CN102560672A - Semi-insulating silicon carbide single crystal material - Google Patents
Semi-insulating silicon carbide single crystal material Download PDFInfo
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- CN102560672A CN102560672A CN2010106174070A CN201010617407A CN102560672A CN 102560672 A CN102560672 A CN 102560672A CN 2010106174070 A CN2010106174070 A CN 2010106174070A CN 201010617407 A CN201010617407 A CN 201010617407A CN 102560672 A CN102560672 A CN 102560672A
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Abstract
The invention discloses a semi-insulating silicon carbide single crystal material. The semi-insulating silicon carbide single crystal or single crystal wafer has resistivity of over 1E5ohm.cm at the room temperature. After the semi-insulating silicon carbide single crystal or single crystal wafer which is subjected to thermal annealing, the resistivity of the semi-insulating silicon carbide single crystal or single crystal wafer is kept greater than 1E5ohm.cm. The semi-insulating silicon carbide single crystal or single crystal wafer at least comprises one compensation dopant; a distance from the electron energy level of the dopant to the edge of a silicon carbide band gap is sufficiently long so as not to generate the electric conduction; the condensation of the compensation dopant is not less than the difference between the concentrations at the shallow donor level and the shallow acceptor level in the crystal and is required to be greater than 5*1,016cm<-3>, so that the concentration of the dopant fixed at the deep level is sufficient for impurities at the shallow level; the concentration of the dopant is less than 5*1,017cm<-3> to prevent the defect of a silicon carbide structure, which is caused by separation of the dopant; and after the silicon carbide single crystal or single crystal wafer is subjected to thermal annealing at a temperature of 1,200 DEG C, the resistivity of the silicon carbide single crystal or single crystal wafer is kept greater than 1E5ohm.cm.
Description
Technical field
The present invention relates to a kind of semiconductor material that can be applied to high-frequency element, relate in particular to a kind of semi-insulating silicon carbide monocrystal material.
Background technology
With silit (SiC), gan (GaN) is the semiconductor material with wide forbidden band of representative, is the third generation semi-conductor after silicon (Si), gallium arsenide (GaAs).Compare with the GaAs conventional semiconductor material with Si, SiC has excellent properties such as high heat conductance, high breaking down field strength, high saturated electrons drift speed and high bonding energy, is having great application prospect aspect high temperature, high frequency, superpower and the radioprotective device.The transistor of semi-insulating silicon carbide preparation can produce the power that surpasses GaAs microwave component five times power density under up to the 10GHz frequency.The people who is familiar with the microwave device technology recognizes; Under the situation of using high resistivity and the semi-insulated silicon carbide substrates of high crystalline quality, just can prepare high performance microwave device, and then be applied to like Application Areass such as cellular communication device and powerful airborne radar, shipborne radars.
At present mainly through in the SiC band gap, forming deep energy level, the mode that compensates the difference of shallow donor that involuntary doping forms and shallow acceptor concentration through deep energy level improves the resistivity of carborundum crystals.Usually the method that forms deep energy level mainly contains following two kinds: (1) forms intrinsic point defects; (2) add magnesium-yttrium-transition metal doping agent, particularly vanadium.Wherein, Method (1) can improve resistivity through in crystal, introducing point defect; But the concentration of point defect can reduce usually behind thermal annealing; Thereby cause resistivity decreased, so this method can not guarantee the consistence of single-crystal silicon carbide resistivity and be applicable to fairly large carborundum crystals production demand.And in the method (2); Concentration range for adding the magnesium-yttrium-transition metal doping agent is too high usually; For example, (publication number: the concentration that requires transition element doped dose CN 1985029A) is less than 2 * 10 to be entitled as the one Chinese patent application of " low-doped semi-insulation SiC crystal and method "
16Cm
-3, and for example USP 5,611, require in 955 transition group doping agent such as the vanadium mass percent scope in the SiC crystal 300 to 1000ppm (about 1 * 10
18Cm
-3To 4 * 10
18Cm
-3).The defective of being brought thus is that crystal mass reduces.For example, exceeded its solid solubility limit (about 5 * 10 when the concentration of doping agent vanadium in the SiC crystal
17Cm
-3) time, just in crystal, form the precipitate of vanadium and produce lattice defect such as microtubule, thereby influence the crystalline crystalline quality, be unfavorable for being used for preparing high performance microwave device.
