CN113026099A - Silicon carbide single crystal growth control device and control method - Google Patents
Silicon carbide single crystal growth control device and control method Download PDFInfo
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- CN113026099A CN113026099A CN202110248412.7A CN202110248412A CN113026099A CN 113026099 A CN113026099 A CN 113026099A CN 202110248412 A CN202110248412 A CN 202110248412A CN 113026099 A CN113026099 A CN 113026099A
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 105
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 105
- 239000013078 crystal Substances 0.000 title claims abstract description 104
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 124
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 96
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 96
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 94
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 94
- 239000010703 silicon Substances 0.000 claims abstract description 94
- 238000010438 heat treatment Methods 0.000 claims abstract description 45
- 238000012544 monitoring process Methods 0.000 claims abstract description 8
- 239000007789 gas Substances 0.000 claims description 191
- 229910052751 metal Inorganic materials 0.000 claims description 25
- 239000002184 metal Substances 0.000 claims description 25
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 19
- 239000001257 hydrogen Substances 0.000 claims description 16
- 229910052739 hydrogen Inorganic materials 0.000 claims description 16
- 239000000126 substance Substances 0.000 claims description 9
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical group ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 claims description 8
- 230000003247 decreasing effect Effects 0.000 claims description 7
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 6
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 5
- 150000001336 alkenes Chemical class 0.000 claims description 5
- 150000001345 alkine derivatives Chemical class 0.000 claims description 5
- 230000002093 peripheral effect Effects 0.000 claims description 5
- 230000020169 heat generation Effects 0.000 claims 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 13
- 239000012495 reaction gas Substances 0.000 description 12
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 11
- 239000012535 impurity Substances 0.000 description 8
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 6
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 6
- 239000001294 propane Substances 0.000 description 5
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 4
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 4
- 229910001425 magnesium ion Inorganic materials 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 235000012431 wafers Nutrition 0.000 description 3
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 2
- 239000001273 butane Substances 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 238000004943 liquid phase epitaxy Methods 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229910001629 magnesium chloride Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 2
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000007792 gaseous phase Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
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- 239000007787 solid Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Images
Classifications
-
- 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
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/16—Controlling or regulating
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/14—Feed and outlet means for the gases; Modifying the flow of the reactive gases
-
- 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
Abstract
The invention provides a silicon carbide single crystal growth control device which comprises a shell, a heating device, a silicon source gas pipeline and a carbon source gas pipeline. A reaction chamber is formed in the shell, and a silicon carbide seed crystal placing position is arranged in the reaction chamber; the heating device is arranged in the shell and used for controlling the internal temperature of the reaction chamber; the silicon source gas pipeline is used for introducing silicon source gas into the reaction chamber, and the carbon source gas pipeline is used for introducing carbon source gas into the reaction chamber; the silicon source gas pipeline is provided with a first mass flow controller used for monitoring and controlling the flow of the silicon source gas; the carbon source gas pipeline is provided with a second mass flow controller for monitoring and controlling the flow of the carbon source gas. The invention also provides a silicon carbide single crystal growth control method. The invention can adjust and control the ratio of the flow of the silicon source gas to the flow of the carbon source gas, so that the ratio of Si in the silicon source gas to C in the carbon source gas in the reaction chamber is 1:1, and the SiC single crystal with high purity and high quality can be prepared.
Description
Technical Field
The invention relates to the technical field of silicon carbide preparation, in particular to a silicon carbide single crystal growth control device and a control method.
Background
Silicon carbide material (SiC) has many advantages: the material has the advantages of wide forbidden band, good heat-conducting property, high breakdown electric field, high electron saturation rate, good thermal stability and strong chemical stability. The SiC has large forbidden band width and is suitable for developing short-wave photoelectronic devices; the heat conducting property is good, and the SiC-based device can work at high temperature; the electron saturation rate is high, and the method is suitable for manufacturing high-frequency devices; the breakdown electric field is high, which is beneficial to manufacturing high-power devices; the chemical stability is strong, and the device can work in a corrosive environment. Therefore, high quality SiC crystals/wafers can be said to be the core foundation of the SiC semiconductor industry, and the links of the SiC semiconductor industry include "SiC single crystal substrate-epitaxial wafer-chip and package-application". Each industrial link has higher requirements on the impurity content of the SiC single crystal wafer. The low quality of the SiC single crystal wafer affects the quality and repeatability of the epitaxial thin film and also causes adverse effects such as excessive leakage current on the device, so high quality of the SiC single crystal is particularly important in the semiconductor industry.
