CN101805927B - Grower of high-purity semi-insulating silicon carbide single crystal - Google Patents
Grower of high-purity semi-insulating silicon carbide single crystal Download PDFInfo
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- CN101805927B CN101805927B CN2010101523944A CN201010152394A CN101805927B CN 101805927 B CN101805927 B CN 101805927B CN 2010101523944 A CN2010101523944 A CN 2010101523944A CN 201010152394 A CN201010152394 A CN 201010152394A CN 101805927 B CN101805927 B CN 101805927B
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- silicon carbide
- semi
- insulating silicon
- cooling water
- growing apparatus
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 50
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 239000013078 crystal Substances 0.000 title abstract description 29
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000010439 graphite Substances 0.000 claims abstract description 38
- 239000000498 cooling water Substances 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000011261 inert gas Substances 0.000 claims abstract description 8
- 241000209456 Plumbago Species 0.000 claims description 33
- 230000000740 bleeding effect Effects 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims 1
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 abstract description 14
- 239000007789 gas Substances 0.000 abstract description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 9
- 229910052786 argon Inorganic materials 0.000 abstract description 7
- 238000005516 engineering process Methods 0.000 abstract description 6
- 229910002804 graphite Inorganic materials 0.000 abstract description 5
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 4
- 229910001873 dinitrogen Inorganic materials 0.000 abstract 1
- 230000006698 induction Effects 0.000 abstract 1
- 239000012466 permeate Substances 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 10
- 239000011229 interlayer Substances 0.000 description 8
- 239000010410 layer Substances 0.000 description 8
- 239000002245 particle Substances 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 229910052720 vanadium Inorganic materials 0.000 description 3
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 3
- 239000002826 coolant Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000008054 signal transmission Effects 0.000 description 2
- 239000011863 silicon-based powder Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 230000032696 parturition Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to a grower of a high-purity semi-insulating silicon carbide single crystal, belonging to the field of crystal growth. The grower comprises a vacuum chamber, a graphite crucible and an induction coil. The grower of the invention is used for growing the high-purity semi-insulating silicon carbide single crystal based on the technology of physical vapor transport (PVT) without specific growing processes. The invention is mainly characterized in that the side wall of a growing furnace is in a multi-layer (at least three-layer) structure, and more than two independent spaces are formed in the side wall and are respectively used for introducing cooling water and high-purity inert gas (generally, high-purity argon gas) or introducing cooling water and vacuumizing. The grower of the invention can be used for effectively isolating the graphite crucible from air, preventing nitrogen gas in the air from entering the graphite crucible in the growing process and effectively controlling nitrogen elements to permeate into the growing silicon carbide crystal, thereby obtaining the high-purity semi-insulating silicon carbide single crystal.
Description
Technical field
The invention belongs to field of crystal growth, be specifically related to a kind of growing apparatus of high-purity semi-insulating silicon carbide body monocrystalline.
Background technology
Silit (SiC) thermal conductivity high (about 5.0W/cm), high (the about 2.7x10 of saturated electrons mobility
7Cm/s), breakdown electric field high (about 3MV/cm), be very suitable for making high pressure, the high-frequency electron device that need under high-power or high temperature, operate.Meanwhile, the chemicalstability of SiC, anti-irradiation ability are all very strong, and therefore, SiC has become the generally acknowledged new generation of semiconductor material that can replace first-generation semi-conductor Si and s-generation semiconductor GaAs.
Semi-insulating silicon carbide crystalloid has important application on devices such as Metal-oxide-semicondutor FET, semi-conductor photoconduction switch.Through in carborundum crystals, mixing a certain amount of v element, a certain amount of deep energy level can be provided, realize the semi-insulating of silit.But in during using the vanadium doped crystal as the substrate making, vanadium can be caught negative charge and caused interior grid (grown-in gate) effect of giving birth to.Therefore, be in device performance and consider, preferably do not use the adulterated semi-insulating silicon carbide crystalloid of vanadium, and use high-purity semi-insulating silicon carbide crystalloid.