But then, if magnesium-yttrium-transition metal doping agent concentration in the SiC crystal is low excessively, also be difficult to realize the stable and repeatable of the semi-insulating performance of SiC crystal.Need (" involuntary doping " refers in the SiC crystal growing process to involuntary doping because this means; Impurity such as the N that contains in the SiC raw material, B; Residual N impurity in impurity such as the B that contains in plumbago crucible that uses and the lagging material, Al and the environment; These involuntary adulterated impurity all can reduce SiC crystalline resistivity) the control of foreign matter content harsh requirement is proposed, so this also is unfavorable for large-scale industrial production.
Summary of the invention
Therefore, the objective of the invention is to overcome the defective of above-mentioned prior art,, a kind of high-quality semi-insulating silicon carbide crystalloid is provided through the concentration range of controlled doping agent in crystal.
The objective of the invention is to realize through following technical scheme:
According to the present invention, a kind of semi-insulating silicon carbide monocrystal material is provided, comprising:
At least a deep level dopant, the electronic level of said deep level dopant apart from silit band gap edge more than or equal to 0.3eV; With
Shallow level impurity, the electronic level of said shallow level impurity apart from silit band gap edge less than 0.3eV;
Wherein, the concentration of said deep level dopant is more than or equal to the concentration of said shallow level impurity, and simultaneously less than the solid solubility limit of said deep level dopant in said single-crystal silicon carbide, said single-crystal silicon carbide material at room temperature has greater than 1 * 10
5The resistivity of Ω cm.
In above-mentioned semi-insulating silicon carbide monocrystal material, the crystal formation of said single-crystal silicon carbide can be 2H, 4H, 6H, a kind of among 3C or the 15R.
In above-mentioned semi-insulating silicon carbide monocrystal material; Said shallow level impurity comprises shallow donor impurity and shallow acceptor impurity; And the concentration of said deep level dopant is not less than the difference between said shallow donor and the acceptor impurity concentration; Compensating clean shallow level impurity, thereby improve single-crystal silicon carbide or single-chip resistivity.In one embodiment, said shallow donor impurity is a nitrogen, and said shallow acceptor impurity is boron and aluminium.
In above-mentioned semi-insulating silicon carbide monocrystal material, said deep level dopant comprises IB in the periodic table of elements, IIB, IIIB, IVB, VB, VIB, VIIB, at least a element of VIIIB family.In one embodiment, the concentration of said deep level dopant is 5 * 10
16Cm
-3~5 * 10
17Cm
-3In the scope.
Above-mentioned semi-insulating silicon carbide monocrystal material resistivity behind 1200 ℃ of thermal annealings still keeps greater than 1 * 10
5Ω cm.
Preferably, above-mentioned semi-insulating silicon carbide monocrystal material has greater than 1 * 10
6The resistivity of Ω cm, and resistivity still keeps greater than 1 * 10 behind 1200 ℃ of thermal annealings
6Ω cm.
Compared with prior art, the invention has the advantages that:
Description of drawings
Followingly the embodiment of the invention is described further with reference to accompanying drawing, wherein:
Fig. 1 is the wafer Raman spectrogram of the embodiment of the invention 1;
Fig. 2 is the wafer Raman spectrogram of the embodiment of the invention 2;
Fig. 3 is the wafer Raman spectrogram of the embodiment of the invention 3.
Embodiment
Below in conjunction with embodiment, further describe content of the present invention and advantage.
