CN115142123B - Method for improving surface type parameters of silicon carbide single crystal substrate by doping germanium - Google Patents
Method for improving surface type parameters of silicon carbide single crystal substrate by doping germanium Download PDFInfo
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- CN115142123B CN115142123B CN202210551272.5A CN202210551272A CN115142123B CN 115142123 B CN115142123 B CN 115142123B CN 202210551272 A CN202210551272 A CN 202210551272A CN 115142123 B CN115142123 B CN 115142123B
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- 239000013078 crystal Substances 0.000 title claims abstract description 57
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 36
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 29
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 229910052732 germanium Inorganic materials 0.000 title claims abstract description 25
- 239000000758 substrate Substances 0.000 title claims abstract description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 28
- 229910002804 graphite Inorganic materials 0.000 claims description 28
- 239000010439 graphite Substances 0.000 claims description 28
- 230000006698 induction Effects 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 4
- 230000000087 stabilizing effect Effects 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 3
- 230000008569 process Effects 0.000 abstract description 12
- 239000012535 impurity Substances 0.000 abstract description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 4
- 238000012545 processing Methods 0.000 abstract description 4
- 229910000078 germane Inorganic materials 0.000 abstract description 2
- 239000011162 core material Substances 0.000 description 10
- 239000007789 gas Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 6
- 230000035882 stress Effects 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000012360 testing method Methods 0.000 description 3
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- 238000002441 X-ray diffraction Methods 0.000 description 2
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- 239000002019 doping agent Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
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- 239000012159 carrier gas Substances 0.000 description 1
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- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000035755 proliferation Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
- C30B23/002—Controlling or regulating
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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
- 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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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- Crystallography & Structural Chemistry (AREA)
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Abstract
The invention discloses a kind of adulterated materialA method for improving the surface type parameter of silicon carbide single crystal substrate by germanium is characterized in that non-electroactive germanium impurities are doped in the process of growing the silicon carbide single crystal by a physical vapor transport method (PVT), the germanium impurities can pin incomplete dislocation of a silicon core, the slip of the incomplete dislocation of the silicon core is prevented by the dislocation pinning effect, and the slip of the single crystal substrate under the mechanical stress in the processing process is restrained, so that the purpose of improving the surface type parameter of the silicon carbide single crystal substrate is realized. Meanwhile, in order to control the high vapor pressure of germanium in the early growth stage, prevent the cluster effect of germanium atoms on the growth surface, ensure the continuous supply of germanium source in the growth process and realize the uniform doping in the crystal growth process, the invention uses germane (GeH) 4 ) The gas is used as a doping source of germanium, and GeH is stably and uniformly introduced into a growth cavity while PVT single crystal grows 4 Gas to achieve the above object.
Description
Technical Field
The invention belongs to the technical field of crystal materials, relates to growth of silicon carbide single crystals, and particularly relates to a method for improving substrate surface type parameters of silicon carbide single crystals by doping germanium.
Background
The semiconductor silicon carbide material has the excellent characteristics of large forbidden bandwidth, high thermal conductivity, high breakdown field intensity, high saturated electron drift rate, good chemical stability and thermal stability and the like, has important application value in the fields of power electronics, radio frequency microwaves, quantum sensing and the like, and is a basic core material for national economic development of new energy technology, smart power grids, information communication, rail transit, national defense and military industry and the like. At present, the method for growing the 4H-SiC single crystal is mainly a physical gas phase transport method, and although the 4H-SiC single crystal obtained by the method is widely applied commercially, the total dislocation density in the 4H-SiC single crystal is still as high as 10 3 -10 4 cm -2 Becomes a key bottleneck problem limiting the application of 4H-SiC materials.
The dislocation types in silicon carbide single crystals are largely classified into threading dislocation (Threading dislocation-TD) and basal plane dislocation (Base plane dislocation-BPD). BPD is generated and slips under thermal stress. Complete BPD Bosch vectorBut it is very easy to pass through the reaction
Into two incomplete dislocations separated by a Stacking Fault (SF). Wherein the slip barrier of Si core incomplete dislocation is much lower than C core incomplete dislocation. Therefore, the slip of the BPD is mainly performed by the slip of the Si core incomplete dislocation.
In addition, mechanical stress during processing of silicon carbide single crystal substrates can cause nucleation and slippage of the BPD, affecting the surface profile parameters (e.g., warpage, curvature, etc.) of the substrate. The slip of the Si core incomplete dislocation under thermal stress and mechanical stress, which is due to the BPD, causes the BPD to be non-uniform in the 4H-SiC single crystal substrate, thereby causing deterioration of the plane type parameters of the substrate.
