CN101302011A - Artificial synthetic method of high-pure SiC power for semiconductor single-crystal growth - Google Patents
Artificial synthetic method of high-pure SiC power for semiconductor single-crystal growth Download PDFInfo
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- CN101302011A CN101302011A CNA2008100166656A CN200810016665A CN101302011A CN 101302011 A CN101302011 A CN 101302011A CN A2008100166656 A CNA2008100166656 A CN A2008100166656A CN 200810016665 A CN200810016665 A CN 200810016665A CN 101302011 A CN101302011 A CN 101302011A
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- 239000004065 semiconductor Substances 0.000 title claims abstract description 18
- 239000013078 crystal Substances 0.000 title claims abstract description 16
- 238000010189 synthetic method Methods 0.000 title abstract description 3
- 239000000843 powder Substances 0.000 claims abstract description 41
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 32
- 239000007789 gas Substances 0.000 claims abstract description 27
- 229910052786 argon Inorganic materials 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 18
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 239000001257 hydrogen Substances 0.000 claims abstract description 15
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 15
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 230000006698 induction Effects 0.000 claims abstract description 12
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 12
- 239000001307 helium Substances 0.000 claims abstract description 7
- 229910052734 helium Inorganic materials 0.000 claims abstract description 7
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims abstract description 7
- 230000035484 reaction time Effects 0.000 claims abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 229910021431 alpha silicon carbide Inorganic materials 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 239000012535 impurity Substances 0.000 abstract description 8
- 229910052799 carbon Inorganic materials 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 6
- 229910052710 silicon Inorganic materials 0.000 abstract description 5
- 230000002194 synthesizing effect Effects 0.000 abstract description 4
- 239000000203 mixture Substances 0.000 abstract 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 25
- 238000006243 chemical reaction Methods 0.000 description 13
- 238000000815 Acheson method Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000003892 spreading Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011982 device technology Methods 0.000 description 1
- 238000002050 diffraction method Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000407 epitaxy Methods 0.000 description 1
- 238000001036 glow-discharge mass spectrometry Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
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Abstract
The invention provides a method for artificially synthesizing high-purity carborundum powder used for growing semiconductor single crystal. The method comprises the following steps of: (1) taking Si powder and C powder according to a mol ratio of 1 to 1; (2) putting the Si powder and the C powder into a crucible after the Si powder and the C powder are mixed uniformly, putting the crucible in a medium frequency induction heating furnace, vacuumizing a growth chamber of the heating furnace, and increasing the temperature to 1000 DEG C; charging high-purity argon gas, helium gas or mixture of argon gas and hydrogen into the growth chamber, heating the mixed gas up to a synthetic temperature of 1000 DEG C, and reducing the synthetic temperature to room temperature after maintaining for certain reaction time; (3) uniformly mixing powder of a product acquired in the primary synthesis, heating the product up to a secondary synthetic temperature of between 1600 and 2000 DEG C, synthesizing for 2 to 10 hours, and reducing the synthesized product to the room temperature to acquire high-purity SiC powder lot applicable to the semiconductor SiC single crystal growth. The method adopts a secondary synthetic method, not only can ensure that Si and C simple substance which are remained during the primary synthesis can completely react, but also can effectively remove most impurity elements carried in the Si powder and the C powder.
Description
Technical field
The present invention relates to a kind of artificial synthesis that is used for the high-pure SiC power of semiconductor single-crystal growth, belong to the sic powder synthesis technical field.
Background technology
Single-crystal silicon carbide is because of it has that energy gap is big, breakdown electric field is high, thermal conductivity is big, electronics saturation drift velocity height, specific inductivity is little, capability of resistance to radiation is strong, good unique characteristics such as chemical stability, have broad application prospects at opto-electronic devices such as demonstration, storage, detection and high temperature, high frequency, high-power electronic device field, be one of optimal third generation semi-conductor in the development of aspects such as single crystalline substrate, iso-epitaxy semiconductor film and device technology rapidly.Semi-insulating silicon carbide has low dielectric loss under high frequency, make it on as the single crystalline substrate based on the high temperature of wide band gap semiconducter (for example SiC, GaN), high-power, high-frequency electron device and transmitter very big advantage be arranged.The purity of SiC powder plays a part very important when subliming method growing semiconductor SiC monocrystalline, directly influences the crystalline quality and the electrical properties of growing single-crystal.