There are three main methods for preparing SiC: liquid Phase Epitaxy (LPE), High Temperature Physical Vapor Transport (HTPVT), and High Temperature Chemical Vapor Deposition (HTCVD). Among them, the HTCVD method has the most important advantage of being advantageous for preparing high-purity and high-quality semi-insulating silicon carbide crystals because of high purity and low impurity content of special gases, but because it is difficult to control the ratio of carbon source to silicon source in the reaction gas, many defects will be formed in the SiC crystal with more or less carbon, which affects the quality and purity of the SiC crystal, and thus the use of HTCVD method for preparing SiC is limited.
Disclosure of Invention
The invention mainly aims to provide a silicon carbide single crystal growth control device, which aims to control the ratio of a silicon source and a carbon source in reaction gas so as to prepare high-purity and high-quality SiC crystals by an HPTVD method.
In order to achieve the above object, the present invention provides a silicon carbide single crystal growth control apparatus comprising:
the device comprises a shell, a reaction cavity is formed in the shell, and a silicon carbide seed crystal placing position is arranged in the reaction cavity;
the heating device is arranged on the shell and used for controlling the internal temperature of the reaction chamber; and the number of the first and second groups,
the silicon source gas pipeline is used for introducing silicon source gas into the reaction cavity, and the carbon source gas pipeline is used for introducing carbon source gas into the reaction cavity; wherein the content of the first and second substances,
the silicon source gas pipeline is provided with a first mass flow controller, the carbon source gas pipeline is provided with a second mass flow controller, the first mass flow controller is used for monitoring and controlling the flow of the silicon source gas, and the second mass flow controller is used for monitoring and controlling the flow of the carbon source gas.
Optionally, the flow directions of the silicon source gas pipeline and the carbon source gas pipeline are from bottom to top.
Optionally, the silicon carbide single crystal growth control device further comprises a hydrogen pipeline, the hydrogen pipeline is communicated with the reaction chamber, and the hydrogen pipeline is used for introducing hydrogen into the reaction chamber; and/or the silicon carbide single crystal growth control device further comprises a metal remover pipeline, the metal remover pipeline is communicated with the reaction chamber, and the metal remover pipeline is used for introducing metal removing gas into the reaction chamber.
Optionally, the silicon carbide seed crystal placement location is disposed at a center of a top wall of the reaction chamber.
Optionally, the heating device is a heating coil, and the heating coil is wound on the peripheral side wall of the reaction chamber.
Optionally, the heating coil includes a plurality of sub-coils arranged side by side from bottom to top, and the heating temperatures of the plurality of sub-coils decrease from bottom to top.
The invention also provides a silicon carbide single crystal growth control method, which comprises the following steps:
placing the silicon carbide seed crystal in a silicon carbide seed crystal placing position in the reaction chamber;
controlling the internal temperature of the reaction chamber by a heating device;
introducing silicon source gas into the reaction chamber through a silicon source gas pipeline;
introducing a carbon source gas into the reaction chamber through a carbon source gas pipeline; and the number of the first and second groups,
a first mass flow controller at the silicon source gas line and a second mass flow controller at the carbon source gas line are adjusted to control the ratio of the silicon source gas flow to the carbon source gas flow.
Further, the control method further includes the steps of:
introducing hydrogen into the reaction chamber through a hydrogen pipeline; and/or introducing dichloroethylene gas into the reaction chamber through a metal remover pipeline.
Further, the silicon source gas pipeline with the airflow direction of carbon source gas pipeline all from the bottom up, heating device is heating coil, heating coil winding set up in reaction chamber's week lateral wall, the step of the inside temperature through heating device control reaction chamber specifically includes following step:
controlling the heating temperature of the heating coil to be decreased from bottom to top;
controlling the temperature range of the silicon source gas and the carbon source gas to be 2300-2800 ℃ when the silicon source gas and the carbon source gas enter the reaction chamber; and the number of the first and second groups,
controlling the temperature range of the silicon carbide seed crystal placement position to be 1800-2200 ℃.
