PRODUCTION METHOD FOR AN SIC VOLUME MONOCRYSTAL OF INHOMOGENEOUS SCREW DISLOCATION DISTRIBUTION AND SIC SUBSTRATE
20240003054 · 2024-01-04
Inventors
- Bernhard Ecker (Nürnberg, DE)
- Ralf Müller (Nürnberg, DE)
- Matthias Stockmeier (Nürnberg, DE)
- Michael Vogel (Nürnberg, DE)
- Arnd-Dietrich Weber (Nürnberg, DE)
Cpc classification
International classification
C30B23/06
CHEMISTRY; METALLURGY
Abstract
An SiC volume monocrystal is processed by sublimation growth. An SiC seed crystal is placed in a crystal growth region of a growing crucible and SiC source material is introduced into an SiC storage region. During growth, at a growth temperature of up to 2,400 C. and a growth pressure between 0.1 mbar and 100 mbar, an SiC growth gas phase is generated by sublimation of the SiC source material and by transport of the sublimated gaseous components into the crystal growth region, where an SiC volume monocrystal grows by deposition from the SiC growth gas phase on the SiC seed crystal. A mechanical stress is introduced into the SiC seed crystal at room temperature prior to the start of the growth to cause seed screw dislocations present in the SiC seed crystal to undergo a dislocation movement so that seed screw dislocations recombine.
Claims
1. A method for producing at least one SiC volume monocrystal by sublimation growth, the method comprising: a) prior to a start of the growth: a1) arranging an SiC seed crystal having a growth surface in a crystal growth region of a growing crucible; and a2) introducing SiC source material into an SiC storage region of the growing crucible; and b) during the growth at a growth temperature of up to 2400 C. and a growth pressure between 0.1 mbar and 100 mbar by means of a sublimation of the SiC source material and by way of a transport of sublimated gaseous components into the crystal growth region, producing an SiC growth gas phase in the crystal growth region, in which an SiC volume monocrystal grows on the SiC seed crystal by deposition from the SiC growth gas phase; and c) prior to the start of the growth, introducing a mechanical stress into the SiC seed crystal at room temperature in order to cause seed screw dislocations present in the SiC seed crystal to undergo a dislocation movement under an influence of the mechanical stress, to cause seed screw dislocations which approach each other in connection with respective dislocation movements thereof to recombine with each other and cancel each other out.
2. The method according to claim 1, which comprises thermally activating the dislocation movements of the seed screw dislocations by heating the SiC seed crystal.
3. The method according to claim 1, which comprises introducing the mechanical stress rotationally symmetrically into the SiC seed crystal.
4. The method according to claim 1, which comprises introducing the mechanical stress by bending the SiC seed crystal.
5. The method according to claim 1, which comprises bending the SiC seed crystal to introduce the mechanical stress with a maximum bending distance between 0.1 mm and 5 mm.
6. The method according to claim 1, which comprises bending the SiC seed crystal by way of at least one punch to introduce the mechanical stress.
7. The method according to claim 6, which comprises placing the at least one punch centrally to act on a center of the SiC seed crystal.
8. The method according to claim 6, wherein the at least one punch is one of several punches acting on the SiC seed crystal.
9. The method according to claim 8, which comprises placing at least a portion of the punches along a notional circular line around a center of the SiC seed crystal.
10. The method according to claim 9, which comprises placing the punches equidistantly along the notional circular line around the center of the SiC seed crystal.
11. The method according to claim 1, wherein the step of introducing the mechanical stress into the SiC seed crystal comprises firmly connecting the SiC seed crystal to an uneven contact surface of a shaped seed holder.
12. A monocrystalline SiC substrate, comprising: a total main surface, said total main surface having an accumulation sub-area formed by at most 20% of said total main surface, and said accumulation sub-area comprising at least 80% of all substrate screw dislocations present on said total main surface.
13. The SiC substrate according to claim 12, wherein said accumulation sub-area has at least 85% of all substrate screw dislocations that are present on said total main surface.
14. The SiC substrate according to claim 12, wherein said accumulation sub-area has at least 90% of all substrate screw dislocations that are present on said total main surface.
15. The SiC substrate according to claim 12, wherein said accumulation sub-area has a size of at most 15% of said total main surface.
16. The SiC substrate according to claim 12, wherein the SiC substrate has a total screw dislocation density of at most 1000 per cm.sup.2.
17. The SiC substrate according to claim 12, wherein the SiC substrate has a total screw dislocation density of at most 500 per cm.sup.2.
18. The SiC substrate according to claim 12, wherein said total main surface has a substrate diameter of at least 150 mm.
19. The SiC substrate according to claim 12, wherein said total main surface has a substrate diameter of at least 200 mm.
20. The SiC substrate according to claim 12, wherein the SiC substrate has an SiC crystal structure with only one single SiC polytype.
21. The SiC substrate according to claim 12, wherein the SiC substrate has an SiC crystal structure with one SiC polytype selected from the group consisting of 4H, 6H, 15R and 3C.
