CN100400723C - Heat treatment method after silicon carbide monocrystal growth - Google Patents
Heat treatment method after silicon carbide monocrystal growth Download PDFInfo
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- CN100400723C CN100400723C CNB2006100812940A CN200610081294A CN100400723C CN 100400723 C CN100400723 C CN 100400723C CN B2006100812940 A CNB2006100812940 A CN B2006100812940A CN 200610081294 A CN200610081294 A CN 200610081294A CN 100400723 C CN100400723 C CN 100400723C
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Abstract
The present invention discloses a heat treatment method after the growth of a silicon carbide single crystal, which comprises the following steps that SiC single crystals coated with carbon films and powder materials are arranged in a copple; the temperature of the SiC single crystals and the powder materials raise to the predetermined heat treating temperature under the protection of argon in a heating furnace, and the temperature is preserved for certain time; the SiC single crystals and the powder materials are cooled with the furnace, and the partial defects of microtubules and wrapped objects can be eliminated by the recrystallization and the solid state diffusion of the SiC crystals in the process of heat treatment. The method of the present invention has the function that the defect number of the microtubules and the wrapped objects in the SiC single crystals is reduced, so that the quality of the SiC single crystals is improved. In addition, the present invention has the advantages of simple process, low cost and easy realization, and has important application values for the defect reduction of the SiC single crystals and the quality improvement of the SiC single crystals.
Description
Technical field
The invention relates to the method that a kind of monocrystalline is handled, particularly relate to the heat treating method after a kind of silicon carbide (SiC) single crystal growing.
Background technology
SiC is an IV-IV family Binary compound semiconductor material, and it has broad-band gap (2.4-3.3eV), high critical breaking down field strength (＞2.0 * 10
5Vcm
-1), high heat conductance (5-7Wcm
-1K
-1), high carrier saturation drift velocity (2.0 * 10
7Cms
-1) etc. characteristic.Compare with s-generation semiconductor material GaAs with first-generation semiconductor material Si, third generation semiconductor material SiC has very big advantage at aspects such as working temperature, radioprotective, anti-high-breakdown-voltages, and its excellent performance can satisfy modern electronic technology to high temperature, high frequency, superpower, high pressure and radiation-resistant requirements at the higher level.Be widely used in Aeronautics and Astronautics detection, nuclear energy exploitation, satellite, oil and geothermal drilling exploration, motor car engine, radar, communicate by letter and military and civilian field (reference: Casady J B such as broadcast television, et al.Solid-State Electronics 39 (1996) 1409, this paper are in conjunction with reference).
At present, large size, the most sophisticated growth method of high quality SiC crystal are " physical vapor transmission method (physical vapor transport method) ", i.e. " PVT method " or " Modified-Lely method " (reference: Garcon I, et al.Mater.Sci.Eng.B29 (1999) 90, this paper are in conjunction with reference).The PVT method is to be proposed by Tairov and Tsvetkov in 1978, its cardinal principle is heated to the SiC powder 2200 ℃-2400 ℃ exactly, make its sublime up into crystallize on the cold junction seed crystal bulk crystals (reference: Tairov Yu M and Tsvetkov V F, J.Cryst.Growth 43 (1978) 209; Tairov Yu M and Tsvetkov V F, J.Cryst.Growth 52 (1978) 146, this paper are in conjunction with reference).Because the processing parameter that the SiC monocrystalline of PVT method growth need be controlled is more, and these parameters constantly change in crystal growing process, so be difficult to control defective in the SiC monocrystalline formation (reference: Li H Q, et al.J.Cyst.Growth 258 (2003) 100; WellmannP J, et al.Mater.Sci.Forum, 457-460 (2004) 55, this paper are in conjunction with reference).Micropipe defects is the anti-personnel defective of tool in the SiC crystal, in the world micropipe density is considered as one of key parameter that characterizes SiC monocrystalline quality (reference: Neudeck P G, IEEE Electron Device Lett.15 (1995) 63, this paper are in conjunction with reference).The wrap defective is the another kind of defective that often occurs in the SiC monocrystalline, is easy to induce in crystal growing process the formation (reference: DudleyM, et al.Appl.Phys.Lett.75 (1999) 784, this paper are in conjunction with reference) of micropipe defects.Therefore, the quantity of microtubule in the SiC monocrystalline and wrap defective is controlled, have very strong necessity and practicality.