Further, in the step of introducing a silicon source gas into the reaction chamber through a silicon source gas pipeline, the silicon source gas is SiH4；
In the step of introducing the carbon source gas into the reaction chamber through the carbon source gas pipeline, the carbon source gas is any one of alkane, alkene and alkyne.
The invention provides a silicon carbide single crystal growth control device, which is characterized in that a silicon source gas pipeline and a carbon source gas pipeline are arranged to introduce silicon source gas and carbon source gas into a reaction chamber, mass flow controllers are respectively arranged at the two gas pipelines to monitor and control the flow of the introduced silicon source gas and carbon source gas, and the ratio of the flow of the silicon source gas to the flow of the carbon source gas is adjusted and controlled, so that the ratio of Si in the silicon source gas to C in the carbon source gas in the reaction chamber is 1:1, and high-purity and high-quality SiC single crystals can be prepared.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the structures shown in the drawings without creative efforts.
FIG. 1 is a schematic structural view of an apparatus for controlling the growth of a silicon carbide single crystal according to an embodiment of the present invention;
FIG. 2 is a schematic structural view of an apparatus for controlling the growth of a silicon carbide single crystal according to another embodiment of the present invention.
The reference numbers illustrate:
| reference numerals | Name (R) | Reference numerals | Name (R) |
| 100 | |
200 | Silicon carbide seed crystal placing |
| 300 | |
410 | Silicon |
| 420 | Carbon |
430 | |
| 440 | |
510 | First |
| 520 | Second mass flow controller |
The implementation, functional features and advantages of the objects of the present invention will be further explained with reference to the accompanying drawings.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that, if directional indications (such as up, down, left, right, front, and back … …) are involved in the embodiment of the present invention, the directional indications are only used to explain the relative positional relationship between the components, the movement situation, and the like in a specific posture (as shown in the drawing), and if the specific posture is changed, the directional indications are changed accordingly.
In addition, if there is a description of "first", "second", etc. in an embodiment of the present invention, the description of "first", "second", etc. is for descriptive purposes only and is not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In addition, the meaning of "and/or" appearing throughout is to include three juxtapositions, exemplified by "A and/or B," including either the A or B arrangement, or both A and B satisfied arrangement. In addition, technical solutions between various embodiments may be combined with each other, but must be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention.
The embodiment of the invention provides a silicon carbide single crystal growth control device, which aims to adopt a high-temperature chemical vapor deposition method (HTCVD) and control the ratio of the flow of a silicon source gas to the flow of a carbon source gas to control the ratio of Si in the silicon source gas to C in the carbon source gas in a reaction cavity so as to prepare high-purity and high-quality SiC crystals.
In an embodiment of the present invention, as shown in fig. 1, the silicon carbide single crystal growth control apparatus includes:
the device comprises a shell 100, wherein a reaction chamber is formed in the shell 100, and a silicon carbide seed crystal placing position 200 is arranged in the reaction chamber;
a heating device 300 disposed in the housing 100 for controlling the internal temperature of the reaction chamber; and the number of the first and second groups,
a silicon source gas pipeline 410 and a carbon source gas pipeline 420 both communicated with the reaction chamber, wherein the silicon source gas pipeline 410 is used for introducing a silicon source gas into the reaction chamber, and the carbon source gas pipeline 420 is used for introducing a carbon source gas into the reaction chamber; wherein the content of the first and second substances,
silicon source gas pipeline 410 is provided with a first mass flow controller 510, carbon source gas pipeline 420 is provided with a second mass flow controller 520, first mass flow controller 510 is used for monitoring and controlling the flow of the silicon source gas, and second mass flow controller 520 is used for monitoring and controlling the flow of the carbon source gas.
It can be understood that, in this embodiment, a high temperature vapor phase transport method (HTCVD) is used to prepare the silicon carbide single crystal, specifically, a high purity silicon source gas and a carbon source gas are dried and purified to remove water vapor, and then introduced into the reaction chamber, and then under a high temperature heating condition, the two reaction gases undergo a chemical reaction to form a silicon carbide crystal, which forms a core at the seed crystal and grows continuously, and finally forms a SiC single crystal. It will be appreciated that the silicon carbide seed placement site 200 is used to place a seed crystal that is used to define the growth region of the SiC single crystal, to promote the formation of the SiC single crystal, and to impart a good crystal orientation thereto.