The key of growth high-purity semi-insulating silicon carbide crystalloid is to reduce the quantity of shallow donor, shallow acceptor energy level, improves resistivity.But owing to containing impurity such as trace of Al, B inevitably in crucible, powder, the lagging material; And; N element in the process of growth air can mix the crystal of growth in a large number; They form a large amount of shallow energy levels in crystal, make the growth of high-purity semi-insulating silicon carbide crystalloid have very big difficulty.
Through using high purity graphite crucible, high-purity powder, high-purity lagging material, can reduce impurity concentrations such as Al, B effectively, reduce the shallow energy level of part.But the stopping property of conventional growth apparatus is limited, and leak rate is generally 10
-5PaL/s; Under growth sublimity, reach the crystal growth more than 50 hours near vacuum; The nitrogen amount that from atmosphere, gets in the chamber is very big, mixes crystalline N amount of element and is difficult to reduce, and becomes the principal element that restriction institute growing crystal improves resistivity, realizes high-purity semi-insulating.If adopt existing crystal growing apparatus, take the growth method of conventional PVT technology, the crystalline resistivity that obtains of can growing is generally less than 10
4Ω cm, micropipe density is 100～300cm
-2
Summary of the invention
The objective of the invention is to overcome the defective of prior art, the growing apparatus of a kind of high-purity semi-insulating (HPSI) silit (SiC) body monocrystalline is provided.
The growing apparatus of high-purity semi-insulating silicon carbide body monocrystalline of the present invention comprises: Vakuumkammer, plumbago crucible and ruhmkorff coil, and wherein, said Vakuumkammer comprises body of heater and bell; Be provided with plumbago crucible and ruhmkorff coil in the said body of heater, and said ruhmkorff coil is around the plumbago crucible outer wall; Said sidewall of the furnace body is provided with separate cavities and advances/bleeding point, and bottom of furnace body also is provided with the bleeding point that is connected with vacuum pump; And said sidewall of the furnace body inside is provided with separate separate cavities and cooling water cavity from inside to outside successively.
Preferable, be filled with high purity inert gas in the said separate cavities or be vacuum.
Preferable, the correspondence position of said separate cavities and cooling water cavity is provided with a plurality of flanges.Its effect is the exchange of the inside and outside material (being mainly pressure equilibrium gas) of realization multiple bedded furnace side structure and the transmission of signal (being mainly pressure data).
Preferably, the quantity of said flange is 2, is provided with two flanges at the correspondence position of the different layers of the sidewall of reactors, is used on the basis that guarantees sealing property, ruhmkorff coil being passed.
Preferable, the interior of said bell is provided with separate separate cavities and cooling water cavity from inside to outside successively, is provided with the cooling water cavity of hollow in the end face of said bell, and the cooling water cavity in the said bell end face is communicated with the interior cooling water cavity of bell sidewall.
Preferable, also be provided with adiabator layer between said plumbago crucible and the ruhmkorff coil.
Preferably, also be provided with TP and pressure transmitter in the said body of heater.
Preferably, said sidewall of the furnace body is respectively equipped with cooling water inlet and cooling water outlet, and further preferred, said cooling water inlet is positioned at the lower sides of reactors, and said cooling water outlet is positioned at the upper portion side wall of reactors.
Preferably, the material of said body of heater and bell is a metallic substance, further is preferably stainless steel.
Can charge into high purity inert gas in the said separate cavities, be preferably high-purity argon gas; Or vacuumize.Through the separate space that forms between close two-layer in the sidewall of the furnace body is applied malleation (feeding high purity inert gas) or negative pressure (vacuumizing); Between air and plumbago crucible inside, form one " gas interlayer "; If should " interlayer " be malleation; Then the high purity inert gas in " interlayer " gets into plumbago crucible, if " interlayer " is negative pressure, then the pressure equilibrium gas (being generally high-purity argon gas) in the plumbago crucible gets into " interlayer "; The situation that all can not occur the air admission plumbago crucible under two kinds of situation is to guarantee that body of heater makes plumbago crucible and air isolated fully in process of growth.