Reduce microtubule and wrap quantity in the SiC monocrystalline, the main at present approach that adopts has following two kinds: optimize PVT method growth technique (reference: Li H Q, et al.Diam.Relat.Mater.13 (2004) 151), this paper in conjunction with reference to) and adopt " repetition a look unfamiliar regular way " (RAF method) (reference: Nakamura D, et al.Nature 430 (2004) 1009, this paper are in conjunction with reference).All there is certain weak point in these two kinds of technology: the former is limited for the minimizing effect of microtubule in the SiC crystal and wrap quantity, and the repeatability of crystal growth and stable aspect exist not enough; Latter's growth method complexity, long to the having relatively high expectations of crystal post-treatment, cost height, cycle, the laboratory study achievement is difficult to realize rapidly using.
Summary of the invention
At the deficiencies in the prior art, purpose of the present invention just provide a kind of technology simple, be easy to realize, the heat treating method after the SiC single crystal growing cheaply, realize the reduction of microtubule and wrap defects count in the SiC monocrystalline, thereby improve the quality of SiC monocrystalline comprehensively.
For achieving the above object, the present invention proposes the heat treating method after a kind of SiC single crystal growing, may further comprise the steps:
1, takes by weighing the powder of suitable proportioning;
2, the SiC single-crystal surface is covered carbon film;
3, powder and SiC monocrystalline are packed in the thermal treatment crucible, the SiC monocrystalline places powder;
4, crucible is placed process furnace, closed system after vacuumizing in the stove, charges into argon gas;
5, be warming up to predetermined heat treatment temperature, and the insulation certain hour, powered-down, furnace cooling;
6, open process furnace and thermal treatment crucible, take out the SiC monocrystalline, and the SiC single-crystal surface is cleaned, grinds and polish, the SiC monocrystalline of the part that can be eliminated microtubule and wrap defective.
Wherein, powder described in the above-mentioned steps 1 can be the SiC powder, also can be the mixture of SiC powder and Si powder, the granularity of SiC powder and Si powder be between 0.01 millimeter and 1 millimeter, and the weight ratio of SiC powder and Si powder is between 100: 1 and 10: 1 in the mixture.
Further, the carbon film described in the step 2, thickness is between 0.01 millimeter and 0.1 millimeter.
Further again, the crucible described in the step 3, material can be graphite, also can be metal tantalum.
Further again, the predetermined heat treatment temperature described in the step 5 can be between 1400 ℃ and 2000 ℃, and soaking time can be between 0.5 hour and 48 hours.
In the heat treatment process after the SiC single crystal growing, the recrystallization of SiC monocrystalline can take place in the rich Si gas phase in the carbon film of SiC single-crystal surface and the thermal chamber, and the SiC monocrystalline of recrystallization is grown in micropipe defects, thereby fills micropipe defects.The solid-state diffusion process takes place in wrap in heat treatment process, thereby eliminates the part wrap in the SiC monocrystalline.The reduction of microtubule and wrap quantity in the SiC monocrystalline has improved SiC monocrystalline quality simultaneously.
Compared with prior art, the present invention adopts the heat treating method after the SiC single crystal growing, has realized the reduction of microtubule and wrap defects count, and has improved SiC monocrystalline quality comprehensively, have technology simple, realize easily, characteristics such as cost is lower.