Specifically, the silicon source gas introduced into the silicon source gas pipeline 410 may be SiH4The carbon source gas introduced into the carbon source gas pipe 420 may be alkane (C)nH2n+2) Olefin (C)nH2n) And alkynes (C)nH2n-2) Any one of them. Wherein the alkane may be methane (CH)4) Ethane (C)2H6) Propane (C)3H8) Butane (C)4H10) Pentane (C)5H12) Hexane (C)6H14) And the like.
When methane is used as the carbon source gas, the chemical equation is as follows:
SiH4+CH4＝SiC+4H2
when propane is used as the carbon source gas, the chemical equation is as follows:
3SiH4+C3H8＝3SiC+10H2
as can be seen from the above chemical equation, since propane (C)3H8) C in (A) is methane (CH)4) And thus, when propane is used as the carbon source gas, the yield of silicon carbide is 3 times that of methane, which can greatly increase the growth rate of silicon carbide crystals. Of course, rather than using methane as the carbon source gas, ethane (C) is used2H6) Propane (C)3H8) Butane (C)4H10) Pentane (C)5H12) Hexane (C)6H14) Olefin (C)nH2n) And alkynes (C)nH2n-2) The growth rate and the yield of the silicon carbide crystal can be effectively improved.
It can be understood that the ratio of Si to C in the reaction gas should be 1:1, and that more Si than C or more C than Si than C will form many defects in the SiC crystal, affecting the quality and purity of the finally produced SiC crystal. Therefore, the quality of the produced SiC crystal can be improved by controlling the ratio of Si to C in the reaction gas.
It will be appreciated that the volume of fluid is a function of fluid temperature and pressure and is a dependent variable, whereas the mass of fluid is a quantity that does not change with changes in time, space temperature, and pressure. Therefore, in the technical solution of this embodiment, a Mass Flow Controller (Mass Flow Controller, abbreviated as MFC) is used to precisely measure and control the Mass Flow of the reaction gas.
Specifically, in the technical scheme of this embodiment, a silicon source gas pipeline 410 and a carbon source gas pipeline 420 are arranged to introduce a silicon source gas and a carbon source gas into the reaction chamber, and mass flow controllers are respectively arranged at the two gas pipelines to monitor and control the flow rates of the introduced silicon source gas and carbon source gas, so as to adjust and control the ratio of the flow rate of the silicon source gas to the flow rate of the carbon source gas, so that the ratio of Si in the silicon source gas to C in the carbon source gas in the reaction chamber is 1:1, thereby facilitating the preparation of high-purity and high-quality SiC single crystals.
Further, as shown in fig. 1, the flow directions of the silicon source gas pipeline 410 and the carbon source gas pipeline 420 are from bottom to top. Specifically, the silicon source gas pipeline 410 and the carbon source gas pipeline 420 penetrate through the bottom of the reaction chamber and extend into the reaction chamber from bottom to top, and the top ends of the silicon source gas pipeline 410 and the carbon source gas pipeline 420 are opened, so that the silicon source gas and the carbon source gas are introduced into the reaction chamber from bottom to top. Of course, in other embodiments, the silicon source gas and the carbon source gas may be introduced into the reaction chamber from other directions. However, the technical solution of the present embodiment is beneficial to the arrangement of the gas pipeline and the arrangement and routing of the mass flow controller. Specifically, the first mass flow controller 510 is installed at the bottom of the reaction chamber and is disposed corresponding to the silicon source gas pipe 410; a second mass flow controller 520 is also installed at the bottom of the reaction chamber and is disposed corresponding to the carbon source gas pipe 420.
In addition, in the embodiment, the silicon carbide seed crystal is placed on the top wall of the reaction chamber, and the temperature gradient between the SiC reaction raw material and the seed crystal is the driving force for SiC crystal growth. Therefore, the silicon source gas and the carbon source gas are introduced into the reaction chamber from bottom to top, and the heating device 300 controls the temperature gradient in the reaction chamber from bottom to top to form a decreasing temperature gradient, so that the SiC crystal is generated even if the temperature of the reaction gas is higher than the temperature of the seed crystal at the growth position when the reaction gas is initially introduced into the reaction chamber, which will be further described below.
