CN111892055A - Silicon carbide powder doped with rare earth elements and preparation method thereof - Google Patents
Silicon carbide powder doped with rare earth elements and preparation method thereof Download PDFInfo
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Abstract
The application discloses a preparation method of rare earth element doped silicon carbide powder, which comprises the following steps: (1) carrying out high-temperature reaction on a rare earth element-containing substance and high-purity silicon powder to obtain a rare earth element silicide; (2) carrying out synthetic reaction on the silicide of the rare earth element, high-purity silicon powder and high-purity carbon powder to obtain high-purity silicon carbide powder doped with the rare earth element; the rare earth element is at least one of cerium, lanthanum, praseodymium, neodymium, scandium and yttrium. According to the method, the silicon carbide powder doped with the rare earth element is obtained by using the substance containing the rare earth element, part of the rare earth element is coated on the surface of the silicon carbide powder, and part of the rare earth element enters the crystal lattice of the silicon carbide powder, so that the distribution uniformity of the rare earth element in the silicon carbide powder is improved; the preparation method is simple, the conditions are easy to control, and the prepared silicon carbide powder doped with the rare earth elements is uniform in rare earth element doping and high in purity.
Description
Technical Field
The application relates to a silicon carbide powder doped with rare earth elements and a preparation method thereof, belonging to the technical field of semiconductor materials.
Background
Silicon carbide (SiC) is widely used in the fields of power electronics, photoelectronic devices, and the like as a third-generation semiconductor material 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.
At present, the Physical Vapor Transport (PVT) method is the main method for growing silicon carbide crystals, and the equipment used for growing the silicon carbide crystals by the physical vapor transport method is simple and the process is easy to control. However, during the growth of silicon carbide crystals by the PVT method, defects such as dislocations and polytype occur. In the prior art, in order to inhibit the generation of polytype in the growth of the silicon carbide crystal, an auxiliary agent is often added in the crystal growth process. The method currently known and widely used in the industry is the doping of lanthanide compounds, the most common of which is the cerium (Ce) compound.
Patent US20090053125a1 discloses that addition of a silicide or carbide of Ce during growth of a 4H-SiC single crystal can suppress generation of polytype defects. In this patent, CeSi2Or CeC2Is placed in a small graphite crucible to be dispersedly buried in a SiC powder source, is sublimated into a gas phase during crystal growth, and is finally doped into silicon carbide crystal lattices, thereby promoting the growth of 4H-SiC and suppressing the generation of other polytypes. From the process perspective: the cerium silicide or carbide is placed in a small graphite crucible and then embedded into a powder source, and the cerium compound cannot be uniformly distributed in the powder, so that the nonuniformity of the distribution of cerium in a gas-phase component in time and space in the whole crystal growth process is inevitably caused, and the inhibition of the crystal form is also unfavorable. Similarly, the dopant is simply stirred and mixed with the silicon carbide powder, and the dopant does not enter the powder, so even if the dopant is uniformly distributed in space, the phenomenon of nonuniform distribution still exists in time in the whole crystal growth process due to the difference between the melting point, sublimation speed and the like of the cerium silicide or carbide and the silicon carbide. The introduction of small graphite crucibles amounts to the introduction of new variables for long crystal systems. For the growth process of the high-purity silicon carbide single crystal, the variable for controlling the purity is increased, the process becomes more complex, and the inhibition effect on polytype in the growth process of the silicon carbide crystal is not ideal.
Disclosure of Invention
In order to solve the problems, the application provides a silicon carbide powder doped with rare earth elements and a preparation method thereof. The method comprises the steps of firstly preparing rare earth element silicide by using a rare earth element-containing substance, and then synthesizing the rare earth element silicide and high-purity silicon carbon powder to ensure that the rare earth element is uniformly doped with silicon carbide powder; the rare earth element in the silicon carbide powder is gradually released along with the sublimation of the powder in the growth process by utilizing the rare earth element doped silicon carbide powder to grow crystals, so that the generation of polytype can be effectively inhibited.
