CN114561694A - Device and method for preparing low-basal plane dislocation silicon carbide single crystal - Google Patents
Device and method for preparing low-basal plane dislocation silicon carbide single crystal Download PDFInfo
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- 239000013078 crystal Substances 0.000 title claims abstract description 107
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 47
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 19
- 230000012010 growth Effects 0.000 claims abstract description 27
- 238000001816 cooling Methods 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 4
- 230000035882 stress Effects 0.000 description 9
- 230000008646 thermal stress Effects 0.000 description 9
- 239000000758 substrate Substances 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 229910002804 graphite Inorganic materials 0.000 description 6
- 239000010439 graphite Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 238000000137 annealing Methods 0.000 description 4
- 238000005336 cracking Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 230000035755 proliferation Effects 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000003698 anagen phase Effects 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000010583 slow cooling Methods 0.000 description 1
- 235000012431 wafers Nutrition 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/002—Controlling or regulating
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/36—Carbides
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- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
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- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a device and a method for preparing low-basal plane dislocation silicon carbide single crystals, which comprises a crucible body and a crucible cover, and further comprises seed crystals and a split type constant diameter ring, wherein the thickness of the seed crystals is more than 3mm, the split type constant diameter ring is provided with steps for placing the seed crystals, a temperature field in the device is designed to have a radial temperature gradient of less than 0.3K/mm, and a cooling strategy is to rapidly reduce the temperature from the growth temperature to a higher temperature and then slowly reduce the temperature from the higher temperature to the lower temperature. The device of the invention has small change, is easy to realize and basically has no influence on the prior device; the invention can effectively reduce the density of basal plane dislocation in the silicon carbide crystal and prepare BPD with the density less than 500 pieces/cm‑2The silicon carbide single crystal of (1).
Description
Technical Field
The invention belongs to the field of crystal growth, and particularly relates to a device and a method for preparing low-basal plane dislocation silicon carbide single crystals.
Background
Silicon carbide (SiC) is considered to be the most promising substrate material for next-generation power devices because of its excellent characteristics of large forbidden bandwidth, high critical breakdown field strength, high thermal conductivity, and the like. In the past decades, although the global silicon carbide device market has been initially scaled, problems still exist in the field of silicon carbide power devices to be broken through urgently compared with advanced silicon power semiconductor devices, and most prominently, the problems that the price of a silicon carbide single crystal substrate is high and the material defects are still not completely solved. Several decades of technological development have shown that micropipe defects in silicon carbide have been substantially eliminated (micro-scale densities of 0 or less than 0.01 cm-2). Currently, zero micropipe wafers are already available from most suppliers. However, the formation of dislocations during the growth of silicon carbide crystals remains a significant obstacle to achieving high performance silicon carbide power devices. Among the dislocation defects commonly found in silicon carbide are threading dislocation (TSD), Threading Edge Dislocation (TED), and Basal Plane Dislocation (BPD).
The presence of thermal stresses during crystal growth is a major cause of BPD formation, which can be easily introduced into the growing ingot when shear stresses exceed a critical value, causing bending of the base sagittal plane.
The following are several causes of stress:
1) the most significant source is thermal stress introduced by inadequate temperature distribution during Physical Vapor Transport (PVT) growth, and temperature gradients in both the radial and axial directions can induce differential thermal expansion in the ingot.
2) The difference in thermal expansion coefficients of SiC and crucible material can produce severe thermal stress, for example, a 3C-SiC crystal with a thermal expansion coefficient of 5.5x10 at 2100K-6K, while the thermal expansion coefficient of the conventional graphite crucible material is 3.8x10-6and/K. The coefficients of thermal expansion of the two are close to a 30% mismatch, so that during the crystal growth phase, the crucible must compress the crystal, thereby introducing stresses in the crystal.
3) At present, the PVT method is used for growing silicon carbide, and the method for introducing the seed crystal generally adopts the bonding technology, namely the seed crystal is fixed on a graphite cover by using an adhesive. The crystal is thus in a constrained state, and stresses are introduced by the crystal expanding to break free at high temperatures.
Chinese patent CN 109234810A provides a silicon carbide single crystal growth device without adhering seed crystal, but the seed crystal adopted by the device is still a commercial substrate sheet with the thickness of 300-500 μm, and under the actual growth temperature, the temperature gradient between the back of the seed crystal and the growth atmosphere is too large and the seed crystal is easy to sublimate and decompose under the protection of no back graphite cover.