Disclosure of Invention
In order to reduce the proliferation and slip of the BPD in the 4H-SiC single crystal substrate under the thermal stress and the mechanical stress and optimize the mechanical property and the surface type parameter of the silicon carbide crystal, the invention provides a method for improving the surface type parameter of the silicon carbide single crystal substrate by doping germanium, wherein non-electroactive germanium impurities are doped in the PVT growth process, the germanium impurities can pin incomplete dislocation of a silicon core, and the slip of the incomplete dislocation of the silicon core is prevented by the dislocation pinning effect, so that the series of purposes are realized. Meanwhile, in order to control the high vapor pressure of germanium in the early growth stage, prevent germanium atoms from clustering on the growth surface and realize uniform doping in the crystal growth process, germane (GeH) 4 ) The gas doping source is used for stably and uniformly introducing GeH into the growth cavity while PVT single crystal grows 4 Gas to achieve the above object.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a method for improving the surface type parameter of silicon carbide monocrystal substrate by doping germanium includes such steps as introducing gaseous germanium source to form stable, uniform and controllable doping atmosphere, and obtaining the uniformly doped germanium-doped silicon carbide monocrystal substrate.
In the invention, the growth device adopts induction heating, combines the advantages of PVT and HTCVD growth, introduces a gaseous growth source and a doping source on the basis of the PVT growth device, and stably introduces GeH while PVT growth 4 And (3) forming a stable, uniform and controllable doping atmosphere, and finally obtaining the uniformly doped germanium-doped silicon carbide single crystal material. It is known that during processing of a silicon carbide single crystal substrate, deterioration of the plane-type parameters is caused by nucleation and slip of the BPD under mechanical stress, and that slip of the BPD is achieved by slip in which Si core is not fully dislocation. In single crystal growth of 4H-SiC, doped Ge can preferentially replace Si atoms at the incomplete dislocation core, and Ge is a non-electroactive impurity and has the effect of pinning the incomplete dislocation of the Si core, and because the incomplete dislocation of the Si core is pinned by the Ge impurity, the slip of the incomplete dislocation of the Si core is restrained under the action of mechanical stress introduced in the processing process of the silicon carbide single crystal substrate. Thus, the Ge doping method helps to enhance the mechanical properties of the 4H-SiC single crystal substrate and improve the surface profile parameters of the silicon carbide single crystal substrate.
As a preferable scheme of the invention, the growth device adopted by the method comprises a graphite crucible, a heat preservation layer, a heater, a graphite support, seed crystals, an induction coil and a temperature measuring hole, wherein the heat preservation layer is positioned below the graphite crucible, and the heater is positioned below the heat preservation layer.
As a preferred embodiment of the present invention, the apparatus further comprises a doping source channel, wherein the doping source channel passes through the heater and is communicated with the insulating layer and the graphite crucible.
As a preferred embodiment of the present invention, the dopant source passageway coincides with the center line of the graphite crucible.
As a preferred embodiment of the present invention, the method specifically comprises:
1) The bottom of the graphite crucible is positioned at the center of the induction coil;
2) Placing a silicon carbide powder source into a graphite crucible, fixing seed crystals on a graphite support, and placing the seed crystals on the top of the graphite crucible;
3) Sealing the growth device, vacuumizing, heating to raise the temperature, and preserving heat;
4) Filling a protective gas through a doping source channel to stabilize the pressure at 400mbar;
5) Heating coil power is improved, and pressure stability is kept;
6) Introducing protective gas doped with germanium source, distributing to reduce pressure to growth state after stabilizing, and starting growth;
7) After the growth is finished, gradually increasing the pressure, reducing the power of a heating coil, and cooling the temperature in the graphite crucible to the room temperature to obtain the germanium-doped silicon carbide single crystal.
As a preferred embodiment of the present invention, in step 3), the vacuum is applied to 1X 10 -5 After Pa, the temperature is increased to 1100-1300 ℃, and the heat preservation time is 5h.
As a preferred embodiment of the invention, in step 5), the temperature is increased to 2000-2200 ℃.
As a preferred embodiment of the invention, in step 6), the germanium source is present in the shielding gas in a volume fraction of 0.5-5%, the distribution reducing pressure is such that the pressure is reduced to 100mbar within 1 hour, the pressure is reduced to 10mbar within 1 hour, and the pressure is reduced to 3mbar within 1 hour.
As a preferred embodiment of the invention, the gaseous germanium source is GeH 4 。
As a preferred embodiment of the invention, in step 7), the pressure is increased stepwise to 800mbar over 1 hour.