According to one aspect of the present application, there is provided a method for preparing a rare earth element-doped silicon carbide powder, the method comprising the steps of:
(1) carrying out high-temperature reaction on a rare earth element-containing substance and high-purity silicon powder to obtain a rare earth element silicide;
(2) carrying out synthetic reaction on the silicide of the rare earth element in the step (1), high-purity silicon powder and high-purity carbon powder to obtain high-purity silicon carbide powder doped with the rare earth element;
according to the preparation method, firstly, a rare earth element-containing substance and high-purity silicon powder are subjected to high-temperature reaction to obtain a rare earth element silicide; and the silicide of the rare earth element reacts with high-purity silicon powder and high-purity carbon powder, firstly the high-purity carbon powder reacts with the high-purity carbon powder to generate silicon carbide, and then the silicide of the rare earth element is doped and wrapped in silicon carbide crystal grains. When the rare earth element-doped silicon carbide powder is used for growing crystals, the melting point of the silicide of the rare earth element is about 1600 ℃, and the silicide of the rare earth element can volatilize when the silicon carbide is sublimated, so that the doping of the rare earth element in time and space is realized, and the crystal growth process can be ensured to effectively inhibit multiple types from beginning to end.
Further, the rare earth element is selected from at least one of lanthanoid, scandium, and yttrium; preferably, the rare earth element is selected from at least one of cerium, lanthanum, praseodymium, neodymium, scandium, and yttrium. More preferably, the rare earth element is cerium.
Further, the purity of the rare earth element-containing substance is not less than 99.99%, preferably, the purity of the rare earth element-containing substance is not less than 99.999%, and the rare earth element-containing substance is solid powder with the particle size of not more than 100 μm.
Further, in the step (1), the molar ratio of the rare earth elements in the rare earth element-containing substance to the high-purity silicon powder is 1: 2-4; preferably, the molar ratio of the rare earth elements in the rare earth element-containing substance to the high-purity silicon powder is 1: 2-3. Preferably, the rare earth element-containing substance is a rare earth element simple substance and/or a rare earth element oxide; preferably, the rare earth element-containing substance is a rare earth element oxide.
Further, in the step (1), the high-temperature reaction conditions are as follows: reacting a rare earth element-containing substance with high-purity silicon powder for 1-5 hours at the temperature of 1400-1800 ℃ under a vacuum condition; preferably, the conditions of the high temperature reaction are: mixing the rare earth element-containing substance with high-purity silicon powder under the condition that the pressure is not higher than 10-2Pa, the temperature is 1500-1600 ℃, and the reaction lasts for 2-4 h.
Further, in the step (2), the mass ratio of the sum of the mass of the high-purity carbon powder and the high-purity silicon powder to the mass of the rare earth element silicide is 100: 0.001-5; preferably, the mass ratio of the sum of the mass of the high-purity carbon powder and the high-purity silicon powder to the mass of the rare earth element silicide is 100: 0.005-2.5.
Further, in the step (2), the molar ratio of the high-purity carbon powder to the high-purity silicon powder is 1-1.5: 1; preferably, the purities of the high-purity carbon powder and the high-purity silicon powder are not less than 99.99%, and the particle sizes of the high-purity carbon powder and the high-purity silicon powder are not more than 100 microns.
Further, in the step (2), the conditions of the synthesis reaction comprise the following steps: firstly, reacting the rare earth element silicide, the high-purity silicon powder and the high-purity carbon powder in the step (1) for at least 5 hours at the temperature of 1100-1600 ℃ under the vacuum condition to obtain rare earth element-doped beta-type silicon carbide powder; preferably, the synthesis reaction further comprises the steps of: firstly, the silicide of the rare earth element in the step (1), the high-purity silicon powder and the high-purity carbon powder are pressed at the pressure of not higher than 10-2Pa, the temperature is 1200-1400 ℃, and the reaction is carried out for 5-15 h, so as to obtain the beta-type silicon carbide powder doped with the rare earth element.
