Production method and growth arrangement for producing a bulk SiC single crystal by arranging at least two insulation cylinder components to control a variation in a volume element density
11261536 · 2022-03-01
Assignee
Inventors
- Bernhard Ecker (Nuremberg, DE)
- Ralf Mueller (Zirndorf, DE)
- Matthias Stockmeier (Egloffstein, DE)
- Michael Vogel (Nuremberg, DE)
- Arnd-Dietrich Weber (Forchheim, DE)
Cpc classification
C30B23/06
CHEMISTRY; METALLURGY
International classification
C30B23/06
CHEMISTRY; METALLURGY
Abstract
A bulk SiC single crystal is produced by placing an SiC seed crystal in a crystal growth region of a growth crucible, and introducing SiC source material into an SiC reservoir region, and the bulk SiC single crystal is grown on from an SiC growth gas phase by deposition. The growth crucible is surrounded by an insulation that extends rotationally symmetrically and axially towards the central middle longitudinal axis. The insulation has mutually concentric insulation cylinder components and the insulation is notionally divided into insulation ring segments that are in turn notionally divided into volume elements. The insulation cylinder components are selected and positioned relative to one another such that every volume element of the insulation ring segment in question has a volume element density varying by not more than 10% from an average insulation ring segment density of the insulation ring segment in question.
Claims
1. A method of producing a bulk SiC single crystal by sublimation growth, the method comprising: a) prior to a commencement of a growing process, placing at least one SiC seed crystal in a crystal growth region of a growth crucible, and introducing SiC source material into a SiC reservoir region of the growth crucible, b) during the growing process, generating an SiC growth gas phase in the crystal growth region by sublimation of the SiC source material and by transporting sublimed gaseous components into the crystal growth region, and growing the bulk SiC single crystal having a central middle longitudinal axis onto the SiC seed crystal by deposition from an SiC growth gas phase; wherein: c) the growth crucible, prior to commencement of the growing process, is surrounded by an insulation that extends in a rotationally symmetric manner and axially in a direction of a central middle longitudinal axis and that has at least two insulation cylinder components; and wherein: c1) the at least two insulation cylinder components are in a mutually concentric arrangement with one inside another, and each of the at least two insulation cylinder components has a wall thickness measured in a radial direction; c2) the insulation is notionally divided into multiple insulation ring segments arranged successively and axially in the direction of the central middle longitudinal axis; c3) each of the insulation ring segments is in turn notionally divided into multiple volume elements arranged alongside one another in a tangential direction; c4) each of the insulation ring segments has an average insulation ring segment density measured over respective wall thicknesses of all of the at least two insulation cylinder components; and c5) the at least two insulation cylinder components, each of which have variances in density in sub-regions, are selected and positioned relative to one another in such a way that every volume element of the insulation ring segment in question has a volume element density varying by not more than 10% from the average insulation ring segment density of the insulation ring segment in question; and c6) every volume element extends in axial direction over an axial element length which is equal to an axial segment length of the insulation ring segment and is up to 50 mm, in circumferential direction over an outer tangential element length of up to 50 mm, and in radial direction over a sum of all wall thicknesses of the at least two insulation cylinder components.
2. The method according to claim 1, which comprises choosing an insulation material having a material density between 0.05 g/cm.sup.3 and 0.5 g/cm.sup.3 for the insulation.
3. The method according to claim 2, which comprises choosing an insulation material having a material density between 0.1 g/cm.sup.3 and 0.2 g/cm.sup.3 for the insulation.
4. The method according to claim 1, which comprises, prior to the commencement of the growing process, determining a density by way of an x-ray method of the at least two insulation cylinder components.
5. The method according to claim 1, which comprises selecting the at least two insulation cylinder components and positioning the at least two insulation cylinder components relative to one another such that every volume element of the insulation ring segment in question has a volume element density varying by no more than 5% from the average insulation ring segment density of the insulation ring segment in question.
6. The method according to claim 1, which comprises choosing the respective insulation ring segment and the volume elements of the insulation ring segment such that the axial element length of the volume elements is 20 mm and the outer tangential element length of the volume elements is 20 mm.
7. The method according to claim 1, wherein the radial wall thickness of the at least two insulation cylinder components in each case lies in a range between 5 mm and 50 mm.
8. The method according to claim 7, wherein the radial wall thickness of the at least two insulation cylinder components in each case lies in a range between 10 mm and 20 mm.
