CN213866495U - Device for producing silicon carbide single crystal by PVT method - Google Patents
Device for producing silicon carbide single crystal by PVT method Download PDFInfo
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Abstract
The application discloses a device for producing silicon carbide single crystals by a PVT method. The device includes long brilliant crucible of carborundum and heating device, the long brilliant crucible periphery of carborundum establishes heat radiation reflection device, heat radiation reflection device can with the heat reflection that gives out is located to the crucible returns crucible department. The device of the utility model can reduce the power used by the crystal growth of the silicon carbide, save the electric energy and the crystal growth cost, and simultaneously can reduce the defects of crystal polytype or microtubule and the like of the silicon carbide crystal, and improve the yield; in addition, the heat is mainly reflected to the crucible after the heat radiation reflection device is used, the heat conducted outwards is little, the outside of the device for producing the silicon carbide single crystal by the PVT method does not need to be cooled, the cooling mode of circulating water or air inlets and air outlets outside the crystal growth device is replaced, and the fluctuation probability of crystal growth conditions is reduced.
Description
Technical Field
The utility model relates to a carborundum single crystal production technology field, concretely relates to device of carborundum single crystal of PVT method production.
Background
Silicon carbide is one of the third generation wide bandgap semiconductor materials following silicon and gallium arsenide, and is widely applied to the fields of power electronics, radio frequency devices, photoelectronic devices and the like because of its excellent properties such as large forbidden bandwidth, high saturated electron mobility, strong breakdown field, high thermal conductivity and the like. High quality crystals are the cornerstone of semiconductor and information industry development, and the level of their fabrication limits the fabrication and performance of downstream devices. Although Physical Vapor Transport (PVT) growth of silicon carbide crystals has advanced sufficiently in recent years, the stability of the grown crystals needs to be further studied, for example, the crystal growth process is influenced by the fluctuation of the temperature of circulating water, and the power consumption of the silicon carbide crystal growth process is too large.
At present, the cooling mode outside the furnace chamber of the crystal growing furnace for growing the silicon carbide crystal mainly comprises two modes: the two methods are limited by the control of the temperature of circulating water, if the temperature of the circulating water fluctuates, the crystal growth condition fluctuates, the final result causes the fluctuation of the crystal growth condition to influence the crystal growth stability, the defects of polytype, microtubule and the like of the crystal are caused, and the yield is influenced.
SUMMERY OF THE UTILITY MODEL
Aiming at the defects in the prior art, the utility model aims to provide a device for producing silicon carbide single crystal by PVT method.
The utility model provides a device for producing silicon carbide single crystal by PVT method, which comprises a silicon carbide crystal growth crucible (such as a graphite crucible) and a heating device,
the periphery (such as the side periphery, and/or the upper part, and/or the lower part) of the silicon carbide crystal growth crucible is provided with a heat radiation reflecting device which can reflect the heat emitted from the crucible back to the crucible,
the heating device is positioned outside the heat radiation reflection device and can heat the crystal growth crucible.
In the device for producing the silicon carbide single crystal by the PVT method, at least the inner side wall of the heat radiation reflection device facing to the side wall of the crucible is a heat radiation reflection mirror surface, and the heat radiation reflection mirror surface can reflect the heat emitted from the crucible back to the crucible;
a vacuum isolation cover is arranged outside the crucible, and the heat radiation reflection device is arranged in the vacuum isolation cover.
In the apparatus for producing a silicon carbide single crystal by the PVT method described above, the thermal radiation reflecting means includes a specific material layer provided on an inner surface of the vacuum insulation cover; or
The heat radiation reflection device comprises a support and a specific material layer arranged on one side of the support, and the melting point of the support and the melting point of the specific material are both higher than the highest temperature at the position of the specific material; the highest temperature refers to the corresponding temperature when the silicon carbide single crystal is produced by a PVT method;
the material of the support and the specific material can be the same (for example, the material of the support is a metal, one side of the support can be used as a heat radiation reflecting mirror), or can be different (for example, a metal coating is arranged on the surface of quartz glass);
wherein the thermal radiation reflecting mirror surface is an outer surface of the specific material layer, and/or,
the heat radiation reflecting mirror surface is an interface between the support and the specific material layer, and the support is made of a transparent material, preferably, quartz glass.
