METHOD AND APPARATUS FOR MANUFACTURING SILICON CARBIDE SINGLE CRYSTAL

Abstract

A method for manufacturing a silicon carbide single crystal by sublimating a silicon carbide raw material to grow a silicon carbide single crystal on a seed crystal substrate in an apparatus for growing a silicon carbide single crystal, the apparatus including at least a growth container and a heat-insulating container that surrounds the growth container and has a hole for temperature measurement. The method includes: measuring a temperature of the growth container via the hole for temperature measurement when the silicon carbide single crystal is grown; and blocking the hole for temperature measurement with a blocking member when the silicon carbide single crystal is cooled after the growth of the silicon carbide single crystal is ended. Consequently, a method and apparatus for manufacturing a silicon carbide single crystal are provided to reduce breaking and cracking of the silicon carbide single crystal ingot and wafer.

Claims

1-5. (canceled)

6. A method for manufacturing a silicon carbide single crystal by sublimating a silicon carbide raw material to grow a silicon carbide single crystal on a seed crystal substrate in an apparatus for growing a silicon carbide single crystal, the apparatus including at least a growth container and a heat-insulating container that surrounds the growth container and has a hole for temperature measurement, the method comprising: measuring a temperature of the growth container via the hole for temperature measurement when the silicon carbide single crystal is grown; and blocking the hole for temperature measurement with a blocking member when the silicon carbide single crystal is cooled after the growth of the silicon carbide single crystal is ended.

7. An apparatus for manufacturing a silicon carbide single crystal by growing the silicon carbide single crystal by a sublimation method, the apparatus comprising at least: a growth container; a heat-insulating container surrounding the growth container and having a hole for temperature measurement; a heating heater; and a blocking member configured to block the hole for temperature measurement.

8. The apparatus for manufacturing a silicon carbide single crystal according to claim 7, wherein the blocking member comprises any material of carbon, titanium, and tantalum.

9. The apparatus for manufacturing a silicon carbide single crystal according to claim 8, wherein the blocking member further comprises a heat-insulating material having a carbon fiber, an alumina fiber, or a porous structure.

10. The apparatus for manufacturing a silicon carbide single crystal according to claim 7, comprising a movement mechanism configured to raise, lower, rotate, or slide the blocking member configured to block the hole for temperature measurement.

11. The apparatus for manufacturing a silicon carbide single crystal according to claim 8, comprising a movement mechanism configured to raise, lower, rotate, or slide the blocking member configured to block the hole for temperature measurement.

12. The apparatus for manufacturing a silicon carbide single crystal according to claim 9, comprising a movement mechanism configured to raise, lower, rotate, or slide the blocking member configured to block the hole for temperature measurement.

Description

BRIEF DESCRIPTION OF DRAWINGS

[0032] FIG. 1 is a flowchart showing an example of the inventive method for manufacturing a silicon carbide single crystal.

[0033] FIG. 2 is a schematic cross-sectional view showing an example of the inventive apparatus for manufacturing a silicon carbide single crystal.

[0034] FIG. 3 is a schematic view for illustrating a case where a blocking member according to the present invention is slid to block a hole for temperature measurement.

[0035] FIG. 4 is a schematic view for illustrating a case where a blocking member according to the present invention is raised and lowered to block the hole for temperature measurement.

[0036] FIG. 5 shows a photograph for showing an exemplar wafer produced in Example.

[0037] FIG. 6 shows photographs for showing exemplar wafers produced in Comparative Example.

[0038] FIG. 7 is a graph showing stress distributions in the wafers of Example and Comparative Example.

[0039] FIG. 8 is a schematic cross-sectional view showing an example of a conventional apparatus for manufacturing a silicon carbide single crystal.

[0040] FIG. 9 is a flowchart showing an example of a conventional method for manufacturing a silicon carbide single crystal.

[0041] FIG. 10 is a schematic cross-sectional view showing heat transfer and temperature distribution in the vicinity of a hole for temperature measurement in the conventional method and apparatus for manufacturing a silicon carbide single crystal.

[0042] FIG. 11 is a schematic cross-sectional view showing a temperature distribution inside a SiC single crystal ingot that is grown by the conventional method and apparatus for manufacturing a silicon carbide single crystal.

DESCRIPTION OF EMBODIMENTS

[0043] As described above, when a SiC single crystal is manufactured using a conventional apparatus for manufacturing a SiC single crystal, there have been problems that the SiC single crystal ingot is cracked, and the wafer is broken or cracked during slicing process.