Further, in the step (2), the synthesis reaction conditions further include the following steps: secondly, introducing protective gas at the temperature of the first step, raising the temperature to 2000-2500 ℃, and reacting for at least 10 hours to obtain rare earth element doped alpha-type silicon carbide powder; preferably, the synthesis reaction conditions further comprise the steps of: secondly, introducing protective gas to the temperature of the first step until the pressure is 500-1000 mbar, raising the temperature to 2200-2400 ℃, and reacting for 10-40 hours to obtain rare earth element doped alpha-type silicon carbide powder; preferably, the protective gas is a mixed gas of inert gas and hydrogen, and the volume fraction of the hydrogen in the mixed gas is 2-3%; the hydrogen is mainly used for inhibiting the carbonization of the silicon carbide powder and homogenizing the atmosphere distribution in the crucible.
According to another aspect of the application, the rare earth element doped silicon carbide powder prepared by the preparation method is also provided. The silicide of the rare earth element in the prepared silicon carbide powder doped with the rare earth element is doped and wrapped in silicon carbide crystal grains, the rare earth element is uniformly doped in the silicon carbide powder, and when the silicon carbide powder is used as a raw material to grow a silicon carbide crystal, the polymorphism of the crystal can be effectively inhibited, and the quality of the obtained crystal is high.
Benefits of the present application include, but are not limited to:
(1) according to the preparation method, the prepared silicide of the rare earth element is utilized to synthesize the silicide of the rare earth element and high-purity silicon carbon powder, and the doped silicide of the rare earth element is wrapped in silicon carbide crystal grains, so that the rare earth element is uniformly doped in the silicon carbide powder; the rare earth element in the silicon carbide powder is gradually released along with the sublimation of the powder in the growth process by utilizing the rare earth element doped silicon carbide powder to grow crystals, so that the generation of polytype can be effectively inhibited.
(2) The preparation method selects the rare earth element-containing substance, has high purity and low cost, greatly reduces the production cost of the rare earth element-doped silicon carbide powder, and simultaneously improves the product purity.
(3) The preparation method is simple, the conditions are easy to control, and the prepared silicon carbide powder doped with the rare earth elements is uniform in rare earth element doping and high in purity.
(4) The rare earth element doped silicon carbide powder prepared by the method is uniform in rare earth element doping and high in purity, and when the silicon carbide powder is used as a raw material to grow a silicon carbide crystal, the obtained silicon carbide crystal is high in purity, few in defects and high in crystal quality.
Detailed Description
The present application will be described in detail with reference to examples, but the present application is not limited to these examples.
Unless otherwise specified, the raw materials and the like mentioned in the examples of the present application were purchased commercially. The embodiment provides a preparation method of the rare earth element doped silicon carbide powder, which comprises the following steps:
(1) uniformly mixing a rare earth element-containing substance with high-purity silicon powder, wherein the rare earth element-containing substance is at least one of powdered cerium (Ce) and other lanthanides (lanthanum La, praseodymium Pr, neodymium Nd and the like) or oxides of yttrium Y and scandium Sc; the oxide of the rare earth element is solid powder with the particle size not more than 100 mu m, and the purity is not lower than 99.99 percent; the molar ratio of the rare earth elements in the rare earth element-containing substance to the high-purity silicon powder is 1: 1.5-2.5; preferably, the molar ratio of the rare earth elements in the rare earth element-containing substance to the high-purity silicon powder is 1: 1.8-2.2;
(2) heating the mixture obtained in the step (1) to 1400-1800 ℃ under a vacuum condition, and reacting for 1-5 hours, wherein the high-purity silicon powder can react with the rare earth element oxide at the temperature to obtain rare earth element-doped silicide; preferably, the reaction temperature is 1500-1600 ℃, and the pressure is not higher than 10-2Pa, and the reaction time is 2-4 h;
(3) uniformly mixing the rare earth element doped silicide, high-purity silicon powder and high-purity carbon powder in the step (2), wherein the mass ratio of the total mass of the high-purity carbon powder and the high-purity silicon powder to the rare earth element doped silicide is 100: 0.001-5; preferably, the mass ratio of the sum of the mass of the high-purity carbon powder and the high-purity silicon powder to the rare earth element-doped silicide is 100: 0.005-2.5;
reacting the mixture for at least 5 hours at 1100-1600 ℃ under a vacuum condition to obtain rare earth element doped beta-type silicon carbide powder; preferably, the above mixture is subjected to a pressure of not higher than 10-2Pa, the temperature is 1300-1500 ℃, and the reaction is carried out for 5-15 h, so as to obtain the beta-type silicon carbide powder doped with the rare earth element.