Further, as shown in fig. 2, the silicon carbide single crystal growth control device further includes a hydrogen pipeline 430, the hydrogen pipeline 430 is communicated with the reaction chamber, and the hydrogen pipeline 430 is used for introducing hydrogen into the reaction chamber. It is understood that the silicon source gas is a relatively high-quality silicon source gas (e.g., SiH)4) And a carbon source gas (e.g. C)3H8)，H2And is lighter. The silicon source gas and the carbon source gas are easy to stay at the place just before entering the reaction chamber and pass through H2The transmission of the reaction chamber can drive the silicon source gas and the carbon source gas to move towards the deep part of the reaction chamber, so that the distribution of the reaction gas is more uniform; meanwhile, H is generated after the reaction of the silicon source gas and the carbon source gas2Thus H is2Does not produce impurities in the resulting silicon carbide crystal.
Further, as shown in fig. 2, the silicon carbide single crystal growth control device further includes a metal remover pipeline 440, the metal remover pipeline 440 is communicated with the reaction chamber, and the metal remover pipeline 440 is used for introducing metal into the reaction chamber to remove the metalAnd (4) removing gas. The metal removing gas is used for carrying out chemical reaction with metal impurities possibly existing in the silicon source gas so as to remove the metal impurities and prevent the metal impurities from influencing the quality of the silicon carbide single crystal. It will be appreciated that the silicon source gas introduced into the reaction chamber is not substantially pure, such as SiH4Metal ions (such as aluminum, lithium, magnesium, etc.) may be carried in the silane, and these metal impurities remain during the preparation of the silane. Alternatively, the metal-removing gas may be a dichloroethylene gas (C)2H2Cl2) Or hydrochloric acid gas (HCl). It should be noted that the use of HCl as the metal removal gas produces Cl2To wait for environmentally unfriendly gases, but to use C2H2Cl2CO is generated2And H2O, compared with environmental protection. Thus, the present example uses dichloroethylene (C)2H2Cl2) The gas acts as a metal remover. Specifically, dichloroethylene can chemically react with magnesium ions to generate magnesium chloride precipitate, so that the magnesium ions cannot enter the SiC single crystal along with the growth of gas reaction, thereby ensuring the high purity of the SiC single crystal. Specifically, the chemical reaction formula of dichloroethylene and magnesium ions is as follows:
C2H2Cl2+Mg+→MgCl2↓
optionally, a silicon carbide seed placement site 200 is provided at the center of the top wall of the reaction chamber. It can be understood that in the process of introducing the silicon source gas and the carbon source gas into the reaction chamber from bottom to top, the silicon carbide seed crystal is placed at the top of the reaction chamber, so that the descending temperature gradient is formed in the reaction chamber from bottom to top, and even if the temperature of the reaction gas entering the reaction chamber for the first time is higher than that of the seed crystal, the generation of the SiC crystal is facilitated. Further, the silicon carbide seed crystal is placed at the center of the top wall of the reaction chamber such that the distances between the silicon source gas and the carbon source gas reaching the silicon carbide seed crystal are uniform, thereby facilitating uniform growth of the silicon carbide single crystal.
In this embodiment, the heating device 300 is a heating coil, and the heating coil is wound around the peripheral wall of the reaction chamber. It can be understood that the circumferential sidewall of the reaction chamber is heated by the heating coil to provide high temperature reaction conditions for the reaction gas in the reaction chamber. The heating coil has the characteristics of softness and slender shape, is easy to wind on the peripheral side wall of the reaction chamber, and occupies small space, thereby being beneficial to reducing the whole volume of the silicon carbide single crystal growth control device; in addition, the heating temperature of the heating coil is easy to control, so that the temperature in the reaction chamber is convenient to control.