4) Stress is introduced into the crystal in the cooling process, thermal stress in the crystal is reduced by slow annealing, and the thermal stress in the crystal is reduced by annealing along with a furnace or secondary annealing after the crystal is taken out in the U.S. Pat. No. 4, 20160083865A1 and Chinese patent CN 200910243520.4. However, both theoretical calculations (Crystal Growth Design 2014,14, 1272-. While thermal stress relief during the annealing stage is achieved at the expense of BPD propagation, the presence of stress increases the system energy from an energy perspective, and dislocations in the crystal propagate to relieve the stress in order to lower the system energy. In the above description, thermal stress relief is achieved by other means. Therefore, it is surprising that rapid cool down is beneficial to reduce BPD. However, excessive thermal stress in the crystal can cause crystal cracking and seriously affect the yield of the crystal.
Disclosure of Invention
The invention aims to reduce the density of basal plane dislocation in a silicon carbide crystal, and provides a device and a method for preparing a low basal plane dislocation silicon carbide single crystal, wherein the low basal plane dislocation silicon carbide single crystal has a BPD density of less than 500 pieces/cm-2The silicon carbide single crystal of (1). The requirement of the current commercial silicon carbide single crystal substrate inspection standard on the dislocation density of the basal plane is less than 2000 pieces/cm-2。
In order to achieve the purpose, the invention adopts the following technical scheme:
the device for preparing the low-basal plane dislocation silicon carbide single crystal comprises a crucible body, a crucible cover, a seed crystal and a split type isometric ring, wherein the thickness of the seed crystal is larger than 3mm, the split type isometric ring is provided with a step, and the step is used for placing the seed crystal.
As a preferable scheme of the invention, the thickness of the seed crystal is less than 10 mm.
As a preferable scheme of the invention, a gap is formed between the two lobes of the split type equal-diameter ring, and the size of the gap is 0.1-1 mm.
In a preferred embodiment of the invention, the temperature field in the device is designed such that the radial temperature gradient is less than 0.3K/mm.
In the invention, aiming at the thermal stress introduced by improper temperature distribution in Physical Vapor Transport (PVT) growth, the radial and axial temperature gradients can induce the uneven thermal expansion in the crystal ingot, and the invention designs a temperature field with proper gradient, and the radial temperature gradient of the temperature field is required to be designed to be less than 0.3K/mm.
Aiming at the stress generated by the SiC and the crucible due to the thermal expansion coefficient, the invention adopts the split type equal-diameter ring, the equal-diameter ring is divided into two parts, a certain gap is reserved between the two petals of equal-diameter rings, and a certain gap is reserved for the thermal expansion of the crystal, so that the extrusion of the crucible to the crystal is avoided, and simultaneously, gas phase components can escape from the gap to inhibit the growth of polycrystal at the periphery of the crystal.
Aiming at the problems that the existing PVT method for growing silicon carbide and introducing seed crystals generally adopts a bonding technology, the method adopts a mode of not bonding the seed crystals, namely the seed crystals are placed on steps reserved in a split type constant diameter ring, so that the situation that the crystals are in a bound state due to adhesives and the stress is introduced due to the fact that the crystals expand and break away at high temperature is avoided, and meanwhile, the method has certain requirements on the thickness of the seed crystals, namely the thickness of the seed crystals is larger than 3mm and smaller than 10 mm.
The invention also provides a method for preparing the low-basal plane dislocation silicon carbide single crystal by adopting the device.
As a preferable scheme of the invention, the method comprises the following steps:
1) placing the powder inside a crucible body, placing a split type constant-diameter ring on a crucible, placing seed crystals on steps of the split type constant-diameter ring, and covering a crucible cover;
2) vacuumizing according to a program, heating, and growing crystals;
3) after the growth is finished, the temperature is reduced from the growth temperature to a first preset temperature within a first preset time;
4) in a second preset time, reducing the temperature from the first preset temperature to a second preset temperature;
5) and turning off the power supply, cooling the furnace to room temperature, and taking out the crystal.
As a preferable scheme of the present invention, in the step 3), the first preset time is 1 to 3 hours, and the first preset temperature is 1750K to 1900K.
In a preferred embodiment of the present invention, the first preset time is 2 hours, and the first preset temperature is 1800K.