9. The method according to claim 1, wherein a quotient of two of the radial wall thicknesses of the at least two insulation cylinder components lies in a range between 0.5 and 2.
10. The method according to claim 1, which comprises constructing the insulation in such a way that two mutually adjacent insulation cylinder components of the at least two insulation cylinder components are radially separated by a distance in a range between 0.1 mm and 5 mm.
11. The method according to claim 10, wherein the at least two insulation cylinder components are separated by a distance between 1 mm and 2 mm.
12. A growth arrangement for producing at least one bulk SiC single crystal by sublimation growth, the growth arrangement comprising: a) a growth crucible having a crystal growth region for accommodating an SiC seed crystal and an SiC reservoir region for accommodating SiC source material; and b) a heating device for heating the growth crucible, to cause, during growth, a sublimation of the SiC source material, a transport of sublimed gaseous components into the crystal growth region, and a generation of an SiC growth gas phase thereon, and as a result to cause the at least one bulk SiC single crystal having a central middle longitudinal axis to grow onto the at least one SiC seed crystal by deposition from the SiC growth gas phase; c) an insulation surrounding the growth crucible, said insulation extending rotationally symmetrically and axially in a direction of the central middle longitudinal axis and having at least two insulation cylinder components, and wherein: c1) the at least two insulation cylinder components are in a mutually concentric arrangement with one inside another, and each of the at least two insulation cylinder components has a wall thickness measured in a radial direction; c2) the insulation is notionally divided into multiple insulation ring segments arranged successively and axially in the direction of the central middle longitudinal axis; c3) each of the insulation ring segments is in turn notionally divided into multiple volume elements arranged alongside one another in a tangential direction; c4) each of the insulation ring segments has an average insulation ring segment density measured over the wall thicknesses of all of the at least two insulation cylinder components; c5) the at least two insulation cylinder components, each of which have variances in density in sub-regions, are selected and positioned relative to one another in such a way that every volume element of the insulation ring segment in question has a volume element density varying by no more than 10% from the average insulation ring segment density of the insulation ring segment in question; and c6) every volume element extends in axial direction over an axial element length that is equal to an axial segment length of the insulation ring segment and is up to 50 mm, in circumferential direction over an outer tangential element length of up to 50 mm, and in radial direction over a sum of all wall thicknesses of the at least two insulation cylinder components.
13. The growth arrangement according to claim 12, wherein the insulation comprises an insulation material having a material density between 0.05 g/cm.sup.3 and 0.5 g/cm.sup.3.
14. The growth arrangement according to claim 13, wherein the insulation comprises an insulation material having a material density between 0.1 g/cm.sup.3 and 0.2 g/cm.sup.3.
15. The growth arrangement according to claim 12, wherein the at least two insulation cylinder components are selected and positioned relative to one another such that every volume element of the insulation ring segment in question has a volume element density varying by no more than 5% from the average insulation ring segment density of the insulation ring segment in question.
16. The growth arrangement according to claim 12, wherein the axial element length of the volume elements is 20 mm and the outer tangential element length of the volume elements is 20 mm.
17. The growth arrangement according to claim 12, wherein the radial wall thickness of each of the at least two insulation cylinder components lies in a range between 5 mm and 50 mm.
18. The growth arrangement according to claim 17, wherein the radial wall thickness of each of the at least two insulation cylinder components lies in a range between 10 mm and 20 mm.
19. The growth arrangement according to claim 12, wherein a quotient of two of the radial wall thicknesses of the at least two insulation cylinder components lies in a range between 0.5 and 2.
20. The growth arrangement according to claim 12, wherein two mutually adjacent insulation cylinder components among the at least two insulation cylinder components each are radially separated by a distance in a range between 0.1 mm and 5 mm.
21. The growth arrangement according to claim 20, wherein each of the at least two insulation cylinder components has a radial separation in the range between 1 mm and 2 mm.