Need to prove; In following examples of the present invention; All crystals all adopts SiC crystal preparation method commonly used---physical vapor transmission method (Physical Vapor Transport Method); The specifying information of relevant this method and the employed silicon carbide crystal growing device of this method is disclosed among the Chinese invention patent ZL 200310113521.X that is entitled as " a kind of silicon carbide crystal growing device " and the Chinese invention patent ZL200310113523.9 of being entitled as of Granted publication on the 28th June in 2006 " method and the device thereof of physical vapor transmission growing silicon carbide single crystal " of Granted publication on the 29th in applicant's March in 2006, this by reference with they with the present invention not contradiction content partly be included in the middle of the present invention.Yet for it will be understood by those skilled in the art that through the for example additive method of high temperature chemical vapor deposition method (HTCVD), liquid phase method, can obtain single-crystal silicon carbide of the present invention equally, following method of the present invention is merely preferred.
The growth of embodiment 1:6H crystal formation semi-insulating silicon carbide monocrystalline
Process of growth: in 1000g silit starting material (purity 99.999%), add the vanadium carbide powder (purity 99.999%) of 500mg, mix with ball mill.The starting material that mix are packed in high-purity plumbago crucible, covered the crucible cover of seed crystal bonding, put into crystal growing furnace and grow.Charge into argon gas in the reactors, pressure-controlling is less than 2000Pa.Seed temperature remains between 2100-2200 ℃, and material temperature remains between 2300-2400 ℃, and the thermograde between raw material and the seed crystal remains between 130-200 ℃.
Crystal after the growth is along the direction section perpendicular to < 0001 >; Choose each a slice of wafer in the early stage of growing, growth mid-term and growth later stage respectively; Through behind the optical polish, with the resistivity of contactless resistance meter measurement wafer, the result obtains the resistivity greater than 1E5 Ω cm.Choose one of them wafer and carry out the Raman test, the Raman spectrogram that obtains is as shown in Figure 1, shows that its crystal formation is the 6H crystal formation.With the content of impurity in second ion mass spectroscopy or the glow discharge mass spectrometry detection wafer, the result sees table 1.
Foreign matter content in table 1, the silicon carbide wafer (unit: cm
-3)
Impurity element | N | B | Al | V |
Constituent content | 1.8E+17 | 2.5E+17 | 2.0E+16 | 2.9E+17 |
From table 1, can find out; The concentration sum of boron and aluminium is greater than the concentration of nitrogen; Therefore vanadium is with the redeeming of alms giver's form; And the concentration of vanadium is poor greater than the concentration of p type shallow donor energy level (boron and aluminium) and n type shallow acceptor energy level (nitrogen), and this concentration is less than the solid solubility limit (5 * 10 of vanadium in single-crystal silicon carbide simultaneously
17Cm
-3).Through the morphology observation of single-crystal silicon carbide is found that the single-crystal silicon carbide crystalline quality is good, micropipe density is little, does not have other visible macroscopic defects.
To this wafer 1200 ℃ of thermal anneal process in the high-purity argon gas protective atmosphere of 50,000 Pa, the room temperature resistivity that records wafer after the processing remains on greater than in the 1E5 Ω cm scope, this shows the resistivity almost not influence of anneal to silicon carbide wafer of the present invention.
The growth of embodiment 2:4H crystal formation semi-insulating silicon carbide monocrystalline
Process of growth: in 1000g silit starting material, add the vanadium carbide powder of .450mg, mix with ball mill.The starting material that mix are packed in high-purity plumbago crucible, covered the crucible cover of seed crystal bonding, put into crystal growing furnace and grow.Charge into argon gas in the reactors, pressure-controlling is less than 2000Pa.Seed temperature remains between 2050-2150 ℃, and material temperature remains between 2250-2350 ℃, and the thermograde between raw material and the seed crystal remains between 130-200 ℃.