As a preferable scheme of the present invention, in the step 4), the second preset time is 10 to 12 hours, and the second preset temperature is 500K to 1000K.
As a preferable embodiment of the present invention, the second preset time is 10 hours, and the second preset temperature is 1000K.
According to the invention, the mobility of BPD is high at high temperature, the temperature needs to be quickly reduced to inhibit the proliferation of BPD, and the figure five shows that the radial temperature gradient change of the quick cooling (1h) is smaller than that of the slow cooling (10h) before 1750K, but becomes larger after 1750K, and the continuous quick cooling only increases the risk of crystal cracking and cannot achieve the effect of inhibiting the proliferation of BPD. Therefore, the temperature reduction strategy designed by the invention is to rapidly reduce the temperature from the growth temperature to a higher temperature and then slowly reduce the temperature from the higher temperature to a lower temperature, so that the design balances the requirements of inhibiting BPD proliferation and preventing crystal cracking.
Compared with the prior art, the invention has the following beneficial effects:
1) the device of the invention has small change, is easy to realize and basically has no influence on the prior device;
2) the invention can effectively reduce the density of basal plane dislocation in the silicon carbide crystal, and the density of the prepared BPD is less than 500/cm-2The silicon carbide single crystal of (1).
Drawings
FIG. 1 is a schematic of the present invention.
FIG. 2 is a schematic diagram of the temperature field design of the present invention.
FIG. 3 is a radial temperature profile from the center of the seed crystal to the edge of the seed crystal.
Fig. 4 is a side view of the split isometric ring of the present invention.
FIG. 5 is a radial temperature gradient profile for different cooling times.
FIG. 6 is a schematic diagram of the cooling of the present invention.
FIG. 7 is a distribution of the dislocation density in the silicon carbide single crystal substrate of example 1.
Fig. 8 is a dislocation density distribution in the silicon carbide single crystal substrate of comparative example 1.
In the figure, 1. crucible cover; 2. seed crystal; 3. a split type equal-diameter ring; 4. a crucible body; 5. and (4) a step.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, 2, 3 and 4, the invention firstly provides a device for preparing low basal plane dislocation silicon carbide single crystal, which comprises a crucible body 4 and a crucible cover 1, and also comprises a seed crystal 2 and a split type equal-diameter ring 3, wherein the thickness of the seed crystal 2 is more than 3mm and less than 10 mm; the split type equal-diameter ring 3 is provided with a step 5, the step 5 is used for placing the seed crystal 2, a gap is arranged between two petals of the split type equal-diameter ring, and the size of the gap is 0.1-1 mm.
The temperature field in the device is designed such that the radial temperature gradient is less than 0.3K/mm.
Example 1
An example is given by taking the growth of a 4H-SiC crystal as an example.
The temperature field design shown in fig. 2 is used. The crucible material selects a graphite crucible, the gap of the split type equal-diameter ring 3 is selected to be 0.8mm, the thickness of the selected 4H-SiC seed crystal 2 is 3mm, and the C surface is finely polished. As shown in figure 1, SiC powder is contained in a crucible body 4, a split type constant diameter ring 3 is placed on a step 5 reserved on the inner wall of the crucible, a thick seed crystal 2 is placed on the step 5 reserved on the split type constant diameter ring 3, and finally a graphite cover 1 is covered.
Will be charged with cruciblePlacing the crucible into a single crystal growth furnace, and vacuumizing to 1.0x10-3Below Pa, filling argon to 70kPa and heating; carrying out crystal growth under the growth conditions of 1kPa and 2100 ℃; after 100 hours of growth, cooling to 1800K for 2 hours, cooling to 1000K (see figure 6) for 10 hours, finally turning off the power supply to cool the crystal to room temperature along with the furnace, opening the growth furnace and taking out the crystal. The measured BPD distribution after slicing the obtained crystal is shown in FIG. 7, and is less than 500 pieces/cm-2。
Comparative example 1
The same as example 1, the temperature field design as shown in fig. 2 was used, except that the constant diameter ring was a closed structure of an annular body, a commercial substrate piece of 300 μm was used as the seed crystal, and the temperature reduction procedure was unchanged. The SiC powder is placed in the crucible, the integrated isometric ring is placed on a step reserved on the inner wall of the crucible, and the graphite cover adhered with seed crystals is placed on the step reserved on the integrated isometric ring. And putting the crucible filled with the materials into a single crystal growth furnace. Vacuum was pulled to 1.0x10-3Pa or less, and then, charging argon gas to 70kPa and raising the temperature. The crystal growth was carried out under growth conditions of 1kPa, 2100 ℃. After 100 hours of growth, cooling to 1800K for 2 hours, cooling to 1000K for 10 hours, finally turning off the power supply to cool the crystal to room temperature along with the furnace, and opening the growth furnace to take out the crystal. The measured BPD distribution after slicing the resulting crystal is shown in FIG. 8.