Further, the heating coil comprises a plurality of sub-coils which are arranged side by side from bottom to top, and the heating temperature of the plurality of sub-coils is decreased progressively from bottom to top. Specifically, the heating temperatures of different sub-coils can be made different by setting the wires of the sub-coils to different thicknesses. From the above analysis, it can be known that the temperature gradient between the SiC reaction raw material and the seed crystal is the driving force for SiC crystal growth, and in this embodiment, the heating coil controls the decreasing temperature gradient formed from bottom to top in the reaction chamber, so that even if the temperature of the reaction gas when initially entering the reaction chamber is higher than the temperature at the growth position of the seed crystal, the SiC crystal is favorably generated. Specifically, the temperature range of the silicon source gas and the carbon source gas entering the reaction chamber is controlled to be 2300-2800 ℃, and the temperature range of the silicon carbide seed crystal placement position 200 is controlled to be 1800-2200 ℃. In addition, preferably, the temperature gradient is set to be between 5 and 20K/cm, and the higher the temperature gradient is, the higher the supersaturation degree of the gaseous phase substance reaching the surface of the seed crystal is, and the faster the growth rate of the SiC crystal is. However, if the temperature gradient is too high, the crystal growth speed is too high (for example, the speed in the crystal growth direction reaches more than 0.5 mm/h), and the SiC crystal is very easy to generate a heterogeneous crystal form, so that the SiC crystal growth process fails.
The embodiment of the invention also provides a silicon carbide single crystal growth control method, which comprises the following steps:
placing the silicon carbide seed crystal in a silicon carbide seed crystal placing position in the reaction chamber;
controlling the internal temperature of the reaction chamber by a heating device;
introducing silicon source gas into the reaction chamber through a silicon source gas pipeline;
introducing a carbon source gas into the reaction chamber through a carbon source gas pipeline; and the number of the first and second groups,
a first mass flow controller at the silicon source gas line and a second mass flow controller at the carbon source gas line are adjusted to control the ratio of the silicon source gas flow to the carbon source gas flow.
It can be understood that, in the technical scheme of this embodiment, a silicon source gas is introduced into the reaction chamber through the silicon source gas pipeline, a carbon source gas is introduced into the reaction chamber through the carbon source gas pipeline, and the flow rates of the introduced silicon source gas and the introduced carbon source gas are monitored and controlled by the mass flow controller, so as to adjust and control the ratio of the flow rate of the silicon source gas to the flow rate of the carbon source gas, so that the ratio of Si in the silicon source gas to C in the carbon source gas in the reaction chamber is 1:1, thereby being beneficial to preparing high-purity and high-quality SiC single crystals.
Further, hydrogen is introduced into the reaction chamber through a hydrogen pipeline. Gaseous and carbon source gas of silicon source stops easily in the place of just going into after getting into reaction chamber, and this embodiment is favorable to driving gaseous and carbon source gas of silicon source and walk toward reaction chamber depths through letting in the hydrogen that the quality is lighter in to reaction chamber for reactant gas's distribution is more even.
Further, dichloroethylene gas is introduced into the reaction chamber through a metal remover pipeline. This example was prepared by reacting dichloroethylene (C)2H2Cl2) The gas is used as a metal remover to chemically react with magnesium ions which are possibly present in the silicon source gas to remove metal impurities, so that the quality and the purity of the generated silicon carbide single crystal are improved.
Wherein the step of controlling the internal temperature of the reaction chamber by the heating device specifically comprises the steps of:
controlling the heating temperature of the heating coil to be decreased from bottom to top;
controlling the temperature range of the silicon source gas and the carbon source gas to be 2300-2800 ℃ when the silicon source gas and the carbon source gas enter the reaction chamber; and the number of the first and second groups,
controlling the temperature range of the silicon carbide seed crystal placement position to be 1800-2200 ℃.
In the embodiment, the heating coil controls the descending temperature gradient formed in the reaction chamber from bottom to top so as to drive the SiC crystal to grow. It should be noted that, besides the temperature at the seed crystal needs to be controlled to be lower than the temperature when the gas enters the reaction chamber initially, the reaction chamber needs to be controlled to be in a low-pressure state, specifically, the pressure in the reaction chamber is 0.2 to 0.7Pa, and the high temperature and the low pressure are matched to ensure that the reaction gas is in a gaseous state, and the solid matter formed by the chemical reaction starts to deposit through the seed crystal.