Crystal after the growth is along the direction section perpendicular to < 0001 >; Choose each a slice of wafer in the early stage of growing, growth mid-term and growth later stage respectively; Through behind the optical polish, with the resistivity of contactless resistance meter measurement wafer, the result obtains the resistivity greater than 1E5 Ω cm.Choose one of them wafer and carry out the Raman test, the Raman spectrogram that obtains is as shown in Figure 1, shows that its crystal formation is the 4H crystal formation.With the content of impurity in second ion mass spectroscopy or the glow discharge mass spectrometry detection wafer, the result sees table 1.
The foreign matter content of table 2, silicon carbide wafer (unit: cm
-3)
Impurity element | N | B | Al | V |
Constituent content | 9.4E+16 | 5.4E+16 | 5.49E+15 | 9.3E+16 |
Can find out that from table 2 the concentration sum of boron and aluminium is less than the concentration of nitrogen, vanadium is with the redeeming of deep acceptor energy level form, and the concentration of vanadium is not less than concentration poor of shallow donor's energy level (boron and aluminium) and shallow acceptor energy level (nitrogen).In addition, this concentration is less than the solid solubility limit (5 * 10 of vanadium in single-crystal silicon carbide
17Cm
-3).Through the morphology observation of single-crystal silicon carbide is found that the single-crystal silicon carbide crystalline quality is good, micropipe density is little, does not have other visible macroscopic defects.
Embodiment 3: the growth of codope 6H crystal formation semi-insulating silicon carbide monocrystalline
Process of growth: in 1000g silit starting material, add vanadium carbide powder (purity 99.999%) and the 100mg scandium powder (purity 99.999%) of 400mg, mix with ball mill.The starting material that mix are packed in high-purity plumbago crucible, covered the crucible cover of seed crystal bonding, put into crystal growing furnace and grow.Charge into argon gas in the reactors, pressure-controlling is less than 2000Pa.Seed temperature remains between 2100-2200 ℃, and material temperature remains between 2300-2400 ℃, and the thermograde between raw material and the seed crystal remains between 130-200 ℃.
Crystal after the growth is along the direction section perpendicular to < 0001 >; Choose each a slice of wafer in the early stage of growing, growth mid-term and growth later stage respectively; Through behind the optical polish, with the resistivity of contactless resistance meter measurement wafer, the result obtains the resistivity greater than 1E5 Ω cm.Choose one of them wafer and carry out the Raman test, the Raman spectrogram that obtains is as shown in Figure 1, shows that its crystal formation is the 6H crystal formation.With the content of impurity in second ion mass spectroscopy or the glow discharge mass spectrometry detection wafer, the result sees table 3.
Foreign matter content in table 3, the silicon carbide wafer (unit: cm
-3)
Impurity element | N | B | Al | V | Sc |
Constituent content | 2.6E+17 | 1.8E+17 | 2.0E+16 | 2.5E+17 | 7.0E+16 |
From table 3, can find out; The concentration sum of boron and aluminium is less than the concentration of nitrogen; Vanadium and scandium are with the redeeming of deep acceptor energy level form; The concentration of vanadium and scandium is poor with the concentration that is not less than shallow donor's energy level (boron and aluminium) and shallow acceptor energy level (nitrogen), and the concentration of vanadium and scandium is respectively less than they solid solubility limits (5 * 10 in single-crystal silicon carbide
17Cm
-3) and (3.2 * 10
17Cm
-3), in addition, it is good to obtain the single-crystal silicon carbide crystalline quality through morphology observation, and micropipe density is little, does not have other visible macroscopic defects.
Can find out from above embodiment,, can prepare high-quality semi-insulating silicon carbide crystalloid through the concentration range of control deep level dopant in crystal.
