal is mixed into the inert gas. The method for producing a single crystal according to claim 17, wherein: 20. The semiconductor device according to claim 20, wherein at least one of N (nitrogen), B (boron), Al (aluminum), P (phosphorus), and As (arsenic) is used as the impurity element. 20. The method for producing a single crystal according to 19. 21. The method for producing a single crystal according to claim 14, wherein silicon carbide is used as the seed crystal, and a silicon carbide source gas is introduced into the growth space of the crucible as the source gas. Forming a silicon carbide single crystal on the growth surface of the seed crystal.