The growing apparatus of high-purity semi-insulating silicon carbide body monocrystalline of the present invention is when being used for crystal growth, and powder (being generally the SiC particle, perhaps the mixture of Si powder and C powder) is positioned at the bottom of plumbago crucible, and seed crystal is positioned at the top of plumbago crucible.
The present invention is based on physical vapor transmission technology growing silicon carbide body monocrystalline; Plumbago crucible and air are isolated fully in the process of growth; Avoid airborne nitrogen entering plumbago crucible and mixed the carborundum crystals of growth, increased crystal resistivity, obtained high-purity semi-insulating silicon carbide crystalloid.Body of heater of the present invention comprises bell and furnace sidewall; In order to realize that plumbago crucible and air are isolated fully in the process of growth; Bell is also similar with furnace sidewall; Be multilayered structure, the separate space that forms between the adjacent layers can be led to water coolant and high purity inert gas (generally being high-purity argon gas) respectively, or leads to water coolant and vacuumize respectively.In the bell by a separate space that forms between the adjacent layers, should with furnace sidewall in be communicated with by a separate space that forms between the adjacent layers, could guarantee that like this entire equipment sealing has also realized the isolated fully of plumbago crucible and air in the poorest place relatively.Isolated fully plumbago crucible and air in the process of grow silicon carbide crystals are avoided airborne nitrogen to get into plumbago crucible and are also further mixed crystals, thereby improve the crystalline resistivity of being grown, and obtain high-purity semi-insulating silicon carbide crystalloid.Through growing apparatus of the present invention, can make crystal resistivity greater than 10
5Ω cm, micropipe density is less than 100cm
-2, and diameter is greater than the many types of high-purity semi-insulating silicon carbide crystal ingot of 2 inches 6H.
Description of drawings
The structural representation of the growing apparatus of Fig. 1 high-purity semi-insulating silicon carbide body of the present invention monocrystalline.
Reference numeral: 1, bell; 2, body of heater; 3, cooling water inlet; 4, cooling water outlet; 5, separate cavities advances/bleeding point; 6, outward flange; 7, inside flange; 8, bleeding point, 9, graphite thermal insulation layer; 10, plumbago crucible; 11, powder; 12, silicon carbide seed; 13, ruhmkorff coil; 14, separate cavities; 15, cooling water cavity; 16, TP; 17, pressure transmitter.
Embodiment
Below will provide two embodiment with reference to the present invention.Yet the present invention can come out with multiple different embodied, and is not to be understood that the embodiment that provides at this for being subject to; Just the opposite, these embodiment being provided is in order to expose more thoroughly with complete, so that scope of the present invention is passed to those skilled in the art fully.
Embodiment 1
The crystal growing furnace that uses in the present embodiment is as shown in Figure 1; The growing apparatus of this high-purity semi-insulating silicon carbide body monocrystalline comprises: body of heater 2 and bell 1, plumbago crucible 10 and ruhmkorff coil 13; Wherein, Be provided with plumbago crucible 10 and ruhmkorff coil 13 in the said body of heater 2, and ruhmkorff coil 13 is around plumbago crucible 10 outer walls; Body of heater 2 sidewalls are provided with separate cavities and advance/bleeding point 5, and the bottom of body of heater 2 also is provided with the bleeding point 8 that is connected with vacuum pump; And body of heater 2 interior are provided with separate separate cavities 14 and cooling water cavity 15 from inside to outside successively.The separate cavities 14 of body of heater 2 interior and the correspondence position of cooling water cavity 15 are provided with outward flange 6 and inside flange 7.The effect of outward flange 6 and inside flange 7 is on the basis that guarantees sealing property; Realize the exchange of the material (being mainly pressure equilibrium gas) that the multiple bedded furnace side structure is inside and outside and the transmission of signal (being mainly pressure data), and the lead-in wire of ruhmkorff coil can be passed through.Also be provided with adiabator layer 9 between plumbago crucible 10 and the ruhmkorff coil 13.Also be provided with TP 16 and pressure transmitter 17 in the body of heater 2.The lower sides of body of heater 2 is provided with cooling water inlet 3, and the upper portion side wall of body of heater 2 is provided with cooling water outlet 4.Wherein, the material of body of heater 2 and bell 1 is a stainless steel.