Thus, the present invention proposes a kind of semi-insulating silicon carbide monocrystalline or monocrystal material, contains at least a compensatory doping agent in this monocrystal material, so that single-crystal silicon carbide or single-chip satisfy semi-insulated electric property.The electronic level of this doping agent is enough dark in the semi-conductor forbidden band; Should be apart from the bottom of the silit conduction band or top of valence band 0.3eV at least; I.e. " deep level dopant "; Because after the element doping of deep level dopant gets into the lattice of silit, in the forbidden band, can form two kinds of electronic levels, thereby reach the compensation purpose.With the v element is example, and a kind of electronic level is the donor level that is positioned at 0.66-0.8eV at the bottom of the conduction band, and another kind is the acceptor level that is positioned at top of valence band 1.5eV.In the above-described embodiments, deep level dopant is vanadium or vanadium and scandium, but is not limited thereto, all can satisfy element in the above conditions of elements periodictable can be by way of compensation unit's resistivity of usually modulating single-crystal silicon carbide; For example in other embodiments, when deep level dopant be transition element (IB, IIB, IIIB; IVB, VB, VIB; When VIIB, in VIIIB) one or more, resulting single-crystal silicon carbide or single-chip record through test can guarantee that resistivity is greater than 1 * 10
5Ω cm, or be preferably greater than 1 * 10
6Ω cm, and resistivity still remains in the same range as after through 1200 ℃ of thermal annealings.
Also comprise shallow level impurity in single-crystal silicon carbide or the single-chip.Said shallow level impurity is meant electronic level apart from the element of silit band gap edge less than 0.3eV, for example the nitrogen in the foregoing description (n type shallow level impurity is also claimed shallow donor impurity), boron and aluminium (p type shallow level impurity is also claimed shallow acceptor impurity).Will be appreciated that; Above-mentioned three kinds of elements are owing to impurity element at the bottom of the very difficult back of the body of controlling of the factors such as purity of vacuum tightness and raw material in the process of growing silicon carbice crystals; But said shallow level impurity is not limited to above-mentioned three kinds of elements, also comprises the equidistant silit band gap of some transition elements edge other element less than 0.3eV.
Can know by above embodiment; In single-crystal silicon carbide of the present invention or monocrystal material; The concentration of said deep level dopant should be not less than the difference between the shallow donor and shallow acceptor impurity concentration in the crystal, compensating clean shallow level impurity, thereby improves single-crystal silicon carbide or single-chip resistivity.Specifically, when the concentration of n type shallow energy level during greater than the concentration of p type shallow energy level, deep level dopant is as receiving main redeeming (like embodiment 2); When the concentration of n type shallow donor energy level during less than the concentration of p type shallow acceptor energy level, deep level dopant is as alms giver's redeeming (like embodiment 1).This compensation mechanism makes that the band gap width of electronic level remains at enough big position in the single-crystal silicon carbide, thereby obtains sufficiently high resistivity.
With the vanadium is example, and the concentration of deep level dopant should be greater than 5 * 10
16Cm
-3, with the adequate remedy shallow level impurity and make the concentration of dopant that is fixed on deep energy level enough high, the resistivity of single-crystal silicon carbide or single-chip resistivity behind thermal annealing keeps greater than 1 * 10
5Ω cm, and the resistivity of different batches growing crystal is consistent.Simultaneously; In crystal growing process; The steam output of vanadium can reduce along with the lengthening of crystal growth time gradually; Thereby the concentration that the concentration through the vanadium of different depths in the control sic raw material guarantees evaporation and is doped to the vanadium before and after the single-crystal silicon carbide in the scope of regulation, thereby guarantee the consistence of crystal longitudinal resistivity, avoid the later stage because the deficiency of vanadium causes the resistivity reduction.But the concentration of deep level dopant should be less than its solid solubility limit in crystal simultaneously, and for example vanadium is 5 * 10
17Cm
-3, with lattice defect even the structural phase transition that prevents to cause owing to separating out of doping agent.
In sum; The present invention is through the concentration range of deep level dopant in the control semi-insulating silicon carbide crystalloid; Obtain the carborundum crystals of high crystalline quality; The requirement of the good high frequency of its characteristic conforms, high-power component, and less demanding to back of the body end impurity, therefore can be in the working range production and the use of broad.The resistivity of this crystal before and after annealing is consistent basically, is more suitable for large-scale industrial production.