Compared with the prior art, the invention has the following beneficial effects:
1) According to the invention, under the condition that no electroactive impurities are introduced, the slippage of the BPD can be slowed down by doping, so that the surface type parameters of the 4H-SiC single crystal substrate are optimized;
2) The invention can relieve the lattice distortion of n-type 4H-SiC;
3) Gas GeH 4 The doping of the source controls the high vapor pressure of Ge in the initial growth stage, prevents the Ge atoms from clustering on the growth surface and realizes uniform and controllable doping in the crystal growth process;
4) The method of the invention has simple operation and no pollution in the preparation process.
Drawings
FIG. 1 is a graph showing the results of a face type parameter test in accordance with an embodiment of the present invention.
FIG. 2 is a graph showing the results of the facial parameters test of the comparative example of the present invention.
FIG. 3 is a schematic view of a growth apparatus of the present invention.
FIG. 4 is a view showing a 4H-SiC single crystal obtained in the example of the present invention.
FIG. 5 is an XRD pattern of a 4H-SiC single crystal prepared in accordance with an embodiment of the present invention.
FIG. 6 is an XRD pattern of a 4H-SiC single crystal obtained in the comparative example.
In fig. 3, 1. Insulation layer; 2. a heater; 3. a graphite crucible; 4. seed crystal; 5. a dopant source channel; 6. an induction coil; 7. and a temperature measuring hole.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Referring to fig. 3, the invention provides a method for improving the substrate profile parameters of silicon carbide single crystal by doping germanium, the adopted growth device comprises a graphite crucible 3, an insulating layer 1, a heater 2, a graphite support, a seed crystal 4, a doping source channel 5, an induction coil 6 and a temperature measuring hole 7, wherein the insulating layer 1 is positioned below the graphite crucible 3, the heater 2 is positioned below the insulating layer 1, the doping source channel 5 is communicated with the graphite crucible 3 through the heater 2, and the central line of the doping source channel 5 and the graphite crucible 3 are coincident.
The heater 2 is a graphite heater, and the temperature measuring hole 7 is positioned at the top of the graphite crucible 3.
Examples
The embodiment provides a method for improving single crystal plane type parameters of silicon carbide by doping germanium, which adopts the growth device and comprises the following steps:
step 1: adjusting the relative position of the graphite crucible and the induction coil to enable the bottom of the graphite crucible to be positioned at the center of the induction coil, so that the top of the graphite crucible obtains a flat temperature field;
step 2: placing a silicon carbide powder source into a graphite crucible, and fixing 4-inch 4H-SiC seed crystals on the top of the graphite crucible;
step 3: covering the crucible cover, sealing the PVT growth furnace, and vacuumizing the growth device to 1×10 -5 Pa, switching on a power supply of a heater, and increasing the temperature to 1100-1300 ℃ by adopting an induction heating mode; stabilizing for 5 hours, and removing harmful impurities such as water, oxygen and the like;
step 4: ar is filled into the doping source channel, so that the pressure in the cavity is stabilized at 400mbar;
step 5, heating coil power is increased, the temperature is increased to 2000-2200 ℃, and the temperature is tested by a thermometer through a top temperature measuring hole; during the temperature rising process, the pressure of the chamber is kept to be 400mbar so as to prevent the overflow of the Si source during the temperature rising process;
step 6, adding 0.5-5% GeH into Ar carrier gas 4 Gradually reducing the pressure to 100mbar within 1 hour after stabilizing for 1 hour, gradually reducing the pressure to 10mbar within 1 hour, and finally reducing the pressure to 3mbar within 1 hour, so as to keep stable growth for 50 hours;
and 7, after the growth time is over, the pressure is increased to 800mbar by using the time length of 1 hour, then the power is gradually reduced to 0 by using the time length of 5 hours, finally, ten hours are waited, and the silicon carbide single crystal can be taken out after the temperature in the crucible is reduced to the room temperature.
The only difference between the comparative example and the examples is that: undoped Ge.
As shown in FIG. 4, the 4H-SiC monocrystal obtained in the embodiment is not filled with nitrogen in the current growth process, and the heat insulation material in the PVT growth furnace can adsorb a large amount of nitrogen, so that the obtained 4H-SiC monocrystal belongs to lightly doped n type.
To verify whether the 4H-SiC single crystal obtained by the method of the present invention reduced lattice distortion caused by N doping, 4H-SiC single crystals obtained without doping Ge under the same conditions were compared.
The 4H-SiC single crystals obtained in examples and comparative examples were sliced, and the third piece was taken as well, and after CMP, the half width was measured by X-rays, as shown in FIG. 5 and FIG. 6, FIG. 5 shows the results obtained in examples of the present invention, and FIG. 6 shows the results obtained in comparative examples without Ge doping under the same conditions. Clearly, the half-width (24.7 arc seconds) of the wafer obtained by the method of the present invention is much smaller than the result (43.7) of undoped Ge, indicating that the method of the present invention is effective in reducing lattice distortion caused by N doping.