22. The SiC substrate according to claim 12, wherein the SiC substrate has an electrical resistivity of 8 mcm to 26 mcm.
23. The SiC substrate according to claim 22, wherein the electrical resistivity of the SiC substrate is 10 mcm to 24 mcm.
Description
BRIEF DESCRIPTION OF THE FIGURES
[0043]
[0044]
[0045]
[0046]
[0047]
[0048]
[0049]
[0050]
[0051]
DETAILED DESCRIPTION OF THE INVENTION
[0052] Parts that correspond to each other are marked with the same reference signs in
[0053]
[0054] In the region of a crucible end wall 7 of the growing crucible 3 opposite the SiC storage region 4, an SiC seed crystal 8 extending axially into the crystal growth region 5 is attached. The manner in which the latter is attached will be described in more detail below. The SiC seed crystal 8 is in particular monocrystalline. In the exemplary embodiment shown, the crucible end wall 7 is formed as the crucible lid of the growing crucible 3. However, this is not mandatory. The SiC volume monocrystal 2 to be grown grows on the SiC seed crystal 8 by means of deposition from an SiC growth gas phase 9 forming in the crystal growth region 5. The growing SiC volume monocrystal 2 and the SiC seed crystal 8 have approximately the same diameter. If at all, there is a deviation of at most 10% by which a seed diameter of the SiC seed crystal 8 is smaller than a monocrystal diameter of the SiC volume monocrystal 2. However, a gap not shown in
[0055] In the exemplary embodiment according to
[0056] The thermally insulated growing crucible 3 is placed inside a tubular container 11, which in the exemplary embodiment is designed as a quartz glass tube and forms an autoclave or reactor. For heating the growing crucible 3, an inductive heating device in the form of a heating coil 12 is arranged around the container 11. The growing crucible 3 is heated to the temperatures required for growth by means of the heating coil 12. In the exemplary embodiment shown, these growth temperatures are at least 2,250 C. The heating coil 12 inductively couples an electric current into the electrically conductive crucible side wall 13 of the growing crucible 3. This electric current flows substantially as a circular current in the circumferential direction within the circular and hollow cylindrical crucible side wall 13, thereby heating the growing crucible 3. If needed, the relative position between the heating coil 12 and the growing crucible 3 can be changed axially, i.e., in the direction of a central longitudinal axis 14 of the growing SiC volume monocrystal 2, in particular in order to adjust and, if necessary, also change the temperature or the temperature profile within the growing crucible 3. The axially variable position of the heating coil 12 during the growth process is indicated in
[0057] The SiC growth gas phase 9 in the crystal growth region 5 is fed by the SiC source material 6. The SiC growth gas phase 9 contains at least gas components in the form of Si, Si.sub.2C and SiC.sub.2 (SiC gas species). The material transport from the SiC source material 6 to a growth interface 16 at the growing SiC volume monocrystal 2 takes place on the one hand along an axial temperature gradient. In the sublimation method (=PVT method) used for SiC crystal growth, the growth conditions including the material transport are adjusted and controlled via the temperatures prevailing in the growing crucible 3. At the growth interface 16 there is a relatively high growth temperature of at least 2,250 C., in particular even of at least 2,350 C. or 2,400 C.. Furthermore, an axial temperature gradient of at least 5 K/cm, preferably of at least 15 K/cm, measured in the direction of the central longitudinal axis 14, is set at the growth interface 16 in particular. The temperature within the growing crucible 3 decreases towards the growing SiC volume monocrystal 2. The highest temperature of approximately 2,450 C. to 2,550 C. prevails in the region of the SiC storage region 4. This temperature profile with a temperature difference of in particular 100 C. to 150 C. between the SiC storage region 4 and the growth interface 16 can be achieved by various measures. For example, axially varying heating can be provided by dividing the heating coil 12 into two or more axial sections, which is not shown in more detail. Furthermore, a stronger heating effect can be set in the lower section of the growing crucible 3 than in the upper section of the growing crucible 3, e.g., by a corresponding axial positioning of the heating coil 12. Moreover, the thermal insulation can be designed differently at the two axial crucible end walls. As schematically indicated in
[0058] In addition, a growth pressure of in particular 0.1 hPa (=mbar) to 10 hPa (=mbar) prevails in the growing crucible 3 during the actual crystal growth.
[0059] The SiC volume monocrystal 2 grows on a growth surface 18 of the SiC seed crystal 8. Said growth takes place in a growth direction 19, which in the exemplary embodiment shown in
[0060] The growing SiC volume monocrystal 2 has an SiC crystal structure of the 4H polytype. In principle, however, another polytype (=another crystal modification), such as 6H-SiC, 3C-SiC or 15R-SiC, is also possible. Advantageously, the SiC volume monocrystal 2 has only one SiC polytype, which in the exemplary embodiment is said 4H-SiC. The SiC volume monocrystal 2 grows with a high modification stability and in this respect has essentially only one single polytype. The latter is favorable with regard to a very low defect high crystal quality.