Description of drawings
Fig. 1 is the light micrograph of microtubule before thermal treatment among the embodiment one;
Fig. 2 is the light micrograph of microtubule after thermal treatment among the embodiment one;
Fig. 3 is the light micrograph of wrap before thermal treatment among the embodiment one;
Fig. 4 is the electron spectroscopy analysis result of wrap in Fig. 3 square frame;
Fig. 5 is the light micrograph of wrap zone after thermal treatment of Fig. 3 among the embodiment one;
Fig. 6 is the electron spectroscopy analysis result of the boxed area of Fig. 5;
Fig. 7 is preceding X-ray diffraction (006) the crystal face rocking curve that obtains in a certain position of SiC monocrystalline of thermal treatment among the embodiment one;
Fig. 8 is X-ray diffraction (006) the crystal face rocking curve that the position identical with Fig. 5 obtains in the SiC monocrystalline after the thermal treatment among the embodiment one.
Embodiment
The present invention proposes the heat treating method after a kind of SiC single crystal growing, that is: the SiC crystal and the powder that will cover carbon film places crucible to put into process furnace, after vacuumizing in the stove, charges into Ar gas, after being warming up to predetermined heat treatment temperature then and being incubated certain hour, furnace cooling; SiC single-crystal surface after the thermal treatment is cleaned, grinds and polishes, the SiC monocrystalline of the part that can be eliminated microtubule and wrap defective.
Specify the heat treating method after the SiC crystal growth by the following examples:
" embodiment one "
With diameter is that 2 inches, thickness are that the SiC single-crystal surface of 1mm covers the thick carbon film of 0.1mm, put into the plumbago crucible of external diameter 80mm, high 80mm, internal diameter 70mm, dark 75mm, dress highly is the 0.01mm particle diameter SiC powder of 35mm and the mixture of Si powder in the crucible, the weight ratio of SiC powder and Si powder is 10: 1 in the crucible, and the SiC wafer that has covered carbon film places the high powder apart from crucible bottom inwall 20mm.Plumbago crucible is put into process furnace, and after process furnace was vacuumized, logical Ar gas made furnace pressure reach 0.5atm.Intensification makes the interior powder temperature of crucible reach 2000 ℃, is incubated furnace cooling after 0.5 hour, obtains to eliminate the SiC monocrystalline of part microtubule and wrap.
Before thermal treatment, micropipe defects observed typical pattern under opticmicroscope is black hexagonal hole hole as shown in Figure 1 in the SiC monocrystalline in the present embodiment.After thermal treatment, the micropipe defects of SiC monocrystalline under opticmicroscope observed typical pattern as shown in Figure 2, the hexagonal hole hole of microtubule is filled by the SiC monocrystalline.Present embodiment is before thermal treatment, and the observed typical pattern under opticmicroscope of the wrap defective in the SiC monocrystalline is the wrap defective in three square frames among Fig. 3 as shown in Figure 3.Figure 4 shows that the electron spectroscopy analysis result of the wrap in the square frame among Fig. 3, the main component of wrap is C, Si, O, N, S and Na element.After thermal treatment, the zone among Fig. 3 under opticmicroscope observed typical pattern as shown in Figure 5, the wrap before the thermal treatment disappears.Square frame position among Fig. 5 is identical with the square frame position among Fig. 3.Figure 6 shows that the electron spectroscopy analysis result of Fig. 5 square frame inner compartment, main component is Si and C, and the atomic percent of Si and C was near 1: 1.Fig. 7 and shown in Figure 8 be respectively before the thermal treatment and thermal treatment after the rocking curve of X-ray diffraction (006) crystal face that obtains at the same position of SiC monocrystalline.Before the thermal treatment, the rocking curve shown in Fig. 7 is that a plurality of peak positions are superimposed, and the peak width at half height that records the unimodal matched curve of its Gauss is 0.314 °.After the thermal treatment, the rocking curve shown in Fig. 8 is a unimodal curve, and recording its peak width at half height is 0.094 °.