SiC powder synthetic method mainly contains three kinds: the organic synthesis method, spread method and Acheson method certainly.The organic synthesis method is mainly used in preparation nano grade Sic powder, in the synthetic raw material Determination of Multi-Impurities is arranged, though can obtain the high-purity alpha-SiC powder of foreign matter content below 1ppm, subsequent processes complexity by subsequent disposal, micro mist is collected difficulty, is not suitable for mass production and uses.The self-propagating high-temperature method is to utilize the effect of conduction certainly of substance reaction heat, makes chemical reaction takes place between the material, forms the high temperature building-up reactions of compound in the short period of time at the utmost point.Because the reaction between Si and the C is weak thermopositive reaction, continue to carry out required heat in order to guarantee to react when synthetic using from spreading method, add other additive therein." silicate journal " adopts in " preheating is from the research that spreads synthetic SiC powder mechanism " that 1998 the 26th volumes were delivered the 2nd phase that spreading method has synthesized β-SiC powder certainly, utilizes SiO
2And the thermopositive reaction between the Mg remedies shortage of heat, but this has introduced metallic impurity Mg and O element undoubtedly, has adopted nitrogen as carrier gas simultaneously, nitrogen enters in the synthetic product as impurity, electrical properties to growing crystal has material impact, and reacts inhomogeneous, and Si simple substance residue is arranged.
Industrial synthetic SiC powder mainly uses the Acheson method at present, and this method is french chemist E.G.Acheson invention in 1893.The Acheson method is under high temperature, highfield effect, SiO
2Reduced by C, at first generate β-SiC, be transformed into α-SiC under the high temperature.This method synthetic SiC powder oxide content reaches 1wt%, has hard solid block, needs operations such as pulverizing, pickling, makes foreign matter content higher, and its purity can't reach the level of growing semiconductor monocrystalline.
Summary of the invention
The present invention is directed to the deficiency that the synthetic SiC powder of traditional Acheson method exists, a kind of artificial synthesis that can access the high-pure SiC power that is used for semiconductor single-crystal growth of high yield is provided.
The artificial synthesis of high-pure SiC power of the present invention may further comprise the steps:
(1) 1: 1 in molar ratio ratio is got Si powder and C powder, and both purity is all greater than 99.998%, and granularity is all less than 500 μ m;
(2) first synthetic: as to put into crucible after getting Si powder and C powder mixed, then crucible is placed Medium Frequency Induction Heating Furnace, the growth room of process furnace is vacuumized, remove oxygen and nitrogen in the growth room, temperature is increased to 1000 ℃ simultaneously; In the growth room, charge into the mixed gas of high-purity argon gas, helium or argon gas and hydrogen then, the purity of argon gas, helium, hydrogen is all greater than 99.999%, be heated to 1500 ℃ of synthesis temperatures, keep 15 minutes reaction times, then reduce to room temperature, will be ground into powder greater than 1 centimetre aggregate in the reacted product less than 1mm;
(3) secondary is synthetic: it is even once synthesize middle products therefrom powder mixes, is reentered in the crucible, and crucible is placed Medium Frequency Induction Heating Furnace, and the growth room of process furnace is vacuumized, and temperature is increased to 1000 ℃ simultaneously; Charge into purity all greater than 99.999% high-purity argon gas, helium or argon gas and the mixed gas of hydrogen to the growth room then, be heated to 1600 ℃ to 2000 ℃ of synthesis temperatures, generated time is 2 hours-10 hours, then reduce to room temperature, can obtain being suitable for the high-purity alpha-SiC powder of semi-conductor SiC single crystal growing.
When charging into the mixed gas of argon gas and hydrogen in step (2) or (3) in the Medium Frequency Induction Heating Furnace growth room, the volume ratio of argon gas and hydrogen is 90: 10.
Because Si and C reaction are weak thermopositive reaction, the heat of id reaction can't be kept the carrying out of reaction, has therefore adopted the method for lasting heating to make reaction continue to carry out.
The present invention adopts synthesis method twice, overcome incomplete, the uneven shortcoming of building-up reactions one time, not only can make remaining Si and C simple substance complete reaction when first synthetic, and the high temperature can adopt secondary synthetic the time is effectively removed the most of impurity element that carries in Si powder and the C powder.Most Si and C have reacted and have generated SiC when once synthetic, can not cause the loss of high temperature Si, on the basis that guarantees synthetic yield, the purity of synthetic powder are improved, impurity concentration low than in the raw material.
Description of drawings
Accompanying drawing is the XRD figure of first synthetic and secondary synthetic product among the embodiment 1.