[0044] The present inventors have diligently studied to solve the problems and consequently found that when a SiC single crystal ingot is being cooled, blocking a hole for temperature measurement can prevent heat radiation through the hole, and thereby make the temperature inside the ingot uniform during the cooling, so that the breaking and cracking of the SiC single crystal ingot and wafer are successfully reduced. This finding has led to the completion of the present invention.

[0045] Hereinafter, the present invention will be described in detail with reference to the drawings as an example of embodiments. However, the present invention is not limited thereto.

[0046] FIG. 1 is a flowchart showing an example of the inventive method for manufacturing a silicon carbide single crystal.

[0047] FIG. 2 is a schematic cross-sectional view of an example of the inventive apparatus for manufacturing a silicon carbide single crystal.

[0048] First, the inventive apparatus for manufacturing a silicon carbide single crystal will be described.

[0049] As shown in FIG. 2, an apparatus 1 for manufacturing a silicon carbide single crystal according to the present invention includes a growth container 4 which is made of carbon graphite, and which has a container main body for housing a SiC raw material 2 and a lid on which a SiC seed substrate 3 is disposed. Moreover, the apparatus 1 for manufacturing a silicon carbide single crystal includes a heat-insulating container 5 made of a heat-insulating material outside the growth container 4, and further includes, outside the heat-insulating container 5, an external container 6 such as a quartz tube or a vacuum chamber for reducing the pressure of the growth container 4, and a heater 7 for heating the SiC raw material 2. Furthermore, the apparatus 1 includes a thermometer 8 such as a temperature-measurement sensor for measuring the temperature inside the growth container 4. The heat-insulating container 5 has a hole 9 for temperature measurement in a top portion thereof. Additionally, the apparatus 1 includes a supply port for supplying an inert gas such as Ar and a discharge port for discharging the inert gas, which are not shown, during SiC crystal growth. The configuration described so far is substantially the same as that of the conventional apparatus. Nevertheless, in the present invention, a blocking member 10 configured to block the hole 9 for temperature measurement in the heat-insulating container 5 is installed.

[0050] This blocking member 10 is configured to be movable such that: the hole 9 for temperature measurement is opened so as to enable the temperature measurement of the growth container 4 through the hole 9 when a SiC single crystal is grown; and the hole 9 is closed when the growth is ended and the single crystal is cooled.

[0051] In addition, a movement mechanism for the blocking member 10 is not particularly limited, and can be such a mechanism configured to raise, lower, rotate, or slide the blocking member 10 with a motor, a hydraulic cylinder, an air cylinder, etc. For example, FIG. 3 shows a case where the blocking member 10 is slid, and FIG. 4 shows a case where the blocking member 10 is raised and lowered and thereby fitted into the hole.

[0052] The blocking member 10 can be made of a material such as carbon, titanium, or tantalum. These materials are capable of withstanding a high temperature of 2000° C. or more and blocking radiant light at the high temperature under vacuum.

[0053] Additionally, the blocking member 10 preferably further contains a heat-insulating material composed of a carbon fiber, a heat-insulating material composed of an alumina fiber, or a heat-insulating material having a porous structure such as carbon foam. The blocking member containing such a heat-insulating material improves the heat-insulating effect and allows the temperature in the crystal to be more uniform during the cooling.

[0054] As described above, the inventive apparatus for manufacturing a silicon carbide single crystal is capable of easily blocking the hole 9 for temperature measurement with the blocking member 10 when a silicon carbide single crystal ingot 11 is cooled, thereby preventing heat radiation through the hole 9 during the cooling of the silicon carbide single crystal. This enables the temperature inside the silicon carbide single crystal to be uniform during the cooling. Thus, the silicon carbide single crystal has less residual strain, and the breaking and cracking are successfully suppressed.

[0055] Next, description will be given of the inventive method for manufacturing a silicon carbide single crystal with the inventive apparatus for manufacturing a silicon carbide single crystal described above.

