JP4288792B2 - Single crystal manufacturing method and single crystal manufacturing apparatus - Google Patents

Description

[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a single crystal manufacturing method and a single crystal manufacturing apparatus suitable for the single crystal manufacturing method for manufacturing a high quality single crystal with few defects in manufacturing a single crystal on a seed crystal mounted on a seed crystal sticking member. It is suitable for use in a silicon carbide single crystal manufacturing method and a silicon carbide semi-crystal manufacturing apparatus for manufacturing a quality silicon carbide single crystal.
[0002]
[Prior art]
Since silicon carbide single crystal has characteristics of high breakdown voltage and high electron mobility, it is expected as a semiconductor substrate for power devices. A single crystal growth method called a sublimation method (improved Rayleigh method) is generally used for silicon carbide single crystal growth.
[0003]
In the modified 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, and the raw material portion is heated to 2200 to 2400 ° C. to sublimate gas. A silicon carbide single crystal is grown by recrystallizing a seed crystal having a temperature lower by several tens to several hundreds of degrees Celsius than the raw material portion.
[0004]
Here, conventionally, a state in which the seed crystal 5 is pasted directly on the inner wall of the graphite crucible or on the protrusion provided on the inner wall of the lid 12 of the graphite crucible 1 as shown in FIG. The crystal was growing. For this reason, as shown in FIG. 5B, with the growth of the silicon carbide single crystal 7 on the seed crystal 5, the polycrystal 8 grows on the inner wall surface of the graphite crucible 1 exposed in the crystal growth space. The polycrystalline carbide 8 adheres to and fuses around the desired silicon carbide single crystal 7, and the peripheral 7 a of the silicon carbide single crystal 7 is polycrystallized, resulting in defects in the silicon carbide single crystal 7. There was a problem.
[0005]
Therefore, in order to solve the above problem, in Japanese Patent Laid-Open No. 6-48898, the single crystal growth is temporarily stopped before the surrounding polycrystal becomes larger than the desired single crystal, and the polycrystal around the single crystal is separated from the graphite crucible. It has been proposed to repeat the process of resuming single crystal growth after removing the crystal many times.
[0006]
[Problems to be solved by the invention]
However, in this method, the above process must be repeated a plurality of times in order to produce one single crystal ingot. In addition, when a single crystal must be grown at a high temperature of 2000 ° C. or more as in the case of manufacturing a silicon carbide single crystal, it takes time to raise and lower the temperature, and thus the single crystal production process takes a long time. . Furthermore, it is very difficult to find the timing when the surrounding polycrystal does not exceed the desired single crystal, that is, the timing immediately before the polycrystal adheres to the single crystal, and to reproduce it stably.
[0007]
The present invention has been made in view of the above problems, and prevents the single crystal grown on the surface of the seed crystal and the polycrystal formed around the single crystal from adhering, so that a high-quality single crystal can be produced. The purpose is to.
[0008]
[Means for Solving the Problems]
In order to achieve the above object, in the invention described in claim 1, the crucible (1) is constituted by the seed crystal sticking member (12b) and the container (11, 12a), and the seed crystal sticking member is surrounded by the container. In addition, the seed crystal sticking member is disposed such that 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. The surface 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 attaching member is disposed, and the surface surrounded by the container of the seed crystal attaching member is attached to the seed crystal. It is characterized by being covered with a seed crystal and a container.
[0009]
According to such a configuration, the surface of the seed crystal sticking member surrounded by the container is covered with the seed crystal and the container, that is, the surface of the seed crystal sticking member is not exposed in the growth space. Polycrystals can be prevented from growing from the surface of the member. For this reason, the polycrystal grown from the seed crystal sticking member can be prevented from adhering to the single crystal grown on the seed crystal, and a high-quality single crystal can be grown.
[0010]
Furthermore, in the first aspect of the invention, 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 material gas in the growth space can be extracted through the gap.
[0011]
In this way, if a gap of a predetermined interval is provided between the seed crystal sticking member and the end face of the container, and the source gas can be extracted from this gap, the seed crystal sticking member is surrounded by the container by the flow of the source gas. Since the polycrystal is not formed on the surface to be bonded, the single crystal and the polycrystal formed on the one surface of the container can be prevented from adhering. Thereby, a high quality single crystal can be grown.