In the above apparatus for producing a silicon carbide single crystal by the PVT method, the specific material is a metal, a silicon compound, a boride, a carbide or a nitride;
the metal includes: tantalum, tungsten, molybdenum, iridium, niobium, germanium, hafnium, or alloys thereof, more preferably, tantalum;
the boride comprises: boron carbide, boron nitride, zirconium boride, lanthanum boride, titanium boride, tantalum boride, chromium boride, tungsten boride, molybdenum boride, vanadium boride, or niobium boride;
the carbide includes: chromium carbide, tantalum carbide, vanadium carbide, zirconium carbide, tungsten carbide, molybdenum carbide, titanium carbide, or niobium carbide;
the nitride includes: titanium nitride, tungsten nitride, molybdenum nitride, chromium nitride, niobium nitride, zirconium nitride, tantalum nitride, or vanadium nitride.
In the apparatus for producing a silicon carbide single crystal by the above PVT method, the specific material is tantalum or tantalum carbide, and the thickness of the specific material layer is 3 μm or more, or 4 to 100 μm, more preferably, 5 to 60 μm, more preferably, 10 to 40 μm, more preferably, 15 to 35 μm;
in the above apparatus for producing a silicon carbide single crystal by the PVT method, the roughness of the heat radiation reflecting mirror surface is less than 25 μm; preferably, the roughness of the heat radiation reflecting mirror surface is less than 15 μm.
The thickness of the specific material layer can be determined according to actual conditions and requirements such as different components of the specific material, different distances between the specific material layer and the outer wall of the crucible, energy consumption requirements and the like;
the smaller the thickness of the specific material layer is, the weaker the heat reflection effect is, and the lower the cost is;
the greater the thickness of the specific material layer, the stronger the effect of reflecting heat, but the higher the cost;
the larger the distance between the specific material layer and the crucible is, the weaker the effect of reflecting heat is, and the stronger the effect is otherwise;
the test results of the embodiment of the application show that when the thickness of Ta is less than 5 μm, the Ta is not compact enough, the crystal quality can only be improved but the energy consumption can not be obviously reduced, but when the thickness of Ta is 15-35 μm or more, the Ta can not only improve the crystal quality but also obviously reduce the energy consumption.
In specific implementation, the melting point of the specific material may be greater than or equal to the melting point of the material of the inner side wall of the vacuum isolation cover, and the specific material is inactive and does not introduce impurities into the silicon carbide single crystal.
Generally, the device for producing silicon carbide single crystal by the PVT method, such as a crystal growth furnace, is a vacuum cavity body made of a quartz tube, and the temperature which the specific material needs to bear is at least equal to or higher than the melting point (1750 ℃) of the quartz tube, so that the safe production can be ensured.
In the device for producing the silicon carbide single crystal by the PVT method, the vacuum isolation cover is made of quartz.
The method for plating the specific material layer on the inner surface or the outer surface of the vacuum isolation cover is not limited to the vacuum plating method such as PVD (physical vapor deposition), CVD (chemical vapor deposition) and the like,
the PVD comprises vacuum evaporation, sputtering coating, arc plasma coating, ion coating and molecular beam epitaxy; the CVD comprises atmospheric pressure chemical vapor deposition, low pressure chemical vapor deposition and plasma chemical vapor deposition which has the characteristics of both CVD and PVD;
the embodiment of the application is specifically sputtering coating.
In the apparatus for producing silicon carbide single crystal by the PVT method, the apparatus for producing silicon carbide single crystal by the PVT method includes a heat insulating structure, and the heat insulating structure is located outside the crucible and inside the heat radiation reflecting device.
In the apparatus for producing a silicon carbide single crystal by the PVT method described above, the apparatus for producing a silicon carbide single crystal by the PVT method includes a temperature monitoring device capable of monitoring the temperature inside the crucible.
In the apparatus for producing silicon carbide single crystal by the PVT method, the apparatus for producing silicon carbide single crystal by the PVT method may or may not include a cooling apparatus for cooling the outside of the apparatus for producing silicon carbide single crystal by the PVT method, and the cooling apparatus may be a circulating water cooling apparatus or an air cooling apparatus.