② charging at the temperature of the step IThe temperature of the protective gas is raised to 2000-2500 ℃, the pressure is controlled to be 500-1000 mbar, and the reaction time is 10-40 h; the introduced protective gas is inert gas and H2The mixed gas of (1), H in the mixed gas2The volume fraction of the rare earth element is 2-3%, and the inert gas is selected from argon and/or helium to obtain the rare earth element doped alpha-type silicon carbide powder.
The difference between the method for preparing the rare earth element-doped silicon carbide powder and the preparation method is shown in table 1, and silicon carbide powder 1#, silicon carbide powder 2#, silicon carbide powder 3#, silicon carbide powder 4#, comparative silicon carbide powder D1#, comparative silicon carbide powder D2# and comparative silicon carbide powder D3# are prepared respectively. Wherein, the purity of the high-purity carbon powder, the high-purity silicon powder and the rare earth element oxide is more than 99.99 percent, and the charged protective gas is the mixed gas of argon and hydrogen.
TABLE 1
The prepared products of the silicon carbide powder No. 1, the silicon carbide powder No. 2, the silicon carbide powder No. 3, the silicon carbide powder No. 4, the comparative silicon carbide powder No. D1, the comparative silicon carbide powder No. D2 and the comparative silicon carbide powder No. D3 are characterized. The silicon carbide powder is used for growing silicon carbide crystals, the polytype of the grown crystals is detected, and the detection results are shown in table 2.
TABLE 2
From the results in table 2, the rare earth element doped silicon carbide powder prepared by the method is light yellow white agglomerated particles, the powder is uniform in rare earth element doping and high in purity, the total impurity content is not more than 10ppm, and the purity is not less than 99.999%. Compared with comparative silicon carbide powder D1# -D3 #, the rare earth element doped silicon carbide powder of the application has uniform doping, low impurity content and higher purity.
The mass ratio of the sum of the mass of high-purity silicon carbide powder in silicon carbide powder 1' #, silicon carbide powder 2' #andsilicon carbide powder 3' #, silicon carbide powder 1' #, silicon carbide powder 2' #andsilicon carbide powder 3' # synthesized by the method provided by the application to cerium silicide is 100:0.004, the silicon carbide powder 1#, the silicon carbide powder 2#, and the silicon carbide powder 3# are respectively used for growing a silicon carbide crystal, the silicon carbide powder 1' # is sampled at a position 80mm away from a crucible opening in a crystal growth crucible, the silicon carbide powder 2' # is sampled at a position 90mm away from the crucible opening, and the silicon carbide powder 3' # is sampled at a position 100mm away from the crucible opening.
The comparative silicon carbide powder D1'#, the comparative silicon carbide powder D2' #andthe comparative silicon carbide powder D3 '#arerespectively used for growing the silicon carbide crystals after mechanically mixing silicon carbide powder and cerium silicide (the mass ratio of the sum of the mass of the high-purity silicon carbide powder to the mass of the cerium silicide is 100:0.004), the comparative silicon carbide powder D1' # is sampled at a position 80mm away from a crucible opening in a crystal growth crucible, the comparative silicon carbide powder D2'# is sampled at a position 90mm away from the crucible opening, and the comparative silicon carbide powder D3' # is sampled at a position 100mm away from the crucible opening.