[0012]
For example, as shown in claim 2 , the distance between the seed crystal sticking member and the end face of the container surrounding the seed crystal sticking member is greater than 0.1 mm and 1 mm along the shape of the seed crystal sticking member. It is preferable to be smaller. That is, if this interval is too short, the effect of separating the seed crystal sticking member and the end face of the container is lost, and if it is too long, the gap formed by separation is substantially equivalent to the growth space. Is preferred. For example, when extracting the source gas as in claim 2, since the flow of the source gas becomes slow if the interval is too long, there is an effect of preventing the polycrystal from adhering to the single crystal due to the gas flow. Fade.
[0013]
Further, as shown in claim 3 , a heat insulating member that suppresses heat transfer from the container to the seed crystal sticking member may be provided between the seed crystal sticking member and the container.
[0014]
If comprised in this way, since the heat transfer from a container to a seed crystal sticking member is suppressed, a temperature difference can be provided in the one surface and the seed crystal sticking member in which the seed crystal sticking member was arrange | positioned.
[0015]
In this case, as shown in claim 4 , if a material through which the source gas can pass is used as the heat insulating member, the effect shown in claim 1 can be obtained. Examples of such a heat insulating member include porous graphite shown in claim 5 .
[0016]
The invention according to claim 6 is characterized in that the surface of the seed crystal is flush with or slightly protrudes from one surface of the container in which the seed crystal sticking member is disposed.
[0017]
If the seed crystal surface is recessed with respect to one surface of the container, the periphery of the grown single crystal is greatly affected by the influence of the container located at the periphery of the seed crystal (for example, the influence of the sublimation gas of the container). In some cases, defects may be formed. For this reason, by setting it as the said structure, it can prevent that a defect is formed in the periphery of a single crystal, and can be set as a high quality single crystal. In particular, when one surface of the container is previously coated with a silicon carbide material or a refractory metal carbide, the effect is increased.
[0018]
In the invention according to claim 7 , the shape of the seed crystal sticking member and the container is configured such that 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 sticking member is disposed. It is characterized by being.
[0019]
Thereby, crystal growth can be performed preferentially on the growth surface of the seed crystal. Specifically, as shown in claim 8 , by providing a counterbore on the opposite side of the surface to which the seed crystal is attached among the seed crystal sticking member, the shape of the seed crystal sticking member and the container can be grown. It can be set as the shape which can give a temperature difference to surface temperature and the surface temperature of the one surface of a container.
[0020]
In addition, as shown in claim 9 , in the single crystal manufacturing apparatus according to claims 1 to 8 , the crucible is made of a carbon material, and a silicon carbide single crystal is grown on a seed crystal made of silicon carbide. When applied as a silicon carbide single crystal manufacturing apparatus, crystal growth is performed at a high temperature, which is particularly preferable.
[0021]
In this case, as shown in claim 10 , if one surface of the container in which the seed crystal sticking member is disposed is coated with a refractory metal carbide, impurities and defects can be prevented from entering the single crystal to be further grown. . As the refractory metal, as shown in claim 11 , at least one of hafnium carbide (HfC), tantalum carbide (TaC), zirconium carbide (ZrC), and titanium carbide (TiC) can be used.
[0025]
In the invention described in claim 12 , the seed crystal sticking member (12b) is disposed with a gap (d) at a predetermined interval between the seed crystal sticking member and the end surface of the container (11, 12a) surrounding the seed crystal sticking member, While pulling the source gas in the growth space through the gap, the single crystal is grown on the growth surface of the seed crystal, so that the single crystal is surrounded by a polycrystal at a predetermined interval. And embedded growth in which a polycrystal is grown together .
[0026]
In this manner, by providing a gap with a predetermined interval between the seed crystal sticking member and the end face of the container, the source gas can be extracted from this gap. Since the crystal growth can be suppressed at the portion where the gas flows in this way, the polycrystal formed on the surface of one surface of the container adheres to the single crystal formed on the growth surface of the seed crystal. This can be prevented. Thereby, a high quality single crystal can be grown.