Embodiment
Embodiment 1
(1) got C powder and Si powder in 1: 1 in molar ratio, wherein C powder purity is greater than 99.998%, and granularity is less than 500 μ m, and Si powder purity is greater than 99.998%, and granularity is less than 500 μ m;
(2) carry out for the first time syntheticly, put into crucible after getting C powder and Si powder mixed, crucible is placed the Frequency Induction Heating growth furnace; The growth room is vacuumized, temperature is increased to 1000 ℃ simultaneously; Charge into purity greater than 99.999% high-purity argon gas to the growth room then, be heated to 1500 ℃, kept 15 minutes, then reduce to room temperature; To use the high purity graphite mortar to be ground into powder less than 1mm greater than 1 centimetre aggregate in the reacted product, this aggregate be very loose, can not introduce other metallic impurity owing to grinding;
(3) carry out secondary and synthesize, the products therefrom powder mixes is even in will once synthesizing, and is reentered in the crucible, crucible is placed the growth furnace of Frequency Induction Heating; The growth room is vacuumized, temperature is increased to 1000 ℃ simultaneously; Charge into purity greater than 99.999% high-purity argon gas to the growth room then, synthesis temperature is heated to 1600 ℃, and generated time is 10 hours, then reduces to room temperature, obtains the high-purity β phase SiC powder that be suitable for semi-conductor SiC single crystal growing of granularity less than 20 μ m.
Adopt powder diffraction method (XRD) that first synthesizing with the secondary synthetic product carried out material phase analysis, obtain XRD figure as shown in drawings.First synthetic powder has Si and C simple substance residue, reacts completely by synthetic the making of secondary.
Embodiment 2
What the difference of present embodiment and embodiment 1 was to charge in the growth room of Frequency Induction Heating growth furnace when synthetic for twice all is mixed gass of argon gas and hydrogen, the volume ratio of argon gas and hydrogen is 90: 10, and the purity of argon gas and hydrogen is all greater than 99.999%.Obtain the high-purity β phase SiC powder that be suitable for semi-conductor SiC single crystal growing of granularity at last less than 20 μ m.
Embodiment 3
The difference of present embodiment and embodiment 1 is that the secondary of step (3) is that synthesis temperature is heated to 1800 ℃ in synthetic, and generated time is 5 hours, obtains the high-purity α phase SiC powder that be suitable for semi-conductor SiC single crystal growing of granularity less than 20 μ m.
Embodiment 4
The difference of present embodiment and embodiment 1 is to charge in the growth room of Frequency Induction Heating growth furnace in step (2) first synthetic is purity greater than high-purity helium of 99.999%, what charge in the growth room of Frequency Induction Heating growth furnace during the secondary of step (3) is synthetic is purity greater than 99.999% high-purity hydrogen, and the synthesis temperature in the step (3) is heated to 2000 ℃, generated time is 2 hours, obtains the high-purity α phase SiC powder that is suitable for semi-conductor SiC single crystal growing of granularity 100 μ m-200 μ m.And the product after synthetic carried out impurity analysis, following table has provided GDMS and has analyzed present embodiment synthetic SiC powder foreign matter content:
Claims (2)
1. an artificial synthesis that is used for the high-pure SiC power of semiconductor single-crystal growth is characterized in that, may further comprise the steps:
(1) 1: 1 in molar ratio ratio is got Si powder and C powder, and both purity is all greater than 99.998%, and granularity is all less than 500 μ m;
(2) first synthetic: as to put into crucible after getting Si powder and C powder mixed, then crucible is placed Medium Frequency Induction Heating Furnace, the growth room of process furnace is vacuumized, remove oxygen and nitrogen in the growth room, temperature is increased to 1000 ℃ simultaneously; In the growth room, charge into the mixed gas of high-purity argon gas, helium or argon gas and hydrogen then, the purity of argon gas, helium, hydrogen is all greater than 99.999%, be heated to 1500 ℃ of synthesis temperatures, keep 15 minutes reaction times, then reduce to room temperature, will be ground into powder greater than 1 centimetre aggregate in the reacted product less than 1mm;
(3) secondary is synthetic: it is even once synthesize middle products therefrom powder mixes, is reentered in the crucible, and crucible is placed Medium Frequency Induction Heating Furnace, and the growth room of process furnace is vacuumized, and temperature is increased to 1000 ℃ simultaneously; Charge into purity all greater than 99.999% high-purity argon gas, hydrogen or both mixed gass to the growth room then, be heated to 1600 ℃ to 2000 ℃ of synthesis temperatures, generated time is 2 hours-10 hours, then reduces to room temperature, can obtain being suitable for the high-purity alpha-SiC powder of semi-conductor SiC single crystal growing.
2. the artificial synthesis that is used for the high-pure SiC power of semiconductor single-crystal growth according to claim 1, it is characterized in that, when charging into the mixed gas of argon gas and hydrogen in described step (2) or (3) in the Medium Frequency Induction Heating Furnace growth room, the volume ratio of argon gas and hydrogen is 90: 10.
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| CN102503474A (en) * | 2011-10-27 | 2012-06-20 | 中钢集团洛阳耐火材料研究院有限公司 | Sintering method of self-bonding SiC refractory material |
| CN102674357A (en) * | 2012-05-29 | 2012-09-19 | 上海硅酸盐研究所中试基地 | Method for synthesizing high-purity silicon carbide raw material for growing silicon carbide single crystals |
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