Description
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWING
(1)
(2)
(3)
(4)
DETAILED DESCRIPTION OF THE INVENTION
(5) Mutually corresponding parts are given the same reference numerals in
(6) Referring now to the figures of the drawing in detail and first, particularly, to
(7) In the region of a crucible end wall 7 of the growth crucible 3 opposite the SiC reservoir region 4, there is mounted an SiC seed crystal 8 that extends axially into the crystal growth region 5. The SiC seed crystal 8 is especially monocrystalline. The crucible end wall 7 may take the form of a crucible lid of the growth crucible 3. However, this is not obligatory. The bulk SiC single crystal 2 to be grown grows on the SiC seed crystal 8 by means of deposition from a SiC growth gas phase 9 that forms in the crystal growth region 5. The growing bulk SiC single crystal 2 and the SiC seed crystal 8 have roughly the same diameter. If any, a variance of not more than 20% by which a seed diameter of the SiC seed crystal 8 is smaller or greater than a single crystal diameter of the bulk SiC single crystal 2 arises. However, a gap (not shown in
(8) In the working example according to
(9) For heating of the growth crucible 3, an inductive heating device in the form of a heating coil 12 is arranged around the outside of the thermally insulated growth crucible 3. The growth crucible 3 is heated to the temperatures required for the growth by means of the heating coil 12. In the working example shown, these growth temperatures are at least 2100° C. The heating coil 12 inductively couples an electrical current into the electrically conductive crucible side wall 13 of the growth crucible 3. This electrical current flows essentially as a circular current in circumferential direction within the circularly cylindrical and hollow-cylindrical crucible side wall 13 and in so doing heats up the growth crucible 3. If required, the relative position between the heating coil 12 and the growth crucible 3 may be altered axially, i.e. in the direction of a middle longitudinal axis 14 of the growing bulk SiC single crystal 2, especially in order to adjust and optionally also to alter the temperature or temperature profile within the growth crucible 3. The position of the heating coil 12 which is variable axially during the growth process is indicated in
(10) 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 constituents in the form of Si, Si.sub.2C and SiC.sub.2 (=SiC gas species). The material transport of the SiC source material 6 to a growth interface 16 on the growing bulk SiC single crystal 2 firstly proceeds along an axial temperature gradient. At the growth interface 16 there is a relatively high growth temperature of at least 2100° C., especially even of at least 2200° C. or 2300° C. In addition, at the growth interface 16, in particular, an axial temperature gradient of at least 5 K/cm, preferably of at least 15 K/cm, is established in the direction of the middle longitudinal axis. The temperature within the growth crucible 3 decreases toward the growing bulk SiC single crystal 2. The highest temperature at about 2300° C. to 2500° C. is in the region of the SiC reservoir region 4. This temperature profile with a temperature differential of especially 100° C. to 150° C. between the SiC reservoir region 4 and the growth interface 16 can be achieved via various measures. For instance, by means of a division (not shown in detail) of the heating coil 12 into two or more axial subsections, it is possible to provide axial variation in heating. In addition, in the lower section of the growth crucible 3, for example by means of appropriate axial positioning of the heating coil 12, it is possible to establish a stronger heating effect than in the upper section of the growth crucible 3.
(11) The thermal insulation 10 has an upper axial insulation lid 11, disposed adjacent to the upper crucible end wall 7 and containing a central cooling opening 17 disposed at the middle longitudinal axis 14. Heat can be removed via the cooling opening 17 and/or the growth crucible 3 can be monitored. In addition, thermal insulation 10 has a lower axial insulation lid 18, disposed below the SiC reservoir region 4, and two insulation cylinder components 19 and 20, in a concentric arrangement relative to the middle longitudinal axis 14 and also concentric relative to one another. The latter surround the crucible side wall 13. The insulation cylinder component 20 has been inserted into the insulation cylinder component 19 (see also
(12) In the partly transparent perspective view of
(13) The mechanical construction of the insulation cylinder components 19, 20 is rotationally symmetric in each case in terms of its construction. Nevertheless, this is not true of all material properties, especially not for the distribution of the material density in tangential direction. There can be variances here, such that the density distribution within the walls of the insulation cylinder components 19, 20 is not absolutely rotationally symmetric overall.
(14) In order to be able to accomplish the described advantageous balancing of local variances in density in the thermal insulation 10, the distribution of the material density is first ascertained in the insulation cylinder components 19, 20 involved. As apparent from
(15) Using this information, it is possible to select the insulation cylinder components 19, 20 to be used to construct the thermal insulation 10 and position them relative to one another such that local density variances are balanced. The selection/testing criterion used as the basis is elucidated in detail with reference to the figure of
(16) For instance, the thermal insulation 10 with the two insulation cylinder components 19, 20 is notionally divided into multiple insulation ring segments in a successive axial arrangement in the direction of the central middle longitudinal axis 14. One of these, namely the insulation ring segment 29, is shown by way of example in the diagram of
(17) The volume element 31 (like every other volume element of the insulation ring segment 29) extends in axial direction over an axial element length H equal to an axial segment length of the insulation ring segment 29. In addition, the volume element 31 extends in tangential direction over an outer tangential element length L and in radial direction over the addition of the radial wall thicknesses of all insulation cylinder components involved, i.e. over the wall thicknesses D1 and D2 of the insulation cylinder components 19, 20 here. The axial element length H and also the outer tangential element length L are each in the range between 10 mm and 50 mm, especially each 50 mm or each 20 mm. The wall thicknesses D1 and D2 are in the range between 5 mm and 50 mm, especially between 10 mm and 20 mm. They may, but need not necessarily, be the same. This is also true when more than the two insulation cylinder components 19, 20 should be present.
