CN103628141A - Method for homogenizing crystalline quality of SiC monocrystal - Google Patents
Method for homogenizing crystalline quality of SiC monocrystal Download PDFInfo
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- CN103628141A CN103628141A CN201310667276.0A CN201310667276A CN103628141A CN 103628141 A CN103628141 A CN 103628141A CN 201310667276 A CN201310667276 A CN 201310667276A CN 103628141 A CN103628141 A CN 103628141A
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Abstract
The invention discloses a method for homogenizing the crystalline quality of a SiC monocrystal, which solves the problem of non-uniform quality of the SiC monocrystal caused by non-uniform stress and thermal field in the existing method for growing the SiC monocrystal. The method comprises the following steps: 1, coating an adhesive Cx(OH)y between a seed crystal and a graphite support, and performing preheating and long-time coking processing on the seed crystal and the graphite support which are coated with the adhesive Cx(OH)y so as to enhance the compactness between the seed crystal and the graphite support; 2, placing powder and the seed crystal in a graphite crucible; 3, performing up-and-down heat-insulating treatment on the crucible and placing the crucible in a rotating mechanism under a vacuum state, wherein the rotating mechanism rotate at the rotating speed of 60 rpm; and 4, growing the SiC monocrystal by a physical vapor phase transmission method. By the method, the requirements of the growth of large-sized high-quality monocrystal materials for the uniformity of the stress and the thermal field are met.
Description
Technical field
The method that the present invention relates to crystal mass homogenizing in a kind of subliming method growth SiC monocrystalline, belongs to electronic industry and technical field of semiconductor.
Background technology
SiC monocrystal material has the advantages such as high heat conductance, high breaking down field strength, high saturated electrons drift speed, the semiconducter device that the SiC monocrystalline of take is prepared as substrate material can improve equipment performance and reliability, in fields such as radar communication, automotive electronics, wind-powered electricity generation, intelligent grid, aerospace, has huge application prospect.At present, generally adopt subliming method to carry out SiC single crystal growing both at home and abroad, the method makes plumbago crucible be warming up to 2200 ℃-2400 ℃ by induction heating, impel SiC split raw material to distil, gaseous substance is transferred to SiC seed crystal face that temperature is lower and formation of deposits monocrystalline on seed crystal under the effect of thermograde
.siC seed crystal and graphite support that this kind of method adopts are all rigid materials, in temperature-rise period due to the difference of thermal expansivity between them the larger stress of SiC crystal inner accumulated that can cause growing.Geometry, the physical attributes etc. such as the lagging material adopting, heater coil, bushing position are not that physics is symmetrical completely, under the condition of high temperature, tend to cause temperature field skewness in plumbago crucible, thereby cause the SiC monocrystalline internal stress distribution of growth uneven, affect the quality of SiC single crystal wafers.Especially along with current 4-6 inch SiC monocrystal material, become the main flow of the market requirement, the growth of this large-size high-quality monocrystal material is stricter for the requirement of stress, warm field uniformity.
Summary of the invention
The invention provides a kind of SiC monocrystalline crystal mass homogenization method, solved stress in existing growth SiC monocrystalline method, a temperature inhomogeneous SiC monocrystalline quality problem of non-uniform causing.
The present invention solves above technical problem by the following technical programs:
A homogenization method for SiC monocrystalline crystal mass, comprises the following steps:
The first step, between seed crystal and graphite support, smear caking agent Cx (OH) y, and by smear the seed crystal of caking agent Cx (OH) y and graphite support when preheating and growing coking process, to strengthen the compactness between seed crystal and graphite support;
Second step, powder, seed crystal are positioned in plumbago crucible;
The 3rd step, crucible is incubated to processing up and down, is then positioned in the rotating mechanism under vacuum state, the rotating speed that rotating mechanism turns with per minute 30 is rotated;
The 4th step, employing physical vapor transport growth SiC monocrystalline.