Further, in the step of introducing a silicon source gas into the reaction chamber through a silicon source gas pipeline, the silicon source gas is SiH4；
In the step of introducing the carbon source gas into the reaction chamber through the carbon source gas pipeline, the carbon source gas is any one of alkane, alkene and alkyne. For the specific carbon source gas types, please refer to the above, and further description is omitted.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, and all modifications and equivalents of the present invention, which are made by the contents of the present specification and the accompanying drawings, or directly/indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (10)
1. An apparatus for controlling the growth of a silicon carbide single crystal, comprising:
the device comprises a shell, a reaction cavity is formed in the shell, and a silicon carbide seed crystal placing position is arranged in the reaction cavity;
the heating device is arranged on the shell and used for controlling the internal temperature of the reaction chamber; and the number of the first and second groups,
the silicon source gas pipeline is used for introducing silicon source gas into the reaction cavity, and the carbon source gas pipeline is used for introducing carbon source gas into the reaction cavity; wherein the content of the first and second substances,
the silicon source gas pipeline is provided with a first mass flow controller, the carbon source gas pipeline is provided with a second mass flow controller, the first mass flow controller is used for monitoring and controlling the flow of the silicon source gas, and the second mass flow controller is used for monitoring and controlling the flow of the carbon source gas.
2. A silicon carbide single crystal growth control apparatus as claimed in claim 1, wherein the flow direction of said silicon source gas conduit and said carbon source gas conduit are from bottom to top.
3. A silicon carbide single crystal growth control device according to claim 2, further comprising a hydrogen gas pipe communicating with the reaction chamber, the hydrogen gas pipe being for introducing hydrogen gas into the reaction chamber; and/or the silicon carbide single crystal growth control device further comprises a metal remover pipeline, the metal remover pipeline is communicated with the reaction chamber, and the metal remover pipeline is used for introducing metal removing gas into the reaction chamber.
4. A silicon carbide single crystal growth control apparatus as set forth in claim 2 wherein said silicon carbide seed crystal placement location is provided at the center of the top wall of said reaction chamber.
5. A silicon carbide single crystal growth control apparatus as set forth in claim 2 wherein said heating means is a heating coil disposed so as to be wound around a peripheral side wall of said reaction chamber.
6. A silicon carbide single crystal growth control apparatus as set forth in claim 5, wherein said heating coil comprises a plurality of sub-coils arranged side by side from bottom to top, the heat generation temperature of said plurality of sub-coils being decreased from bottom to top.
7. A silicon carbide single crystal growth control method, characterized by comprising the steps of:
placing the silicon carbide seed crystal in a silicon carbide seed crystal placing position in the reaction chamber;
controlling the internal temperature of the reaction chamber by a heating device;
introducing silicon source gas into the reaction chamber through a silicon source gas pipeline;
introducing a carbon source gas into the reaction chamber through a carbon source gas pipeline; and the number of the first and second groups,
a first mass flow controller at the silicon source gas line and a second mass flow controller at the carbon source gas line are adjusted to control the ratio of the silicon source gas flow to the carbon source gas flow.
8. A silicon carbide single crystal growth control method according to claim 7, further comprising the step of:
introducing hydrogen into the reaction chamber through a hydrogen pipeline; and/or introducing dichloroethylene gas into the reaction chamber through a metal remover pipeline.
9. A silicon carbide single crystal growth control method according to claim 8, wherein the silicon source gas pipe and the carbon source gas pipe are arranged in a gas flow direction from bottom to top, the heating device is a heating coil wound around a peripheral side wall of the reaction chamber, and the step of controlling the internal temperature of the reaction chamber by the heating device specifically comprises the steps of:
controlling the heating temperature of the heating coil to be decreased from bottom to top;
controlling the temperature range of the silicon source gas and the carbon source gas to be 2300-2800 ℃ when the silicon source gas and the carbon source gas enter the reaction chamber; and the number of the first and second groups,
controlling the temperature range of the silicon carbide seed crystal placement position to be 1800-2200 ℃.
10. The method for controlling growth of a silicon carbide single crystal as claimed in claim 7, wherein in the step of introducing a silicon source gas into the reaction chamber through a silicon source gas line, the silicon source gas is SiH4；
In the step of introducing the carbon source gas into the reaction chamber through the carbon source gas pipeline, the carbon source gas is any one of alkane, alkene and alkyne.
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