[0061] The growth method carried out by means of the growth arrangement 1 to produce the SiC volume monocrystal 2 is also characterized in other respects by a high crystal quality that is achieved. For instance, within any cross-sectional area perpendicular to the growth direction 19, the growing SiC volume monocrystal 2 has an inhomogeneous distribution of volume monocrystal screw dislocations 20 (see
[0062] This high quality of the SiC volume monocrystal 2 is also due to the underlying SiC seed crystal 8, which has a similar favorable inhomogeneous distribution of its seed screw dislocations 24 as the SiC volume monocrystal 2 growing thereon during the subsequent growth. In particular, the seed screw dislocations 24 present in the SiC seed crystal 8 continue in the growth direction 19 in the growing SiC volume monocrystal 2, which is shown in the representation according to
[0063] In this respect, it is favorable if the SiC seed crystal 8 has, in particular at the latest at the time when the actual growth of the SiC volume monocrystal 2 starts, a distribution of its seed screw dislocations 24 and/or a total seed screw dislocation density related to its growth surface 18, which should and can be inherited at least approximately in this form in the SiC volume monocrystal 2.
[0064] In order to achieve this, the SiC seed crystal 8 is subjected to a treatment prior to its use for growing the SiC volume monocrystal 2, which leads to an at least partial recombination and mutual cancellation of the seed screw dislocations 24 that may still be quite numerous in the SiC seed crystal 8 at this initial stage. For this purpose, the SiC seed crystal 8 is preferably subjected to a mechanical stress while still at room temperature and then heated in particular. This leads to a dislocation movement of initially existing seed screw dislocations 24. In the course of this dislocation movement, seed screw dislocations 24 with opposing Burgers vectors can approach each other to such an extent that recombination and mutual cancellation of the respective pair of seed screw dislocations 24 occurs. This advantageous selective reduction of the seed screw dislocations 24 is thus mechanically induced (by the mechanical stress introduced into the SiC seed crystal 8) and thermally activated (by the thermal treatment carried out thereafter). During the thermal treatment that initiates the favorable dislocation movement, the mechanically strained SiC seed crystal 8 is brought to a temperature of up to 200 C. below the growth temperature that will later prevail on the SiC seed crystal 8 during the actual growth. For example, the treatment temperature is about 2,100 C. This thermal treatment preferably lasts about 200 minutes. After completion of this upstream treatment, the SiC seed crystal 8 has the favorable inhomogeneous distribution of the seed screw dislocations 24 indicated by the example in the representation according to
[0065] Examples for introducing the advantageous mechanical stress into the seed crystal 8 are described below.
[0066]
[0067] The adjustable punch 28 has a cylindrical shape. Its punch tip, which presses against the back of the holding plate 27, can have different shapes. Three exemplary embodiments are shown in
[0068] In
[0069] In
[0070] By means of the seed holders 25 and 31, the bow of the SiC seed crystal 8 can only be adjusted during the pre-treatment to reduce the seed screw dislocations 24 present in the SiC seed crystal. After completion of the pre-treatment, the punches 28, 32 can be retracted and the seed holder 25 or 31 including the SiC seed crystal 8 attached thereto can be returned to the unbent state, in which the actual growth of the SiC volume monocrystal 2 is then subsequently carried out.
[0071] In contrast, there are further exemplary embodiments shown in
[0072] If necessary, the SiC seed crystal 8 can first be examined for the presence of seed screw dislocations 24. This examination is carried out e.g., by X-ray topography. A sub-region that has been found to be particularly loaded with seed screw dislocations 24 during this examination can then be selectively subjected to a mechanical stress in order to reduce the unusually (or above-average) high number of seed screw dislocations 24 especially there.
[0073] Overall, the growth arrangement 1 in conjunction with the described different variants for reducing the seed screw dislocations 24 present in the SiC seed crystal 8 enables the growth of a high-grade SiC volume monocrystal 2 which has only a few volume monocrystal screw dislocations 20, wherein the latter are inhomogeneously distributed and preferably concentrated within the accumulation sub-region 21, which can advantageously be left out in the further use of the SiC volume monocrystal 2 for the production of high-grade electronic components.
[0074] From these high-grade SiC volume monocrystals 2, equally high-grade SiC substrates 38, 39 (see schematic plan view representations according to
[0075] In the SiC substrate 38 according to
[0076] In the case of the SiC substrate 39 according to
[0077] In the case of the SiC substrates 38, 39, the respective utilization sub-region 45 or 47 is significantly larger than the respective accumulation sub-region 44 or 46. The respective accumulation sub-region 44 or 46 has an associated accumulation sub-region 48 or 49, which is part of the respective total main surface 41 or 42 and accounts for at most 20% thereof. Nevertheless, at least 80% of all substrate screw dislocations 43 present on the associated total main surface 41 or 42 are located within this accumulation sub-region 48 or 49. The boundary between the smaller accumulation sub-region 44 or 46 and the larger usage sub-region 45 or 47 intended for further use is indicated in