(18) Taking account of the above selection/testing criterion, the two insulation cylinder components 19, 20 have been selected as suitable for the thermal insulation 10. The insulation cylinder components 19, 20 have then been assembled with suitable orientation with respect to one another, again taking account of the above selection/testing criterion. The thermal insulation 10 thus produced can then be subjected once again to an x-ray analysis according to
(19)
(20) Overall, the growth crucible 34 has a construction which is mirror-imaged or symmetric in the direction of the middle longitudinal axis 14 in a transverse plane (not included in
(21) A further difference from the growth arrangement 1 according to
(22) However, the insulation cylinder components 42, 43, 44 do not have perfect rotational symmetry in all material properties. Variances occur especially in the case of the density distribution. For instance, there are two variance sites 45 and 46. The first variance site 45 is at the height of the first crystal growth region 5. The local density ρ0 in the outer insulation cylinder component 42 and the local density ρ2 in the inner insulation cylinder component 44 vary there from the base density ρ1 that otherwise exists in the three insulation cylinder components 42, 43, 44. The second variance site 46 is at the height of the second SiC seed crystal 37. The local density ρ0 in the middle insulation cylinder component 43 and the local density ρ2 in the outer insulation cylinder component 42 vary there from the base density ρ1. Again, the following relationship is applicable in each case: ρ0<ρ1<ρ2. In the case of the growth arrangement 32 as well, the three insulation cylinder components 42, 43, 44 are specifically selected and positioned relative to one another using the above-elucidated selection/testing criterion in such a way that the local density variances at the variance sites 45 and 46 very substantially balance out. For instance, the thermal insulation 41 overall has a largely ideally rotationally symmetric density distribution viewed over the wall thicknesses D1, D2 and D3 of the three insulation cylinder components 42, 43, 44. In this respect, a rotationally symmetric temperature field is also established within the growth crucible 34, by means of which the two bulk SiC single crystals 2 and 33 grow in a rotationally symmetric and hence very homogeneous and defect-free manner.
(23) In principle, the use of the thermal insulation 41 with the three insulation cylinder components 42, 43, 44 is not limited to the growth arrangement 32 according to
(24) In this respect, the growth arrangements 1 and 32 enable the production of high-quality bulk SiC single crystals 2, 33 that can be processed further with high yield to give components.
(25) More particularly, it is possible to produce bulk SiC single crystals 2, 33, in each of which the maximum and minimum difference in length between crystal surface and the reverse side of the crystal at the crystal edge vary by not more than 10% from the measured average crystal length of the crystal edge. At the processing outline defined by the processing diameter, which is equal to the substrate diameter of the monocrystalline SiC substrates (=SiC wafers) obtained at a later stage from the bulk SiC single crystals 2, 33, the maximum and minimum difference in length between the crystal surface and the reverse side of the crystal of the bulk SiC single crystals vary by a maximum of 5% from the average crystal length measured at the processing outline. More particularly, the bulk SiC single crystals 2, 33 produced have essentially just a single SiC polytype, for example 4H—SiC, 6H—SiC, 3C—SiC or 15R—SiC. Preference is given to 4H—SiC. In addition, the crystal structure of the bulk SiC single crystals 2, 33 may have a slightly tilted orientation (=off orientation), where the tilt angle is in the range between 0° and 8°, preferably 4°. The bulk SiC single crystals 2, 33 have a crystal diameter of especially at least 100 mm, preferably of at least 150 mm. An upper limit in the crystal diameter is especially 250 mm. A preferred crystal diameter is 150 mm. In addition, the bulk SiC single crystals 2, 33 especially have a specific electrical resistivity in the range between 12.Math.10.sup.−3 Ωcm and 26.Math.10.sup.−3 Ωcm, preferably in the range between 16.Math.10.sup.−3 Ωcm and 24.Math.10.sup.−3 Ωcm.