" embodiment two "
With diameter is that 1 inch, thickness are that the SiC single-crystal surface of 0.3mm covers the thick carbon film of 0.01mm, put into the plumbago crucible of external diameter 80mm, high 80mm, internal diameter 70mm, dark 75mm, dress highly is the 1mm particle diameter SiC powder of 28mm in the crucible, and the SiC wafer that has covered carbon film places the SiC powder high apart from crucible bottom inwall 15mm.Plumbago crucible is put into process furnace, and after process furnace was vacuumized, logical Ar gas made furnace pressure reach 0.5atm.Intensification makes the interior SiC powder temperature of crucible reach 1400 ℃, is incubated furnace cooling after 48 hours, obtains to eliminate the SiC monocrystalline of part microtubule and wrap.
In the present embodiment before thermal treatment with thermal treatment after the microtubule pattern identical with embodiment one, the wrap pattern before the thermal treatment is similar to embodiment one with composition, the pattern in wrap zone is similar to embodiment one with composition after the thermal treatment.X-ray diffraction (006) the crystal face rocking curve of SiC monocrystalline is similar to embodiment one before the thermal treatment, the multimodal stack.X-ray diffraction (006) the crystal face rocking curve of SiC monocrystalline same position is similar to embodiment one after the thermal treatment, is unimodal curve, and the peak width at half height of the peak width at half height of rocking curve before than thermal treatment is little.
" embodiment three "
With diameter is that 1 inch, thickness are that the SiC single-crystal surface of 0.5mm covers the thick carbon film of 0.01mm, put into the tantalum crucible of external diameter 80mm, high 80mm, internal diameter 70mm, dark 75mm, dress highly is the 1mm particle diameter SiC powder of 33mm in the crucible, and the SiC wafer that has covered carbon film places the SiC powder high apart from crucible bottom inwall 18mm.Tantalum crucible is put into process furnace, and after process furnace was vacuumized, logical Ar gas made furnace pressure reach 0.5atm.Intensification makes the interior SiC powder temperature of crucible reach 2000 ℃, is incubated furnace cooling after 0.5 hour, obtains to eliminate the SiC monocrystalline of part microtubule and wrap.
In the present embodiment before thermal treatment with thermal treatment after the microtubule pattern identical with embodiment one, the wrap pattern before the thermal treatment is similar to embodiment one with composition, the pattern in wrap zone is similar to embodiment one with composition after the thermal treatment.X-ray diffraction (006) the crystal face rocking curve of SiC monocrystalline is similar to embodiment one before the thermal treatment, the multimodal stack.X-ray diffraction (006) the crystal face rocking curve of SiC monocrystalline same position is similar to embodiment one after the thermal treatment, is unimodal curve, and the peak width at half height of the peak width at half height of rocking curve before than thermal treatment is little.
" embodiment four "
With diameter is that 2 inches, thickness are that the SiC single-crystal surface of 1mm covers the thick carbon film of 0.1mm, put into the tantalum crucible of external diameter 80mm, high 80mm, internal diameter 70mm, dark 75mm, dress highly is the 0.01mm particle diameter SiC powder of 30mm and the mixture of Si powder in the crucible, the weight ratio of SiC powder and Si powder is 100: 1 in the crucible, and the SiC wafer that has covered carbon film places the high powder apart from crucible bottom inwall 16mm.Tantalum crucible is put into process furnace, and after process furnace was vacuumized, logical Ar gas made furnace pressure reach 0.5atm.Intensification makes the interior powder temperature of crucible reach 1400 ℃, is incubated furnace cooling after 48 hours, obtains to eliminate the SiC monocrystalline of part microtubule and wrap.
In the present embodiment before thermal treatment with thermal treatment after the microtubule pattern identical with embodiment one, the wrap pattern before the thermal treatment is similar to embodiment one with composition, the pattern in wrap zone is similar to embodiment one with composition after the thermal treatment.X-ray diffraction (006) the crystal face rocking curve of SiC monocrystalline is similar to embodiment one before the thermal treatment, the multimodal stack.X-ray diffraction (006) the crystal face rocking curve of SiC monocrystalline same position is similar to embodiment one after the thermal treatment, is unimodal curve, and the peak width at half height of the peak width at half height of rocking curve before than thermal treatment is little.