[0027]
According to a thirteenth aspect of the present invention, if 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 sticking member is disposed, the crystal growth is preferentially performed on the growth surface of the seed crystal. Can be
[0028]
For example, as shown in claim 14 , by spraying a low temperature gas on the opposite side of the surface to which the seed crystal is attached of the seed crystal sticking member, the growth surface temperature of the seed crystal is higher than the surface temperature of one surface of the container. Can also be lowered.
[0029]
In this case, as shown in claim 15 , the same inert gas as the inert gas introduced into the growth space of the crucible can be used as the low temperature gas. In addition, as described in claim 16 , if an element that becomes an impurity of a single crystal is mixed in the same inert gas as that introduced into the growth space of the crucible as a low-temperature gas, a desired impurity is added to the single crystal. It is also possible to dope. For example, at least one of N (nitrogen), B (boron), Al (aluminum), P (phosphorus), and As (arsenic) is used as an impurity element as shown in claim 17. it can.
[0030]
In addition, the code | symbol in the bracket | parenthesis of each said means shows the correspondence with the specific means as described in embodiment mentioned later.
[0031]
DETAILED DESCRIPTION OF THE INVENTION
Hereinafter, embodiments shown in the drawings will be described.
[0032]
FIG. 1 shows a graphite crucible 1 as a crystal growth apparatus used in this embodiment. This figure shows graphite obtained when a silicon carbide raw material 2 provided in a graphite crucible 1 is sublimated by heat treatment to grow a silicon carbide single crystal 7 on a seed crystal 5 composed of a silicon carbide single crystal layer. 2 is a cross-sectional view of the crucible 1 made.
[0033]
The graphite crucible 1 is composed of a crucible body 11 having an open top surface and a lid member 12 that closes the opening of the crucible body 11. In the graphite crucible 1, the lid 12 serves as a pedestal that supports the seed crystal 5.
[0034]
The lid member 12 is composed of a lid portion 12a and a seed crystal sticking member 12b. The lid portion 12a constitutes the outer shape of the lid member 12 and has a shape in which the central portion is opened in a circular shape. The seed crystal sticking member 12 b is configured to be removable at the opening of the lid portion 12 a and has a surface for attaching the seed crystal 5. The seed crystal sticking member 12b is formed in a substantially cylindrical shape, and the end on the opposite side to the side on which the seed crystal 5 is attached is formed in a flange shape. And when the seed crystal sticking member 12b is arrange | positioned in the opening part of the center of the cover material 12a, a flange part becomes a hook and the seed crystal sticking member 12b is fixed to the predetermined position of the cover material 12a.
[0035]
Further, the inner diameter of the central opening portion of the lid portion 12a is substantially equal to the outer diameter of the seed crystal pasting portion 12b, and when the seed crystal pasting portion 12b is attached to the lid portion 12a, the opening portion of the lid portion 12a. The distance d is set between the inner peripheral wall (end face) and the outer peripheral wall of the seed crystal pasting member 12b. At this time, the distance d is larger than 0.1 mm and smaller than 1.0 mm. This is because if the distance d is too small, it will be substantially the same as if the distance is not spaced, and if it is too large, it will act in the same way as the growth space.
[0036]
Furthermore, the thickness (axial length) of the seed crystal sticking member 12b is substantially equal to or slightly smaller than the thickness of the seed crystal 5 than the thickness of the lid portion 12a. That is, when the lid 12 is viewed as a whole, when the single crystal 5 is not attached, the portion to which the seed crystal 5 is attached is configured to be recessed, and when the seed crystal 5 is attached, the seed crystal 5 is attached. This growth surface is flush with the surface of the lid portion 12a, or is slightly protruded.
[0037]
Thus, since the inner diameter of the central opening of the lid 12a is substantially equal to the outer diameter of the seed crystal pasting portion 12b, the surface on which the seed crystal 5 is disposed (the lid material) of the seed crystal pasting member 12b. The bottom surface of the dent 12) is almost completely covered by the seed crystal 5 when the seed crystal 5 is disposed, and is not exposed to the outside.
[0038]
In addition, since the growth surface of the seed crystal 5 does not become a position recessed from the adjacent lid portion 12a, the carbon gas sublimated from the end of the lid portion 12a adjacent to the seed crystal 5 is absorbed by the seed crystal 5. It is possible not to affect the growth surface.