Be noted that preceding text explain and explain design of the present invention and principle, and the foregoing description also is merely schematic purpose.Under the situation of the spirit and scope of the present invention that do not depart from claim and limited, those skilled in the art can make various modifications and distortion to the present invention.
Claims (10)
1. semi-insulating silicon carbide monocrystal material comprises:
At least a deep level dopant, the electronic level of said deep level dopant apart from silit band gap edge more than or equal to 0.3eV; With
Shallow level impurity, the electronic level of said shallow level impurity apart from silit band gap edge less than 0.3eV;
Wherein, the concentration of said deep level dopant is more than or equal to the concentration of said shallow level impurity, and simultaneously less than the solid solubility limit of said deep level dopant in said single-crystal silicon carbide, said single-crystal silicon carbide material at room temperature has greater than 1 * 10
5The resistivity of Ω cm.
2. semi-insulating silicon carbide monocrystal material according to claim 1, the crystal formation of said single-crystal silicon carbide is 2H, 4H, 6H, a kind of among 3C or the 15R.
3. semi-insulating silicon carbide monocrystal material according to claim 1, said shallow level impurity comprise shallow donor impurity and shallow acceptor impurity, and the concentration of said deep level dopant is not less than the difference between said shallow donor and the shallow acceptor impurity concentration.
4. semi-insulating silicon carbide monocrystal material according to claim 3, said shallow donor impurity are nitrogen, and said shallow acceptor impurity is boron and aluminium.
5. semi-insulating silicon carbide monocrystal material according to claim 1, said deep level dopant comprises IB in the periodic table of elements, IIB, IIIB, IVB, VB, VIB, VIIB, at least a element of VIIIB family.
6. semi-insulating silicon carbide monocrystal material according to claim 3, said deep level dopant are vanadium.
7. semi-insulating silicon carbide monocrystal material according to claim 3, the concentration of said deep level dopant is 5 * 10
16Cm
-3~5 * 10
17Cm
-3In the scope.
8. according to the described semi-insulating silicon carbide monocrystal material of claim 1, said semi-insulating silicon carbide monocrystal material resistivity behind 1200 ℃ of thermal annealings still keeps greater than 1 * 10
5Ω cm.
9. according to the described semi-insulating silicon carbide monocrystal material of claim 1, said semi-insulating silicon carbide monocrystal material has greater than 1 * 10
6The resistivity of Ω cm.
10. according to the described semi-insulating silicon carbide monocrystal material of claim 1, said semi-insulating silicon carbide monocrystal material resistivity behind 1200 ℃ of thermal annealings still keeps greater than 1 * 10
6Ω cm.
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CN106894090B (en) * | 2017-03-17 | 2019-09-24 | 山东大学 | A kind of p-type SiC single crystal preparation method of high quality low-resistivity |
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CN109280965A (en) * | 2018-10-16 | 2019-01-29 | 山东天岳先进材料科技有限公司 | A kind of high quality Semi-insulating silicon carbide mono-crystal and substrate adulterating a small amount of vanadium |
WO2020077846A1 (en) * | 2018-10-16 | 2020-04-23 | 山东天岳先进材料科技有限公司 | Semi-insulating silicon carbide single crystal doped with small amount of vanadium, substrate prepared therefrom, and preparation method therefor |
TWI703242B (en) * | 2018-10-16 | 2020-09-01 | 大陸商山東天岳先進材料科技有限公司 | Semi-insulating silicon carbide single crystal doped with a small amount of vanadium, substrate and preparation method |
CN113341485A (en) * | 2020-03-02 | 2021-09-03 | Ii-Vi特拉华有限公司 | Optical grade vanadium compensated 4H single crystal and 6H single crystal |
CN113981536A (en) * | 2020-07-27 | 2022-01-28 | 环球晶圆股份有限公司 | Silicon carbide ingot and preparation method thereof |
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