The sidewall of bell 1 is provided with separate separate cavities 14 and cooling water cavity 15 from inside to outside successively, is provided with the cooling water cavity 15 of hollow in the end face of bell 1, and the cooling water cavity 15 in the bell 1 is communicated with the interior cooling water cavity 15 of bell 1 sidewall.
Charge into high-purity argon gas in the separate cavities 14.Through the separate space that forms between separate cavities 14 in body of heater 2 sidewalls and the cooling water cavity 15 is applied malleation (feeding high purity inert gas); Between air and plumbago crucible inside, form one " gas interlayer "; Because should " gas interlayer " be malleation; Therefore the high-purity argon gas in " gas interlayer " gets into plumbago crucible, can not occur the situation of air admission plumbago crucible in this case, to guarantee that body of heater makes plumbago crucible and air isolated fully in process of growth.
When being used for crystal growth, powder 11 (this powder is the SiC particle, perhaps the mixture of Si powder and C powder) is positioned at the bottom of plumbago crucible 10, and silicon carbide seed 12 is positioned at the top of plumbago crucible 10.
Adopt the growing apparatus of high-purity semi-insulating silicon carbide body monocrystalline as shown in Figure 1; Wherein advance/bleeding point 5 feeding high-purity argon gas, put into the SiC powder 11 of 100 microns of particle diameters in the plumbago crucible 10, use 6H-SiC (0001) Si face as silicon carbide seed 12 from separate cavities; Use traditional P VT technology; Power on the control ruhmkorff coil 13 is 7.2Kw, and reactors internal pressure 30Torr grows after 50 hours; Can obtain length greater than 2cm, diameter is greater than the many types of high-purity semi-insulating silicon carbide crystal ingot of 2 inches 6H.Crystal resistivity is greater than 10
5Ω cm, micropipe density is less than 100cm
-2
Adopt the growing apparatus of high-purity semi-insulating silicon carbide body monocrystalline as shown in Figure 1, wherein separate cavities advance/bleeding point 5 connects vacuum pump and vacuumizes, and puts into the SiC powder 11 of 100 microns of particle diameters in the crucible 10; Use 4H-SiC (000-1) C face as seed crystal, use traditional P VT technology, the power on the control ruhmkorff coil 13 is 6.8Kw; Reactors internal pressure 10Torr; Grow after 50 hours, can obtain length greater than 2cm, diameter is greater than the many types of high-purity semi-insulating silicon carbide crystal ingot of 2 inches 4H.Crystal resistivity is greater than 10
5Ω cm, micropipe density is less than 100cm
-2
Claims (9)
1. the growing apparatus of a semi-insulating silicon carbide body monocrystalline, this growing apparatus comprises: Vakuumkammer, plumbago crucible and ruhmkorff coil, wherein, said Vakuumkammer comprises body of heater and bell; Be provided with plumbago crucible and ruhmkorff coil in the said body of heater, and said ruhmkorff coil is around the plumbago crucible outer wall; Said sidewall of the furnace body is provided with separate cavities and advances/bleeding point, and bottom of furnace body also is provided with the bleeding point that is connected with vacuum pump; And said sidewall of the furnace body inside is provided with separate separate cavities and cooling water cavity from inside to outside successively.
2. the growing apparatus of the semi-insulating silicon carbide body monocrystalline described in claim 1 is characterized in that, is filled with high purity inert gas in the said separate cavities or is vacuum.
3. the growing apparatus of the semi-insulating silicon carbide body monocrystalline described in claim 1; It is characterized in that; The interior of said bell is provided with separate separate cavities and cooling water cavity from inside to outside successively; Said bell top is provided with the cooling water cavity of hollow, and the cooling water cavity in the said bell top is communicated with the interior cooling water cavity of bell sidewall.