In the present invention, the material such as the insulation of employing can be selected the hard felt of graphite, soft felt, the hard felt of C-C conjugated fibre.The better quality that can further improve SiC monocrystal material of consistence, homogeneity of the lagging material adopting.In the present invention, adopting Cx (OH) y can be the materials such as edible sucrose, glucose, caramel, because SiC seed crystal and graphite support are all rigid materials, in temperature-rise period, due to the difference of thermal expansivity between them the larger stress of SiC crystal inner accumulated that can cause growing, make crystal mass poor.Caking agent Cx (OH) y is processed in coking when preheating and growing, and strengthens the compactness between seed crystal and graphite support, can alleviate the stress accumulation problems that thermal expansivity difference is brought, thereby improve crystal mass.
Described rotating mechanism can be support type rotating mechanism, can be also pull-type rotating mechanism.
Described rotation mode can be plumbago crucible rotation, and outer insulation maintains static, and can be also outer insulation rotation, and plumbago crucible maintains static.The mechanism design that realizes crucible rotation in vacuum system is relatively more easy.
What the present invention adopted is that outer insulation maintains static, and the mode of plumbago crucible rotation is carried out the growth of SiC monocrystalline, has met the growth of large-size high-quality monocrystal material for the requirement of stress, warm field uniformity.Improved the homogeneity of resistivity in the peak width at half height homogeneity of SiC monocrystalline and doping process.
Accompanying drawing explanation
Fig. 1 is seed crystal technique for sticking route map of the present invention;
Fig. 2 is the photo of employing seed crystal technique for sticking of the present invention 1 growing crystal;
Fig. 3 is the photo of employing seed crystal technique for sticking of the present invention 1 growing crystal;
Fig. 4 is employing of the present invention photo and the quality test of wafer peak width at half height of technique growing crystal without spin;
Fig. 5 is photo and the quality test of wafer peak width at half height of employing rotating technics growing crystal of the present invention;
Fig. 6 is the employing of the present invention growing semi-insulated monocrystalline resistivity distribution of technique and the quality test of wafer peak width at half height without spin;
Fig. 7 is the growing semi-insulated monocrystalline resistivity distribution of employing rotating technics of the present invention and the quality test of wafer peak width at half height.
Embodiment
Below the preferred embodiments of the present invention are described, preferred embodiment described herein only, for description and interpretation the present invention, is not intended to limit the present invention.
Embodiment 1:
The SiC powder that employing purity is 99.99% is as raw material, adopting 3 inches of 4H-SiC wafers is seed crystal, powder and seed crystal are positioned in crucible, seed crystal technique for sticking is according to the technique 1 in Fig. 1, the 30mm that is specially that makes to expect seed crystal, growth temperature is controlled at 2000-2300 ℃, pours Ar gas to 100Pa, grow and after 50 hours, obtain crystal material piece (being designated as material piece 1, as Fig. 2); With same assembling, carry out SiC single crystal growing again, seed crystal technique for sticking, according to the technique 2 in Fig. 1, obtains crystal material piece (being designated as material piece 2, as Fig. 3) after growing 50 hours.It is more that visible adopting process 1 obtains the defects such as crystals cavity, microtubule, and the crystals transparency defect that adopting process 2 obtains is less.
Embodiment 2:
The SiC powder that employing purity is 99.99% is as raw material, adopting 3 inches of 4H-SiC wafers is seed crystal, powder and seed crystal are positioned in crucible, make to expect the 30mm that is specially of seed crystal, growth temperature is controlled at 2000-2300 ℃, pour Ar gas to 100Pa, after growing 50 hours, obtain crystal material piece (being designated as material piece 3, as Fig. 4); With same assembling, carry out SiC single crystal growing again, setting crucible rotation rate is 5 revs/min, obtains crystal material piece (being designated as material piece 4, as Fig. 5) after growing 50 hours.Adopt opticmicroscope crystalline substance to crystal edge analysis, adopt the crystal edge quality of crucible rotation technique growth to be obviously better than not rotating the monocrystalline of growth, material piece is carried out carrying out analytical test after round as a ball, cutting, grinding and polishing, adopt the crystal peak width at half height of rotating technics growth more even.