[0056] As described in FIG. 1(a), the raw material 2 and the seed substrate 3 are disposed in the growth container 4. Next, as described in FIG. 1(b), the growth container 4 is disposed in the heat-insulating container 5. Next, as described in FIG. 1(c), the heat-insulating container 5 as a whole is disposed in the external container 6. Next, as described in FIG. 1(d), the inside of the external container 6 is made vacuum, and the temperature is raised while a predetermined pressure is being kept. Preferably, in this event, the temperature is 2000° C. or more, and the pressure is 100 Torr (1.3×10.sup.2 hPa) or less. Next, as described in FIG. 1(e), the SiC single crystal 11 is grown by a sublimation method. Note that when the SiC single crystal is grown, the temperature of the growth container 4 is measured via the hole 9 for temperature measurement provided in the heat-insulating container 5. In other words, the hole 9 for temperature measurement is opened during the SiC single crystal growth.

[0057] Finally, as described in FIG. 1(f), the growth is stopped by increasing the vacuum back pressure and decreasing the partial pressure of the sublimated gas as performed in the stopping process of a typical sublimation method. In the sublimation method described so far, the temperature is raised and the pressure is controlled in the same manner as in a typical conventional sublimation method. After the crystal growth is stopped, the hole 9 for temperature measurement is covered with the blocking member 10 as shown in FIG. 2.

[0058] According to the manufacturing method as described above, when the grown SiC single crystal ingot 11 is cooled, the hole 9 for temperature measurement is blocked. This makes it possible to prevent heat radiation through the hole 9, and the temperature inside the SiC single crystal ingot 11 is made uniform during the cooling. From this state, the resultant is restored to ambient temperature, so that a SiC single crystal ingot with less residual strain can be obtained. In this way, the inventive manufacturing method makes it possible to reduce the residual strain of the SiC single crystal ingot, and suppress the breaking and cracking.

EXAMPLE

[0059] Hereinafter, the present invention will be more specifically described by showing Example and Comparative Example. However, the present invention is not limited thereto.

Example

[0060] Using the apparatus 1 for manufacturing a silicon carbide single crystal shown in FIG. 2, a SiC single crystal with a diameter of 4 inches (100 mm) was grown under the following growth conditions by the inventive method for manufacturing a silicon carbide single crystal.

<Conditions>

[0061] Seed crystal substrate . . . SiC single crystal substrate with a diameter of 4 inches (100 mm) having a main surface tilted from the {0001} plane by 4° in the <11-20> direction [0062] Growth temperature . . . 2200° C. [0063] Pressure . . . 10 Torr (1.3×10 hPa) [0064] Atmosphere . . . argon and nitrogen gases

[0065] According to the procedure as described in FIG. 1, the hole 9 for temperature measurement was blocked with the blocking member 10 when a grown SiC single crystal was cooled. In this way, five SiC single crystal ingots were consequently prepared. As a result of examining the crack formation statuses of the five SiC single crystal ingots, no crack was formed in any of the five ingots. Four among these ingots were each sliced into four wafers to examine the crack formation statuses, and no crack was formed in all of the 16 wafers. FIG. 5 shows a photograph of such a wafer. Moreover, FIG. 7 shows the result of examining the stress distribution of the wafer. The stress distribution was measured by the Raman spectroscopy, and shown as relative stresses based on a small piece of SiC with no stress.

Comparative Example

[0066] Five SiC single crystal ingots were prepared according to the procedure described in FIG. 9. The conditions were the same as those in Example, except that the hole for temperature measurement was not blocked during the cooling.

[0067] As a result of examining the crack formation statuses of the five SiC single crystal ingots, cracking was observed from one among the five ingots. Each of the four ingots with no cracks was sliced into four wafers to examine the crack formation statuses, and cracks were formed in all of the 16 wafers. Photographs of such wafers are shown in FIGS. 6(a) (b). Moreover, FIG. 7 shows the result of examining the stress distributions of the wafers.

[0068] As apparent from the result shown in FIG. 7, unlike Comparative Example, the stress is not increased at positions apart from the center of the wafer in Example. This indicates that the inventive method and apparatus for manufacturing a silicon carbide single crystal make it possible to obtain a SiC single crystal ingot with less residual strain.

[0069] Moreover, it was found as described above that the present invention successfully reduces the breaking and cracking of the manufactured silicon carbide single crystal ingots in comparison with Comparative Example.

[0070] Further, FIGS. 5 and 6 revealed that the present invention successfully suppresses the breaking and cracking of the wafers.

[0071] It should be noted that the present invention is not limited to the above-described embodiments. The embodiments are just examples, and any examples that have substantially the same feature and demonstrate the same functions and effects as those in the technical concept disclosed in claims of the present invention are included in the technical scope of the present invention.