Therefore, the BPD density of the silicon carbide single crystal obtained by the device and the method is less than 500 pieces/cm-2The method can effectively reduce the density of the dislocation of the basal plane in the silicon carbide crystal.
While the invention has been described with respect to a preferred embodiment, it will be understood by those skilled in the art that the foregoing and other changes, omissions and deviations in the form and detail thereof may be made without departing from the scope of this invention. Those skilled in the art can make various changes, modifications and equivalent arrangements, which are equivalent to the embodiments of the present invention, without departing from the spirit and scope of the present invention, and which may be made by utilizing the techniques disclosed above; meanwhile, any changes, modifications and variations of the above-described embodiments, which are equivalent to those of the technical spirit of the present invention, are within the scope of the technical solution of the present invention.
Claims (10)
1. The device for preparing the low-basal plane dislocation silicon carbide single crystal comprises a crucible body and a crucible cover, and is characterized by further comprising a seed crystal and a split type isodiametric ring, wherein the thickness of the seed crystal is larger than 3mm, the split type isodiametric ring is provided with a step, and the step is used for placing the seed crystal.
2. An apparatus for producing a low basal plane dislocation silicon carbide single crystal as claimed in claim 1, wherein the seed crystal has a thickness of less than 10 mm.
3. An apparatus for producing a low basal plane dislocation silicon carbide single crystal as claimed in claim 2, wherein the two lobes of the split type constant diameter ring have a gap therebetween, the gap being in the range of 0.1 to 1 mm.
4. An apparatus for producing a low basal plane dislocation silicon carbide single crystal as claimed in claim 3, wherein the temperature field in the apparatus is designed so that the radial temperature gradient is less than 0.3K/mm.
5. A method for producing a low basal plane dislocation silicon carbide single crystal, characterized by using the apparatus of any one of claims 1 to 4.
6. A method of producing a low basal plane dislocation silicon carbide single crystal as claimed in claim 5, comprising the steps of:
1) placing the powder inside a crucible body, placing a split type constant-diameter ring on a crucible, placing seed crystals on steps of the split type constant-diameter ring, and covering a crucible cover;
2) vacuumizing according to a program, heating, and growing crystals;
3) after the growth is finished, the temperature is reduced from the growth temperature to a first preset temperature within a first preset time;
4) in a second preset time, reducing the temperature from the first preset temperature to a second preset temperature;
5) and turning off the power supply, cooling the furnace to room temperature, and taking out the crystal.
7. The method for producing a low basal plane dislocation silicon carbide single crystal according to claim 6, wherein in the step 3), the first preset time is 1-3h, and the first preset temperature is 1750K-1900K.
8. The method for producing a low basal plane dislocation silicon carbide single crystal as claimed in claim 7, wherein the first predetermined time is 2 hours and the first predetermined temperature is 1800K.
9. The method for producing a low basal plane dislocation silicon carbide single crystal according to claim 6, wherein in step 4), the second predetermined time is 10 to 12 hours and the second predetermined temperature is 500K to 1000K.
10. A method of producing a low basal plane dislocation silicon carbide single crystal as claimed in claim 5, wherein the second predetermined time is 10 hours and the second predetermined temperature is 1000K.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115537927A (en) * | 2022-12-01 | 2022-12-30 | 浙江晶越半导体有限公司 | Silicon carbide single crystal ingot growth system and method for preparing low-basal plane dislocation |
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2022
- 2022-02-25 CN CN202210182802.3A patent/CN114561694A/en active Pending
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Cited By (2)
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| CN115537927A (en) * | 2022-12-01 | 2022-12-30 | 浙江晶越半导体有限公司 | Silicon carbide single crystal ingot growth system and method for preparing low-basal plane dislocation |
| CN115537927B (en) * | 2022-12-01 | 2023-03-10 | 浙江晶越半导体有限公司 | Silicon carbide single crystal ingot growth system and method for preparing low-basal plane dislocation |
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