[0039]
Moreover, since the silicon carbide sticking member 12b is separated from the lid portion 12a and is made thinner than the lid portion 12a, the growth surface temperature of the seed crystal 5 is slightly higher than the surface temperature of the lid portion 12a due to heat conduction. Can be low temperature. For this reason, it is possible to preferentially cause crystal growth on the growth surface of the seed crystal 5.
[0040]
The graphite crucible 1 can be heated by a heater in a vacuum vessel (heating furnace) into which argon gas can be introduced. By adjusting the power of the heater, the temperature of the seed crystal 5 can be adjusted to a silicon carbide raw material. It can be kept at a temperature lower by about 10 to 100 ° C. than the temperature of the powder 2.
[0041]
When the silicon carbide single crystal 7 is grown on the growth surface of the seed crystal 5 using the graphite crucible 1 configured in this way, as shown in FIG. The growth progresses while being expanded, and after the diameter has expanded to a certain extent, the growth proceeds with substantially the same diameter thereafter. At this time, polycrystal 8 is similarly grown along the growth of silicon carbide single crystal 7 from the surface of lid portion 12a. Polycrystal 8 is separated from silicon carbide single crystal 7 by a predetermined distance. It was found that the crystal grew so as to surround the crystal 7. That is, the silicon carbide single crystal 7 grows in a state where it grows in a state where it is buried in the polycrystal 8.
[0042]
As described above, when the single crystal and the polycrystal are grown on the adjacent different growth surfaces (in the case of the present embodiment, the surface of the seed crystal 5 and the surface of the lid portion 12a) having substantially the same height, And the polycrystals can be grown so as not to be fused at a predetermined interval.
[0043]
Thereby, generation | occurrence | production of the crystal defect resulting from a polycrystal adhering to a single crystal can be prevented, and the high quality and large diameter silicon carbide single crystal 7 can be manufactured.
[0044]
Next, experimental results in which the silicon carbide single crystal 7 is actually formed on the surface of the seed crystal 5 using the graphite crucible 1 having the above-described configuration will be described.
[0045]
The growth of the silicon carbide single crystal 7 was performed as follows.
[0046]
First, as the seed crystal 5, a silicon carbide single crystal produced by the Atchison method was cut into a diameter of 10 mm and a thickness of 1 mm, and the surface was mirror finished. At this time, the crystal orientation was determined so that the growth surface of the seed crystal 5 was a (000-1) just surface.
[0047]
And after attaching this seed crystal 5 to the seed crystal sticking member 12a, it attached to the cover part 12a. At this time, the gap d between the seed crystal sticking member 12b and the lid portion 12a of the single crystal manufacturing apparatus was set to 0.5 mm.
[0048]
The lid portion 12a and the seed crystal pasting member 12b were 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, the temperature of the silicon carbide raw material powder 2 is 2290 ° C., the growth surface temperature of the seed crystal 5 is 2230 ° C., and the atmospheric pressure is 1 Torr for 24 hours. Silicon carbide single crystal 7 was grown by the sublimation method.
[0049]
Silicon carbide single crystal 7 thus obtained had a growth height of about 12 mm and a maximum diameter of about 15 mm. Moreover, there was almost no polycrystal generation from the seed crystal sticking member 12b, and the polycrystal 8 generated from the surface of the single crystal manufacturing apparatus around the seed crystal 5 and the grown silicon carbide single crystal 6 could be completely separated. The peripheral portion of the silicon carbide single crystal substrate cut out from the silicon carbide single crystal 7 had almost no polycrystals, cracks or subgrain-like defects caused by fusion with the polycrystals.
[0050]
(Second Embodiment)
The graphite crucible 1 in the present embodiment is different from the first embodiment only in the configuration of the lid member 12, and therefore only the parts different from the first embodiment will be described.
[0051]
FIG. 2 shows a cross-sectional view of the lid member 12 of the graphite crucible 1 as a crystal growth apparatus in the present embodiment. Moreover, the front view and back view of the lid | cover material 12 shown in FIG. 2 are respectively shown to Fig.3 (a) and (b).
[0052]
In the present embodiment, the lid member 12 is composed of a single member, and a substantially circular recess 13 is formed in the center of the lid member 12, and the seed crystal pasting member 12 b in the first embodiment is configured by the recess 13. The seed crystal 5 is arranged in the recess 13.