" embodiment five "
The SiC single-crystal surface that will be of a size of 10mm * 10mm, thickness and be 0.8mm covers the thick carbon film of 0.05mm, put into the plumbago crucible of external diameter 80mm, high 80mm, internal diameter 70mm, dark 75mm, dress highly is the 0.5mm particle diameter SiC powder of 37mm and the mixture of Si powder in the crucible, the weight ratio of SiC powder and Si powder is 20: 1 in the crucible, and the SiC wafer that has covered carbon film places the high powder apart from crucible bottom inwall 20mm.Plumbago crucible is put into process furnace, and after process furnace was vacuumized, logical Ar gas made furnace pressure reach 0.5atm.Intensification makes the interior powder temperature of crucible reach 1800 ℃, is incubated furnace cooling after 4 hours, obtains to eliminate the SiC monocrystalline of part microtubule and wrap.
In the present embodiment before thermal treatment with thermal treatment after the microtubule pattern identical with embodiment one, the wrap pattern before the thermal treatment is similar to embodiment one with composition, the pattern in wrap zone is similar to embodiment one with composition after the thermal treatment.X-ray diffraction (006) the crystal face rocking curve of SiC monocrystalline is similar to embodiment one before the thermal treatment, the multimodal stack.X-ray diffraction (006) the crystal face rocking curve of SiC monocrystalline same position is similar to embodiment one after the thermal treatment, is unimodal curve, and the peak width at half height of the peak width at half height of rocking curve before than thermal treatment is little.
" embodiment six "
The SiC single-crystal surface that will be of a size of 10mm * 10mm, thickness and be 1mm covers the thick carbon film of 0.1mm, put into the tantalum crucible of external diameter 80mm, high 80mm, internal diameter 70mm, dark 75mm, dress highly is the 0.5mm particle diameter SiC powder of 35mm in the crucible, and the SiC wafer that has covered carbon film places the high powder apart from crucible bottom inwall 20mm.Tantalum crucible is put into process furnace, and after process furnace was vacuumized, logical Ar gas made furnace pressure reach 0.5atm.Intensification makes the interior SiC powder temperature of crucible reach 1700 ℃, is incubated furnace cooling after 5 hours, obtains to eliminate the SiC monocrystalline of part microtubule and wrap.
In the present embodiment before thermal treatment with thermal treatment after the microtubule pattern identical with embodiment one, the wrap pattern before the thermal treatment is similar to embodiment one with composition, the pattern in wrap zone is similar to embodiment one with composition after the thermal treatment.X-ray diffraction (006) the crystal face rocking curve of SiC monocrystalline is similar to embodiment one before the thermal treatment, the multimodal stack.X-ray diffraction (006) the crystal face rocking curve of SiC monocrystalline same position is similar to embodiment one after the thermal treatment, is unimodal curve, and the peak width at half height of the peak width at half height of rocking curve before than thermal treatment is little.
Claims (7)
1. the heat treating method behind the silicon carbide monocrystal growth is characterized in that: may further comprise the steps:
(1) take by weighing suitable proportioning the SiC powder or, the mixture of SiC and Si powder;
(2) the SiC single-crystal surface is covered carbon film;
(3) powder and SiC monocrystalline are packed in the thermal treatment crucible, the SiC monocrystalline places powder;
(4) crucible is placed process furnace, closed system after vacuumizing in the stove, charges into argon gas;
(5) be warming up to predetermined heat treatment temperature, and the insulation certain hour, powered-down, furnace cooling;
(6) open process furnace and thermal treatment crucible, take out the SiC monocrystalline, and the SiC single-crystal surface is cleaned, grinds and polish, the SiC monocrystalline of the part that can be eliminated microtubule and wrap defective.