In addition, the surface type parameter test is carried out on the 4H-SiC single crystals obtained in the examples and the comparative examples, and the results are shown in fig. 1 and 2, and the values of each surface type parameter of the 4H-SiC single crystal obtained by the method are superior to those of the 4H-SiC single crystal without doped Ge, so that the surface type parameter of the crystal is effectively optimized by doped Ge.
Therefore, under the condition of no introduction of electroactive impurities, the invention can slow down the slippage of BPD by doping, thereby optimizing the surface type parameter of 4H-SiC monocrystal, and can slow down the lattice distortion of n-type 4H-SiC, and the gas GeH 4 The doping of the source controls the high vapor pressure of Ge in the initial growth stage, prevents the Ge atoms from clustering on the growth surface and realizes the uniform and controllable doping in the crystal growth process.
While the invention has been described with respect to preferred embodiments thereof, it will be understood by those skilled in the art that various modifications and additions may be made without departing from the scope of the invention. Equivalent embodiments of the present invention will be apparent to those skilled in the art having the benefit of the teachings disclosed herein, when considered in the light of the foregoing disclosure, and without departing from the spirit and scope of the invention; meanwhile, any equivalent changes, modifications and evolution of the above embodiments according to the essential technology of the present invention still fall within the scope of the technical solution of the present invention.
Claims (2)
1. The method for improving the surface type parameters of the silicon carbide single crystal substrate by doping germanium is characterized by comprising the steps of introducing a gaseous germanium source on the basis of a PVT method to form a stable, uniform and controllable doping atmosphere, and finally obtaining the uniformly doped germanium-doped silicon carbide single crystal material; the gaseous germanium source is GeH 4；
The method specifically comprises the following steps:
1) The bottom of the graphite crucible is positioned at the center of the induction coil;
2) Placing a silicon carbide powder source into a graphite crucible, fixing seed crystals on a graphite support, and placing the seed crystals on the top of the graphite crucible;
3) Sealing the growth device, and vacuumizing to 1×10 -5 After Pa, the temperature is increased to 1100-1300 ℃, and the heat preservation time is 5 hours;
4) Filling a protective gas through a doping source channel to stabilize the pressure at 400mbar;
5) Heating coil power is improved, and pressure stability is kept;
6) Introducing protective gas doped with germanium source, distributing to reduce pressure to growth state after stabilizing, and starting growth; wherein the volume fraction of the germanium source in the shielding gas is 0.5-5%, the distribution reducing pressure is that the pressure is firstly reduced to 100mbar within 1 hour, then the pressure is reduced to 10mbar within 1 hour, and finally the pressure is reduced to 3mbar within 1 hour;
7) After the growth is finished, the pressure is gradually increased to 800mbar within 1 hour, the power of a heating coil is reduced, and the temperature in the graphite crucible is reduced to room temperature, so that the germanium-doped silicon carbide single crystal is obtained.
2. A method for improving a substrate profile parameter of a silicon carbide single crystal as recited in claim 1, wherein in step 5), the temperature is increased to 2000-2200 ℃.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102005049932A1 (en) * | 2005-10-19 | 2007-04-26 | Sicrystal Ag | Growth of silicon carbide-germanium-volume mixed crystals, comprises producing silicon-, carbon- and germanium gas phase from two source materials containing silicon, carbon and germanium by sublimation and evaporation |
| CN102465336A (en) * | 2010-11-05 | 2012-05-23 | 上海华虹Nec电子有限公司 | Method for germanium-silicon epitaxy of high germanium concentration |
| CN105568385A (en) * | 2016-01-22 | 2016-05-11 | 山东大学 | Growth method of germanium-doped SiC body single-crystal material |
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| US20220049373A1 (en) * | 2020-08-11 | 2022-02-17 | II-VI Delaware, Inc | Sic single crystal(s) doped from gas phase |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102005049932A1 (en) * | 2005-10-19 | 2007-04-26 | Sicrystal Ag | Growth of silicon carbide-germanium-volume mixed crystals, comprises producing silicon-, carbon- and germanium gas phase from two source materials containing silicon, carbon and germanium by sublimation and evaporation |
| CN102465336A (en) * | 2010-11-05 | 2012-05-23 | 上海华虹Nec电子有限公司 | Method for germanium-silicon epitaxy of high germanium concentration |
| CN105568385A (en) * | 2016-01-22 | 2016-05-11 | 山东大学 | Growth method of germanium-doped SiC body single-crystal material |
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