The comparative silicon carbide powder R1#, the comparative silicon carbide powder R2#, and the comparative silicon carbide powder R3# are respectively prepared by placing cerium silicide in a graphite small crucible (the mass ratio of the total mass of high-purity silicon carbide powder to cerium silicide in the small crucible is 100:0.004), embedding the cerium silicide in silicon carbide powder for the growth of silicon carbide crystals, sampling the comparative silicon carbide powder R1# at a position 80mm away from a crucible opening in the same long crystal crucible, sampling the comparative silicon carbide powder R2# at a position 90mm away from the crucible opening, and sampling the comparative silicon carbide powder R3# at a position 100mm away from the crucible opening.
GDMS is utilized to detect the concentration of cerium (Ce) in samples of silicon carbide powder 1'#, silicon carbide powder 2' #, silicon carbide powder 3'#, comparative silicon carbide powder D1' #, comparative silicon carbide powder D2'#, comparative silicon carbide powder D3' #, comparative silicon carbide powder R1#, comparative silicon carbide powder R2#, and comparative silicon carbide powder R3#, and the polycrystalline area of a crystal bar grown from the silicon carbide raw material is detected, and the results are shown in Table 3.
TABLE 3
As can be seen from the results in table 3, the Ce concentration in the raw material before the crystal growth reaction was about the same as the Ce concentration in the raw material (the Ce concentration results were different because cerium silicide was not completely and uniformly mixed in the raw material and the material taking heights of the raw material were different); while Ce was not detected in comparative silicon carbide powder R1# -R3#, in which cerium silicide was embedded in silicon carbide powder using a small crucible. The crystal growth is carried out for 20 hours, and as the cerium silicide is doped into the silicon carbide crystal phase, the cerium is released uniformly and slowly; in the method of directly mixing the cerium silicide and the silicon carbide raw materials, the cerium silicide has low melting point and is volatilized quickly, so the concentration of Ce in the raw materials is reduced quickly; the cerium silicide embedded in the small crucible gradually diffuses into the silicon carbide mass, but at a lower concentration and becomes harder to detect the further away from the small crucible. When the crystal growth is finished, because the cerium silicide is doped into the silicon carbide crystal phase, the residual cerium dopant in the raw materials can still be detected after the reaction is finished, and the cerium silicide is volatilized quickly in the early stage by the direct mixing method, so that few residues are left in the raw materials after the reaction. The cerium silicide in the small crucible diffuses out, and the concentration is higher as the small crucible is closer. In conclusion, cerium silicide in the raw materials of the application is uniformly volatilized, and the crystal bar is not in polytype; cerium silicide and silicon carbide powder are directly mixed, a large amount of cerium silicide volatilizes in the early stage, cerium silicide is insufficient in the later stage, and polytype is easily generated in the later stage; cerium silicide is buried in the crucible, and polytype is easily generated due to insufficient cerium silicide at the early stage.
The above description is only an example of the present application, and the protection scope of the present application is not limited by these specific examples, but is defined by the claims of the present application. Various modifications and changes may occur to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the technical idea and principle of the present application should be included in the protection scope of the present application.
Claims (10)
1. A preparation method of rare earth element doped silicon carbide powder is characterized by comprising the following steps:
(1) carrying out high-temperature reaction on a rare earth element-containing substance and high-purity silicon powder to obtain a rare earth element silicide;
(2) and (2) carrying out synthetic reaction on the silicide of the rare earth element in the step (1), high-purity silicon powder and high-purity carbon powder to obtain the high-purity silicon carbide powder doped with the rare earth element.
2. The production method according to claim 1, wherein the rare earth element is at least one selected from lanthanoid elements, scandium, and yttrium;
preferably, the rare earth element is selected from at least one of cerium, lanthanum, praseodymium, neodymium, scandium, and yttrium.
3. The production method according to claim 1, wherein the rare earth element-containing substance has a purity of not less than 99.99%,
preferably, the purity of the rare earth element-containing substance is not less than 99.999%;
preferably, the rare earth element-containing substance is a solid powder having a particle diameter of not more than 100 μm;
4. the preparation method according to claim 1, wherein in the step (1), the molar ratio of the rare earth elements in the rare earth element-containing substance to the high-purity silicon powder is 1: 2-4;
preferably, the rare earth element-containing substance is a rare earth element oxide.