2. the heat treating method behind a kind of silicon carbide monocrystal growth according to claim 1 is characterized in that: the described powder of step (1), its granularity is between 0.01 millimeter and 1 millimeter.
3. the heat treating method behind a kind of silicon carbide monocrystal growth according to claim 1 is characterized in that: the weight ratio of described SiC powder of step (1) and Si powder is between 100: 1 and 10: 1.
4. the heat treating method behind a kind of silicon carbide monocrystal growth according to claim 3 is characterized in that: the thickness of the described carbon film of step (2) is between 0.01 millimeter and 0.1 millimeter.
5. the heat treating method behind a kind of silicon carbide monocrystal growth according to claim 4 is characterized in that: the material of the described crucible of step (3) is graphite or metal tantalum.
6. the heat treating method behind a kind of silicon carbide monocrystal growth according to claim 5 is characterized in that: the described predetermined heat treatment temperature of step (5) is between 1400 ℃ and 2000 ℃.
7. the heat treating method behind a kind of silicon carbide monocrystal growth according to claim 6 is characterized in that: the described soaking time of step (5) is between 0.5 hour and 48 hours.
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| CN102534805B (en) * | 2010-12-14 | 2014-08-06 | 北京天科合达蓝光半导体有限公司 | Silicon carbide crystal annealing process |
| CN103114336A (en) * | 2013-03-12 | 2013-05-22 | 中国科学院上海硅酸盐研究所 | Method for annealing silicon carbide wafer |
| CN104538549A (en) * | 2014-12-30 | 2015-04-22 | 厦门大学 | Manufacturing method of SrTiO3 single-crystal resistance switch device |
| CN105543967B (en) * | 2016-02-02 | 2023-02-03 | 北京世纪金光半导体有限公司 | Raw material treatment method for growing 4H high-purity silicon carbide single crystal form by stable PVT method |
| CN106637418B (en) * | 2016-12-09 | 2019-04-09 | 河北同光晶体有限公司 | A kind of heat treatment method of SiC jewel |
| CN107190323A (en) * | 2017-06-06 | 2017-09-22 | 宝鸡文理学院 | A kind of method for growing low defect single-crystal silicon carbide |
| CN107385512B (en) * | 2017-06-30 | 2019-06-25 | 山东天岳先进材料科技有限公司 | The growing method of carbon package volume defect in a kind of inhibition single-crystal silicon carbide |
| CN112048769B (en) * | 2020-07-24 | 2021-08-31 | 山东天岳先进科技股份有限公司 | Device for healing silicon carbide crystal micropipe and application |
| CN111962157B (en) * | 2020-07-24 | 2021-09-28 | 山东天岳先进科技股份有限公司 | Healing method of silicon carbide crystal micropipe, silicon carbide product and application |
| JP2022064015A (en) * | 2020-10-13 | 2022-04-25 | 一般財団法人電力中央研究所 | Manufacturing method and manufacturing apparatus for silicon carbide single crystal, and silicon carbide single crystal ingot |
| JP2023132352A (en) * | 2022-03-10 | 2023-09-22 | キオクシア株式会社 | Evaluation device |
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Effective date of registration: 20191226 Address after: Room 301, Building 9, Tianrong Street, Daxing Biomedical Industry Base, Zhongguancun Science and Technology Park, Daxing District, Beijing 102600 Patentee after: TANKEBLUE SEMICONDUCTOR Co.,Ltd. Address before: 100080 No. 8, South Third Street, Haidian District, Beijing, Zhongguancun Patentee before: INSTITUTE OF PHYSICS, CHINESE ACADEMY OF SCIENCES |
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Application publication date: 20061227 Assignee: Shenzhen Reinvested Tianke Semiconductor Co.,Ltd. Assignor: TANKEBLUE SEMICONDUCTOR Co.,Ltd. Contract record no.: X2023990000684 Denomination of invention: A Heat Treatment Method for Silicon Carbide Single Crystal Growth Granted publication date: 20080709 License type: Common License Record date: 20230725 |