[0053]
In addition, a notch 14 is formed on the outer periphery of the recess 13 of the lid member 12 up to a predetermined depth of the lid member 12, and the back side of the lid member 12 (opposite surface on which the seed crystal 5 is disposed). The gas vent holes 15 communicating with the notches 14 are formed at a plurality of locations (six locations in FIG. 3).
[0054]
The gas in the graphite crucible 1 is allowed to escape through the notches 14 and the vent holes 15. In addition, the depth of the recess 13 is formed to be equal to or slightly shallower than the thickness of the seed crystal 5, and the width of the notch 14 is between the lid portion 12a and the seed crystal sticking member 12b in the first embodiment. Similarly, the distance d is set.
[0055]
Next, experimental results in which the silicon carbide single crystal 7 is actually formed on the surface of the seed crystal 5 using the graphite crucible 1 having the above-described configuration will be described.
[0056]
First, a seed crystal 5 similar to that used in the experiment of the first embodiment is prepared, this seed crystal 5 is pasted in a recess 13, and a lid 12 is attached to a crucible body 11 in which silicon carbide raw material powder 2 is previously placed. Installed.
[0057]
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 Torr for 24 hours. Silicon carbide single crystal 7 was grown by the sublimation method.
[0058]
Silicon carbide single crystal 7 thus obtained had a growth height of about 15 mm and a maximum diameter of about 15 mm. Part of the sublimation gas that passed through the vent hole 15 adhered to the other part of the graphite crucible 1 and was polycrystallized.
[0059]
Moreover, there was almost no polycrystal generation from the seed crystal sticking member 2, and the polycrystal 8 generated from the surface of the lid 12 around the seed crystal 5 and the grown silicon carbide single crystal 6 could be completely separated.
[0060]
The peripheral portion of the silicon carbide single crystal substrate cut out from the silicon carbide single crystal 7 had almost no polycrystals, cracks or subgrain-like defects caused by fusion with the polycrystals.
[0061]
(Third embodiment)
The graphite crucible 1 in the present embodiment is different from the first embodiment only in the configuration of the lid member 12, and therefore only the parts different from the first embodiment will be described.
[0062]
FIG. 4 shows a cross-sectional view of the lid member 12 of the graphite crucible 1 as a crystal growth apparatus in the present embodiment.
[0063]
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 overhang of the flange portion of the seed crystal sticking member 12b is increased and the lid is covered. The space between the portion 12a and the seed crystal pasting portion 12b is widened, and the porous graphite is filled in the space. The porous graphite has heat insulation properties and can suppress heat conduction from the lid portion 12a to the seed crystal pasting member 12b, and has pores that allow the raw material gas in the graphite crucible 1 to pass therethrough. Material.
[0064]
Other configurations such as the thickness of the seed crystal sticking member 12b are the same as those in the first embodiment.
[0065]
Next, experimental results in which the silicon carbide single crystal 7 is actually formed on the surface of the seed crystal 5 using the graphite crucible 1 having the above-described configuration will be described.
[0066]
First, a seed crystal 5 similar to that used in the experiment of the first embodiment is prepared. Subsequently, the seed crystal sticking 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 sticking member 12b.
[0067]
And the lid | cover material 12 was mounted | worn to the crucible main body 1 which put the silicon carbide raw material powder 2 beforehand.
[0068]
Then, the graphite crucible 1 is placed in a heating furnace, the temperature of the silicon carbide raw material powder 2 is 2290 ° C., the growth surface temperature of the seed crystal 5 is 2230 ° C., and the atmospheric pressure is 1 Torr for 24 hours. Silicon carbide single crystal 7 was grown by the sublimation method.
[0069]
The thus obtained silicon carbide single crystal 7 had a growth height of about 13 mm and a maximum diameter of about 18 mm. The diameter of the silicon carbide single crystal 7 is 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 from the silicon carbide single crystal 7 had almost no polycrystals, cracks or subgrain-like defects caused by fusion with the polycrystals. .
[0070]
(Comparative example)
As a reference, experimental results when a silicon carbide single crystal is grown using the graphite crucible 1 having the conventional structure shown in FIG. 5 are shown.