The utility model has the advantages as follows:
the PVT method silicon carbide single crystal production device provided by the utility model has the advantages that the design is ingenious and reasonable, the heat radiation reflection device can reflect the heat radiated from the interior of the crystal growth crucible back to the interior of the crucible, the power used by crystal growth is reduced, the electric energy and the crystal growth cost are saved, meanwhile, the defects of crystal polytype or microtubule and the like of the silicon carbide crystal can be reduced, and the yield is improved; in addition, the heat is mainly reflected to the crucible after the heat radiation reflection device is used, the heat conducted outwards is little, the outside of the device for producing the silicon carbide single crystal by the PVT method does not need to be cooled, the cooling mode of circulating water or air inlets and air outlets outside the crystal growth device is replaced, and the fluctuation probability of crystal growth conditions is reduced.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the application and together with the description serve to explain the application and not to limit the application. In the drawings:
FIG. 1 is a schematic view showing the structure of an apparatus for producing a silicon carbide single crystal by a PVT method.
Fig. 2 is an enlarged view and a schematic diagram of a portion of the structure of fig. 1 in a dashed frame.
The reference numerals in the figures are as follows:
the device comprises a crystal growth crucible 1, a temperature monitoring device 2, a vacuum isolation cover 3, a heat insulation structure 4, a heating device 5, a heat radiation reflection device 6, a seed crystal 7, a raw material 8 and a vacuum system 9.
Detailed Description
EXAMPLE 1 apparatus for producing silicon carbide single crystal by PVT method
As shown in fig. 1, the apparatus for producing a silicon carbide single crystal by the PVT method according to the present embodiment includes: the device comprises a silicon carbide crystal growth crucible 1, a temperature monitoring device 2, a vacuum isolation cover 3, a heat preservation structure 4, a heating device 5 and a vacuum system 9;
the temperature monitoring device 2 can monitor the internal temperature of the crucible 1 (graphite crucible), and comprises a pyrometer arranged above the crucible 1;
the vacuum isolation cover 3 is arranged on the periphery (comprising a side wall, a top and/or a bottom) of the crystal growth crucible 1, the heat radiation reflection device 6 is arranged on the inner side of the vacuum isolation cover 3, the heat radiation reflection device 6 comprises a metal coating, a heat radiation reflection mirror surface can be formed on the outer surface of the metal coating, and the metal coating is made of tantalum (Ta);
the vacuum system 9 is arranged above the vacuum isolation cover 3, can vacuumize the growth cavity in the crucible 1 and detect the vacuum degree, and specifically can comprise a mechanical pump, a molecular pump and a vacuum degree measuring device.
As shown in fig. 2, the heat radiation reflecting means 6 is coated on the inner sidewall of the vacuum insulation cover 3 by a vacuum coating method; the vacuum isolation cover 3 is made of quartz, and the vacuum isolation cover 3 is a single layer;
the heat insulation structure 4 is positioned outside the crucible 1 and in the heat radiation reflecting mirror surface;
the heating device 5 is specifically a heating coil, and can heat the inside of the crystal growth crucible 1;
the device for producing the silicon carbide single crystal by the PVT method does not comprise a cooling device or comprises the cooling device, but the cooling function of the cooling device is closed;
the crystal growth crucible 1 is cylindrical, the vacuum isolation cover 3 is cylindrical, and the two are coaxial, so that the outer part and/or the inner part of the crucible can be uniformly heated.
The device for producing the silicon carbide single crystal by the PVT method comprises the following using method: the silicon carbide single crystal production according to the conventional PVT method is carried out, the seed crystal 7 is arranged above the inside of the crystal growth crucible 1, and the raw material 8 is arranged below the inside of the crystal growth crucible 1, and the operation of the device is different from that of other devices in that the temperature in the crystal growth crucible 1 needs to be monitored so as to adjust the power of the heating device 5 in time.