4. the growing apparatus of the semi-insulating silicon carbide body monocrystalline described in claim 1 is characterized in that, also is provided with adiabator layer between said plumbago crucible and the ruhmkorff coil.
5. the growing apparatus of the semi-insulating silicon carbide body monocrystalline described in claim 1 is characterized in that, also is provided with TP and pressure transmitter in the said body of heater.
6. the growing apparatus of the semi-insulating silicon carbide body monocrystalline described in claim 1 is characterized in that said sidewall of the furnace body is respectively equipped with cooling water inlet and cooling water outlet.
7. the growing apparatus of the semi-insulating silicon carbide body monocrystalline described in claim 6 is characterized in that said cooling water inlet is positioned at the lower sides of body of heater, and said cooling water outlet is positioned at the upper portion side wall of body of heater.
8. like the growing apparatus of arbitrary described semi-insulating silicon carbide body monocrystalline among the claim 1-7, it is characterized in that the material of said body of heater and bell is a metal.
9. the growth method of a semi-insulating silicon carbide body monocrystalline is carried out in the growing apparatus of this method arbitrary described semi-insulating silicon carbide body monocrystalline in claim 1-8.
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| CN101805927A CN101805927A (en) | 2010-08-18 |
| CN101805927B true CN101805927B (en) | 2012-05-30 |
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| CN102260934A (en) * | 2011-02-24 | 2011-11-30 | 西安诚瑞科技发展有限公司 | Continuous induction heating type fiber high-temperature carbonizing device |
| CN202643822U (en) * | 2011-06-17 | 2013-01-02 | 天津津航技术物理研究所 | Device capable of preparing zinc selenide or zinc sulfide lamination polycrystal optical material |
| JP5556761B2 (en) | 2011-07-28 | 2014-07-23 | 株式会社デンソー | Silicon carbide single crystal manufacturing equipment |
| CN103320851A (en) * | 2013-06-05 | 2013-09-25 | 中国科学院上海硅酸盐研究所 | Large-size 15R silicon carbide crystal preparation method |
| CN106048729B (en) * | 2016-06-28 | 2019-04-09 | 山东天岳先进材料科技有限公司 | A kind of PVT method major diameter silicon carbide monocrystal growth device |
| CN107723798B (en) * | 2017-10-30 | 2020-06-02 | 中国电子科技集团公司第四十六研究所 | Growth device and method for efficiently preparing high-purity semi-insulating silicon carbide single crystal |
| CN108130593A (en) * | 2017-12-20 | 2018-06-08 | 中国科学院上海硅酸盐研究所 | A kind of crystal growing furnace attemperator |
| CN111074333A (en) * | 2018-10-19 | 2020-04-28 | 中国电子科技集团公司第四十八研究所 | Single crystal growth equipment and use method thereof |
| CN111411401A (en) * | 2020-05-22 | 2020-07-14 | 北京北方华创微电子装备有限公司 | Silicon carbide crystal growing device |
| CN113122923B (en) * | 2021-04-16 | 2022-07-12 | 上海天岳半导体材料有限公司 | High-quality silicon carbide crystal and growing method and device thereof |
| CN113637953B (en) * | 2021-08-06 | 2023-09-01 | 苏州步科斯新材料科技有限公司 | Rapid cooling silicon carbide coating deposition device and use method |
| CN116815001A (en) * | 2023-08-31 | 2023-09-29 | 西安聚能超导线材科技有限公司 | Preparation method of tin-titanium alloy rod, tin-titanium alloy rod and superconducting wire |
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| US5683507A (en) * | 1995-09-05 | 1997-11-04 | Northrop Grumman Corporation | Apparatus for growing large silicon carbide single crystals |
| CN1247831C (en) * | 2003-11-14 | 2006-03-29 | 中国科学院物理研究所 | Silicon carbide crystal growth apparatus |
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