[0071]
First, a seed crystal 5 having the same configuration as in the first embodiment was prepared. And this seed crystal 5 was affixed on the projection part of the cover part 12 of the graphite crucible 1 as shown in FIG. 5, and was mounted | worn with the crucible main body 1 into which the silicon carbide raw material powder 2 was put beforehand.
[0072]
Then, the graphite crucible 1 is placed in a heating furnace, the temperature of the silicon carbide raw material powder 2 is 2290 ° C., the growth surface temperature of the seed crystal 5 is 2230 ° C., and the atmospheric pressure is 1 Torr for 24 hours. Silicon carbide single crystal 7 was grown by the sublimation method.
[0073]
Silicon carbide single crystal 7 thus obtained had a growth height of about 12 mm and a maximum diameter of about 15 mm.
[0074]
However, the polycrystal 8 is generated around the protrusion, and the polycrystal 8 grows from the polycrystal 8 along the periphery of the silicon carbide single crystal 7. Polycrystalline, cracks, or subgrain-like defects caused by fusion with the polycrystal were observed at the peripheral portion 7a of the silicon carbide single crystal substrate cut out from the silicon carbide single crystal 7.
[0075]
(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 also be used for other crystal growth.
[0076]
In the above embodiment, the graphite crucible 1 itself is used in the single crystal growth apparatus. However, the inner wall of the graphite crucible 1 may be covered with a refractory metal and its carbide. By covering the inner wall of the graphite crucible 1 with a refractory metal in this manner, the silicon carbide single crystal 7 having a uniform Si / C ratio and having no crystal defects can be formed. As the refractory metal carbide, for example, any of hafnium carbide (HfC), tantalum carbide (TaC), zirconium carbide (ZrC), and titanium carbide (TiC) can be used.
[0077]
In the third embodiment, porous graphite is used, but other materials may be used as long as gas can pass therethrough.
[0078]
Furthermore, in the above embodiment, in order to make it difficult for heat transfer to the seed crystal sticking member 12b, porous graphite is disposed between the lid portion 12a and the seed crystal sticking member 12b. A counterbore is provided on the opposite side (hereinafter referred to as the back surface) of the seed crystal pasting portion 12b to the side where the seed crystal 5 is disposed so that the growth surface temperature is lower than the surface temperature of the adjacent lid portion 12a. Also good. Moreover, low temperature gas can be sprayed on the back surface of the seed crystal sticking member 12b, and the growth surface of the seed crystal 5 can also be made lower temperature than the surface of the cover part 12a. At this time, the low temperature gas may be the same as the inert gas introduced into the graphite crucible 1 during crystal growth. And when forming a desired dope single crystal as the silicon carbide single crystal 7, you may make it contain the element required for dope in the inert gas sprayed on the seed crystal sticking member 12b. For example, N (nitrogen), B (boron), Al (aluminum), P (phosphorus), As (arsenic), or the like is included in the inert gas as an element to be doped.
[Brief description of the drawings]
FIG. 1 is a diagram showing a cross-sectional configuration of a graphite crucible 1 in a first embodiment of the present invention.
FIG. 2 is a diagram showing a cross-sectional configuration of a lid member 12 in a second embodiment of the present invention.
3A is a front view of the lid member 12 shown in FIG. 2, and FIG. 3B is a rear view of the lid member 12 shown in FIG.
FIG. 4 is a diagram showing a cross-sectional configuration of a lid member 12 according to a third embodiment of the present invention.
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 the lid 12 of the graphite crucible 1 shown in FIG. 5A.
[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, 12a ... Lid, 12b ... Seed crystal sticking member,
13 ... dent, 14 ... notch, 15 ... gas vent.