5. The method according to claim 1, wherein in the step (1), the high-temperature reaction conditions are as follows: reacting a rare earth element-containing substance with high-purity silicon powder for 1-5 hours at the temperature of 1400-1800 ℃ under a vacuum condition;
preferably, the conditions of the high temperature reaction are: mixing the rare earth element-containing substance with high-purity silicon powder under the condition that the pressure is not higher than 10-2Pa, the temperature is 1500-1600 ℃, and the reaction lasts for 2-4 h.
6. The preparation method according to claim 1, wherein in the step (2), the mass ratio of the sum of the mass of the high-purity carbon powder and the high-purity silicon powder to the mass of the rare earth element silicide is 100: 0.001-5;
preferably, the mass ratio of the sum of the mass of the high-purity carbon powder and the high-purity silicon powder to the mass of the silicide of the rare earth element is 100: 0.005-2.5;
7. the preparation method according to claim 6, wherein in the step (2), the molar ratio of the high-purity carbon powder to the high-purity silicon powder is 1-1.5: 1;
preferably, the purities of the high-purity carbon powder and the high-purity silicon powder are not less than 99.99%, and the particle sizes of the high-purity carbon powder and the high-purity silicon powder are not more than 100 microns.
8. The method according to claim 1, wherein in the step (2), the conditions of the synthesis reaction comprise the steps of: firstly, reacting the rare earth element silicide, the high-purity silicon powder and the high-purity carbon powder in the step (1) for at least 5 hours at the temperature of 1100-1600 ℃ under the vacuum condition to obtain rare earth element-doped beta-type silicon carbide powder;
preferably, the conditions of the synthesis reaction comprise the following steps: firstly, the silicide of the rare earth element in the step (1), the high-purity silicon powder and the high-purity carbon powder are pressed at the pressure of not higher than 10-2Pa, the temperature is 1300-1500 ℃, and the reaction is carried out for 5-15 h, so as to obtain the beta-type silicon carbide powder doped with the rare earth element.
9. The method according to claim 8, wherein in the step (2), the synthesis reaction further comprises the steps of: secondly, introducing protective gas at the temperature of the first step, raising the temperature to 2000-2500 ℃, and reacting for at least 10 hours to obtain rare earth element doped alpha-type silicon carbide powder;
preferably, the synthesis reaction conditions further comprise the steps of: secondly, introducing protective gas to the temperature of the first step until the pressure is 500-1000 mbar, raising the temperature to 2200-2400 ℃, and reacting for 10-40 hours to obtain rare earth element doped alpha-type silicon carbide powder;
preferably, the protective gas is a mixed gas of inert gas and hydrogen, and the volume fraction of the hydrogen in the mixed gas is 2-3%.
10. The rare earth element-doped silicon carbide powder prepared by the preparation method of any one of claims 1 to 9.
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| WO2022000997A1 (en) * | 2020-06-30 | 2022-01-06 | 山东天岳先进科技股份有限公司 | Rare earth element-doped silicon carbide powder |
| CN114853022A (en) * | 2021-02-03 | 2022-08-05 | 比亚迪股份有限公司 | Composite powder for preparing silicon carbide and preparation method and application thereof |
| CN114853022B (en) * | 2021-02-03 | 2024-04-16 | 比亚迪股份有限公司 | Composite powder for preparing silicon carbide as well as preparation method and application thereof |
| CN115259163A (en) * | 2022-07-19 | 2022-11-01 | 宁波合盛新材料有限公司 | Synthesis method of cerium silicide |
| CN115259163B (en) * | 2022-07-19 | 2023-10-10 | 宁波合盛新材料有限公司 | Synthesis method of cerium silicide |
| CN115478324A (en) * | 2022-08-31 | 2022-12-16 | 昆明理工大学 | Method for growing single crystal or polycrystalline SiC crystal by cosolvent method |
| CN119352162A (en) * | 2024-10-12 | 2025-01-24 | 国芯半导体(仪征)有限公司 | A semiconductor multilayer epitaxial wafer material and preparation method thereof |
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