The preparation method (PVD-sputter coating) of the metal coating of the heat radiation reflecting device 6 is as follows:
background vacuum degree of shooting chamber is 1.0 x 10-4～9.9×10-4Pa or 1.0X 10-5～9.9×10-5Pa, introducing 99.99 percent purity argon into the film coating chamber for 0.5 to 1 hour before sputtering, and maintaining the pressure at 0.1 to 1.5 Pa; the pressure of high-purity argon with the purity of 99.99% is 0.2-2.7 Pa during sputtering, a vacuum isolation cover 3 (namely a quartz tube) is firstly cleaned by acetone and then by deionized water, a high-purity Ta target with the purity of 99.999% is adopted for sputtering, the sputtering power is 50W, the sputtering is carried out for 2-3 hours, a metal coating is obtained, and the thickness of the metal coating is measured by a step instrument method or an XRT method.
As a result: the compact surface of the plating layer is a smooth mirror surface, and the roughness of the mirror surface is less than 25 mu m.
Secondly, in the device for producing silicon carbide single crystal by the PVT method described in the first paragraph:
1) in another embodiment, the heat radiation reflecting device 6 further includes a support, a metal coating with a high melting point, such as a Ta coating, is attached to an outer wall of the support made of quartz, and a heat radiation reflecting mirror surface is formed at an interface between the support made of quartz and the Ta coating;
2) in another embodiment, the vacuum isolation cover 3 may also be a double layer, and the middle part of the double layer is a vacuum layer;
3) in another embodiment, the crystal growth crucible 1 is spherical, and the vacuum isolation cover 3 is spherical, and the two are concentric, so that the outer part and/or the inner part of the crystal growth crucible 1 can be heated uniformly.
EXAMPLE 2 production of silicon carbide Single Crystal by PVT method
The method comprises the following steps: silicon carbide single crystal (crystal form 4H) was produced according to the conventional PVT method using the apparatus of "one" in example 1, wherein the thickness of the metal plating layer was set to different values.
The specific process for producing the silicon carbide single crystal by the PVT method comprises the following steps:
1) putting silicon carbide powder as a raw material 8 into a crucible 1; putting the seed crystal 7 into the inner top of the crucible 1, and sealing the crucible 1;
2) the crucible 1 is evacuated to an atmospheric pressure of 10-6Below mbar, introducing inert gas to 400mbar, repeating the process for 2-3 times, and finally pumping the gas pressure in the crucible 1 to 10-6mbar or more;
3) slowly raising the temperature in the crucible 1 to 1000 ℃, introducing inert gas into the crucible to raise the gas pressure to 700mbar, and keeping the gas pressure for 8 hours;
4) reducing the pressure in the crucible 1 to a single crystal growth pressure of 30mbar, and raising the temperature in the crucible 1 to 2200 ℃ for 150 hours under the condition of keeping the pressure in the crucible 1 unchanged;
6) after the growth of the single crystal is finished, the temperature and the pressure in the crucible 1 are reduced to room temperature and room pressure, the crucible 1 is opened, and the silicon carbide single crystal is taken out.
As a result: the medium frequency power usage during the growth of the silicon carbide single crystal and the crystal was examined as shown in table 1. The quartz tube in table 1 is a vacuum isolation cover 3, the vacuum isolation cover 3 enables the crucible 1 to be performed in a sealed environment, and the specific metal coating of the thermal radiation reflection device 6 is a Ta coating.
TABLE 1 results of experiments on the production of silicon carbide single crystal by PVT method using the apparatus of example 1
The results in Table 1 show that when the thickness of the coating Ta is less than 5 μm, the coating is not dense enough, the quality of the silicon carbide crystal cannot be improved obviously, and the energy consumption cannot be reduced obviously, and when the thickness of the coating Ta is 5-35 μm or more, the crystal quality can be improved obviously, and the energy consumption can be reduced obviously.
EXAMPLE 3 production of silicon carbide Single Crystal by PVT method
The method comprises the following steps: silicon carbide single crystal (crystal form 4H) was produced according to the conventional PVT method using the apparatus of "two" in "1" in example 1, wherein the thickness of the metal plating layer was set to different values.
The specific process for producing a silicon carbide single crystal by the above-described PVT method is exactly the same as in example 2.
As a result: the medium frequency power usage during the growth of the silicon carbide single crystal and the crystal was examined as shown in table 2.