Claims (18)

It has a crucible (1) provided with a container (11, 12a) in which a seed crystal sticking member (12b) is arranged on one surface, and attaches the seed crystal (5) to the surface of the seed crystal sticking member, A single crystal manufacturing apparatus for growing a single crystal on a growth surface of the seed crystal by introducing a single crystal source gas to be grown in a growth space in a crucible,
The seed crystal affixing member is surrounded by the container, and is disposed with a predetermined gap between the container and an end surface of the portion of the container surrounding the seed crystal affixing member. It is configured so that the source gas can be extracted,
The surface to which the seed crystal is attached of the seed crystal sticking member is positioned so as to be recessed from one surface of the container in which the seed crystal sticking member is disposed, and when the seed crystal is attached, The single crystal manufacturing apparatus, wherein the seed crystal and the container do not expose the growth space. 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 smaller than 1 mm along the shape of the seed crystal sticking member. The single crystal manufacturing apparatus according to claim 1 . The single-piece | unit of Claim 1 or 2 provided with the heat insulation member which suppresses the heat transfer from the said container to the said seed crystal sticking member between the said seed crystal sticking member and the said container. Crystal manufacturing equipment. The single-crystal manufacturing apparatus according to claim 3 , wherein the heat insulating member is a material through which the source gas can pass. The single crystal manufacturing apparatus according to claim 4, wherein the heat insulating member is porous graphite. Growth surface of the seed crystal can be of any claims 1 to 5, characterized in that the seed crystal adhering member protrudes either flush with, or slightly weight to one side of the container which is arranged The single-crystal manufacturing apparatus as described in any one. The shape of the seed crystal sticking member and the container is configured such that 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 sticking member is disposed. single crystal manufacturing apparatus according to any one of claims 1 to 6, wherein. The single crystal manufacturing apparatus according to claim 7 , wherein a counterbore is provided on a side opposite to a surface on which the seed crystal is attached in the seed crystal sticking member. In the single crystal manufacturing apparatus according to any one of claims 1 to 8 ,
The crucible is made of a carbon material, and a silicon carbide single crystal is grown on a growth surface of the seed crystal made of silicon carbide. The single crystal manufacturing apparatus according to claim 9 , wherein one surface of the container in which the seed crystal sticking member is disposed is coated with a refractory metal carbide. It said refractory metal carbide, hafnium carbide (HfC), tantalum carbide (TaC), zirconium carbide (ZrC), in claim 10, characterized in that it is composed of at least one of titanium carbide (TiC) The silicon carbide single crystal manufacturing apparatus as described. After attaching the seed crystal (5) to the surface of the seed crystal sticking member of the crucible (1) provided with the container (11, 12a) in which the seed crystal sticking member (12b) is disposed on one surface, the inside of the crucible A single crystal manufacturing method in which a single crystal source gas and an inert gas to be grown in a growth space are introduced, the source gas is supplied to the seed crystal, and a single crystal is grown on the growth surface of the seed crystal. There,
Surrounding the seed crystal affixing member with the container, and placing the seed crystal affixing member with a predetermined gap between the end surface of the container surrounding the seed crystal affixing member, and drawing the source gas in the growth space through the gap, And the surface to which the said seed crystal is attached among the said seed crystal sticking members is located so that it may dent rather than the one surface of the said container by which this seed crystal sticking member was arrange | positioned, and the said seed crystal is said seed crystal sticking member The single crystal is grown on the seed crystal by covering the entire surface with the seed crystal and the container when attached to the single crystal, so that the single crystal is surrounded by a polycrystal at a predetermined interval. A method of manufacturing a single crystal comprising performing embedded growth in which the single crystal and the polycrystal are grown together while being surrounded by a circle . 13. The method for producing a single crystal according to claim 12 , 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 sticking member is disposed. The single crystal manufacturing method according to claim 13 , wherein a low-temperature gas is sprayed on the opposite side of the surface to which the seed crystal is attached, of the seed crystal sticking member. 15. The method for producing a single crystal according to claim 14 , wherein the same inert gas as the inert gas introduced into the growth space of the crucible is used as the low temperature gas. The inert gas that 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 that becomes the impurity of the single crystal is mixed in the inert gas. Item 16. A method for producing a single crystal according to Item 15 . The single element according to claim 16 , wherein at least one of N (nitrogen), B (boron), Al (aluminum), P (phosphorus), and As (arsenic) is used as the impurity element. Crystal manufacturing method. The method for producing a single crystal according to any one of claims 12 to 17 ,
Silicon carbide is used as the seed crystal, and a silicon carbide single crystal is grown on the growth surface of the seed crystal by introducing a silicon carbide source gas as the source gas into the growth space of the crucible. Silicon single crystal manufacturing method.

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