Embodiment 3:
The SiC powder that employing purity is 99.999% is as raw material, and 3 inches of 4H-SiC monocrystalline, as seed crystal, are mixed the single crystal growing of vanadium semi-insulation SiC.Powder and seed crystal are positioned in crucible, make to expect the 30mm that is specially of seed crystal, growth temperature is controlled at 2000-2300 ℃, pours Ar gas to 100Pa, obtains crystal material piece (being designated as material piece 5, as Fig. 6) after growing 100 hours.With same assembling, carry out SiC single crystal growing again, setting crucible rotation rate is 5 revs/min, obtains crystal material piece (being designated as material piece 6, as Fig. 7) after growing 100 hours.Material piece is justified, carried out analytical test after cutting, grinding and polishing, better before single crystal wafers resistivity distribution and peak width at half height distributing homogeneity more do not rotate.
Finally it should be noted that: the foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, although the present invention is had been described in detail with reference to previous embodiment, for a person skilled in the art, it still can be modified or be equal to replacement aforementioned each embodiment.Within the spirit and principles in the present invention all, any modification of doing, be equal within replacement, improvement etc. all should be included in protection scope of the present invention.
Claims (1)
1. a SiC monocrystalline crystal mass homogenization method, comprises the following steps:
The first step, between seed crystal and graphite support, smear caking agent Cx (OH) y, and by smear the seed crystal of caking agent Cx (OH) y and graphite support when preheating and growing coking process, to strengthen the compactness between seed crystal and graphite support;
Second step, powder, seed crystal are positioned in plumbago crucible;
The 3rd step, crucible is incubated to processing up and down, is then positioned in the rotating mechanism under vacuum state, the rotating speed that rotating mechanism turns with per minute 30 is rotated;
The 4th step, employing physical vapor transport growth SiC monocrystalline.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105040103A (en) * | 2015-06-25 | 2015-11-11 | 江苏艾科勒科技有限公司 | Growing device for high-quality silicon carbide crystals |
| CN105256371A (en) * | 2015-11-30 | 2016-01-20 | 山东省科学院能源研究所 | Device for improving temperature field uniformity of crystal growing furnace of physical vapor transport method |
| CN105442044A (en) * | 2015-12-17 | 2016-03-30 | 中国电子科技集团公司第二研究所 | Crucible independent rotating mechanism of SiC single crystal growth equipment |
| CN105442038A (en) * | 2015-12-17 | 2016-03-30 | 中国电子科技集团公司第二研究所 | Crucible rotating-type silicon carbide single crystal growth method |
| CN105568370A (en) * | 2016-03-01 | 2016-05-11 | 山东大学 | Centrally symmetric silicon carbide (SiC) single crystal growing device and method |
| CN108588836A (en) * | 2018-06-14 | 2018-09-28 | 河北普兴电子科技股份有限公司 | Growing silicon carbice crystals thermal field rotating device |
| CN109957841A (en) * | 2017-12-25 | 2019-07-02 | 昭和电工株式会社 | The manufacturing method of single-crystal silicon carbide |
| WO2020103279A1 (en) * | 2018-11-23 | 2020-05-28 | 山东天岳先进材料科技有限公司 | Method for improving yield of silicon carbide powder |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105040103A (en) * | 2015-06-25 | 2015-11-11 | 江苏艾科勒科技有限公司 | Growing device for high-quality silicon carbide crystals |
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| CN105442038A (en) * | 2015-12-17 | 2016-03-30 | 中国电子科技集团公司第二研究所 | Crucible rotating-type silicon carbide single crystal growth method |
| CN105568370A (en) * | 2016-03-01 | 2016-05-11 | 山东大学 | Centrally symmetric silicon carbide (SiC) single crystal growing device and method |
| CN109957841A (en) * | 2017-12-25 | 2019-07-02 | 昭和电工株式会社 | The manufacturing method of single-crystal silicon carbide |
| CN108588836A (en) * | 2018-06-14 | 2018-09-28 | 河北普兴电子科技股份有限公司 | Growing silicon carbice crystals thermal field rotating device |
| WO2020103279A1 (en) * | 2018-11-23 | 2020-05-28 | 山东天岳先进材料科技有限公司 | Method for improving yield of silicon carbide powder |
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Application publication date: 20140312 |