TABLE 2 results of experiments on the production of silicon carbide single crystal by PVT method using another apparatus of example 1
The results in tables 1 and 2 show that the coating Ta on the inner or outer wall of the support does not differ significantly from the values of the parameters examined in the table. I.e. the result of the coating Ta being provided inside or outside the quartz tube is not very different.
EXAMPLE 4 production of silicon carbide Single Crystal by PVT method
The method comprises the following steps: the procedure of example 2 was followed except that: the vacuum isolation cover 3, namely the quartz tube is internally provided with a tantalum carbide (TaC) coating.
As a result: the medium frequency power usage during the growth of the silicon carbide single crystal and the crystal was examined as shown in table 3.
TABLE 3 Experimental results of the PVT method for producing silicon carbide single crystal
Comparative example 1 production of silicon carbide Single Crystal by PVT method-Using existing apparatus
The method comprises the following steps: the procedure of example 2 was followed except that: the apparatus for producing silicon carbide single crystal by PVT method used was the apparatus of "one" in example 1, in which the inner surface of the quartz vacuum insulated housing 3 (i.e., quartz tube) was not coated with metal and different types of circulating water cooling apparatus were provided (see table 4).
As a result: the medium frequency power usage during the growth of the silicon carbide single crystal and the crystal was examined as shown in table 4.
TABLE 4 Crystal growth by circulating Water
The results of examples 2-4 and comparative example 1 show that compared with cooling with circulating water, the crystal growth device of examples 2-4 has the advantages of obviously improving the crystal growth stability, effectively controlling the crystal polytype defects, reducing the micropipe density, obviously improving the crystallization quality, obviously reducing the consumption of electric energy during crystal growth and reducing the cost.
Those not described in detail in this specification are within the skill of the art. The above description is only an example of the present application and is not intended to limit the present application. Various modifications and changes may occur to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the scope of the claims of the present application.
Claims (9)
1. An apparatus for producing a silicon carbide single crystal by a PVT method, which is characterized by comprising a silicon carbide crystal growth crucible and a heating device,
the periphery of the silicon carbide crystal growth crucible is provided with a heat radiation reflecting device which can reflect the heat emitted from the crucible back to the crucible,
the heating device is positioned outside the heat radiation reflection device and can heat the crystal growth crucible.
2. The apparatus according to claim 1, wherein at least an inner side wall of the thermal radiation reflecting means facing the crucible side wall is a thermal radiation reflecting mirror surface capable of reflecting heat emitted at the crucible back to the crucible;
a vacuum isolation cover is arranged outside the crucible, and the heat radiation reflection device is arranged in the vacuum isolation cover.
3. The apparatus of claim 2, wherein said thermal radiation reflecting means comprises a layer of a specified material, said specified material in said layer of specified material being a metal, a silicon compound, a boride, a carbide or a nitride, said layer of specified material being disposed on said vacuum insulation cover inner surface; or
The heat radiation reflection device comprises a support and a specific material layer arranged on one side of the support, and the melting point of the support and the melting point of the specific material are higher than the highest temperature of the support and the specific material at the positions of the support and the specific material; wherein,
the thermal radiation reflecting mirror surface is an outer surface of the specific material layer, and/or,
the heat radiation reflecting mirror surface is an interface between the support and the specific material layer, and the support is made of a transparent material.
4. The apparatus according to claim 3, wherein the specific material is tantalum or tantalum carbide, and the thickness of the specific material layer is 5 to 60 μm.
5. The apparatus according to claim 4, wherein the roughness of the thermal radiation reflecting mirror surface is less than 25 μm.
6. The apparatus of claim 3, wherein the vacuum isolation enclosure is made of quartz.
7. The apparatus according to any one of claims 1 to 6, wherein the apparatus for producing a silicon carbide single crystal by the PVT method comprises a heat retaining structure which is located outside the crucible and inside the heat radiation reflecting means.
8. The apparatus according to any one of claims 1 to 6, wherein the apparatus for producing a silicon carbide single crystal by the PVT method comprises a temperature monitoring device capable of monitoring the temperature inside the crucible.
9. The apparatus according to any one of claims 1 to 6, wherein the apparatus for producing a silicon carbide single crystal by the PVT method comprises or does not comprise a cooling device for cooling the outside of the apparatus for producing a silicon carbide single crystal by the PVT method.
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