CN109537055A - A kind of semi-insulating gallium oxide crystal and preparation method thereof - Google Patents
A kind of semi-insulating gallium oxide crystal and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/34—Edge-defined film-fed crystal-growth using dies or slits
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Abstract
The present invention provides a kind of semi-insulating gallium oxide crystal and preparation method thereof.The crystal molecule formula is β-(Ga1‑xAx)2O3, A represents Ca, Zn, Ti or Ni element, 0.0001≤x≤0.2.Growing method can be the common growing methods such as light float-zone method, czochralski method, EFG technique.Compared with prior art, the present invention, which obtains gallium oxide crystal, has high resistivity, can be used as semi-insulating substrate, for devices such as field effect transistor, high mobility transistors.
Description
Technical field
The present invention relates to a kind of semi-insulating gallium oxide crystal and preparation method thereof, in particular to Ca, Zn, Ti, Co, Ni element
Gallium oxide body block crystal and preparation method thereof is adulterated, semiconductor material and preparation field are belonged to.
Background technique
Gallium oxide (β-Ga2O3) with its excellent physical property and low-cost advantage, by the extensive of scientific circles and industrial circle
Concern.β-Ga at present2O3Field effect transistor, schottky diode device performance are increased dramatically, in terms of disruptive field intensity
Through the theoretical limit more than SiC, GaN.β-Ga2O3Huge competitive advantage is shown in high voltage, low-loss field, becomes a kind of
The super semiconductor material with wide forbidden band quickly grown.
In the preparation of scene effect transistor, need high resistant or even semi-insulating chip as substrate material, to reduce device dark
Electric current improves devices switch ratio.Therefore, in high performance field effect transistors, high mobility transistor and hetero-epitaxy device
In have important application value.Oxidation gallium material contains the accompanying impurities such as Si, Zr, Sn, and the gallium oxide crystal for growing acquisition is logical
Normal carrier concentration with higher, it is difficult to be directly used as semi-insulating substrate.High pure raw material can be used for growing high resistant gallium oxide
Crystal, but cost of material is higher, operating process requires height, therefore crystal higher cost to clean level.Above-mentioned factor causes
Semi-insulating gallium oxide crystal growth difficulty is big, at high cost.
Element doping is the common method for regulating and controlling semiconductor resistor rate.Such as it is mixed in GaAs and mixes V in Cr, SiC
Realize the preparation of high-resistance crystalline.But different semiconductor material doped chemical types and doping process are very different, after doping
The carrier concentration of crystal is influenced also different.Different doped chemicals can also have the differences such as gap, displacement in crystal of the same race
Doped forms.Therefore, it is necessary to dopant and adulterate work according to element example radius, Doped ions valence state and impurity energy level depth
Skill is explored.The current report for having had Mg, Fe doping high-resistance crystalline, but Mg2+Opposite Ga3+Radius is smaller, be easy to cause
Larger distortion of lattice reduces crystal quality.Fe3+After incorporation, black can be presented in crystal, and crystal absorbs big, crystal in visible waveband
Quality is lower.Different doped chemicals influence difference to crystal electrical properties, and furthermore various concentration also can be to crystal carrier concentration
And monocrystalline quality causes Different Effects, other crystal of simple analogy or doped chemical can not achieve gallium oxide crystal electrical properties and
The Effective Regulation of crystal quality.
Therefore, suitable doped chemical and doping concentration are found, design grows inexpensive high resistant gallium oxide single crystal with weight
The application value wanted.
Summary of the invention
In view of the problems of the existing technology, crystal is reduced caused by especially doped chemical is improper in the prior art to carry
It flows the ineffective of sub- concentration and adulterates the problem of causing crystal quality to deteriorate, the present invention has screened the doped chemical to work well
And doping concentration, a kind of semi-insulating gallium oxide crystal and preparation method thereof is provided, which can be used as high quality High resistivity substrate
It is made for semiconductor devices.
Technical scheme is as follows:
A kind of semi-insulating gallium oxide crystal, the crystal molecule formula are β-(Ga1-xAx)2O3, it is first that A represents Ca, Zn, Ti or Ni
Element, 0.0001≤x≤0.2.
, according to the invention it is preferred to, A represents Ti element, 0.005≤x≤0.15.Titanium elements belong to the 4th subgroup, in crystalline substance
Trivalent and 4 valences can be presented in body.According to common sense, titanium can generate free carrier in crystal.But by testing us
It was found that titanium replaces gallium that can generate deeper energy level in forbidden band in gallium oxide, the background carriers in crystal can be captured, in turn
Improve crystal resistivity.After titanium elements mix crystal, trivalent is mainly presented, it is identical as Ga element valence.The doping of element can reach
To higher concentration, carrier concentration can be reduced to lower, increase the resistivity of crystal to higher level.
, according to the invention it is preferred to, A represents Ca or Zn element, 0.0001≤x≤0.01.Ca, Zn element doping can also incite somebody to action
The carrier concentration of crystal reduces, and increases the resistivity of crystal.Doping concentration is unsuitable excessively high, to be less than Ga element mole
0.1% is advisable.Ca, Zn are belonging respectively to the second main group and the second subgroup, two elements closer valence band in gallium oxide crystal energy band,
But the activation energy of Ca, Zn in gallium oxide crystal is higher, it is difficult to realize hole conduction, but can neutralize the electricity in crystal
Son, and then reduce the electron concentration in crystal.Opposite Mg element, Ca, Zn element ion radius and Ga ion half of period 4
Diameter difference is smaller, and Ca, Zn mix that rear distortion of lattice is small, and crystal structure quality is higher.In addition, crystal will not generate after doping Ca, Zn
Apparent color can widen the application range of crystal.
, according to the invention it is preferred to, A represents the 8th subgroup Ni element, 0.0001≤x≤0.001.Ni element doping can be with
Deep energy level defect is formed, the carrier concentration of crystal is reduced, the resistivity of crystal is increased.And it is dense that carrier can be effectively reduced
Degree, but doping concentration is unsuitable excessively high, is advisable be less than Ga element mole 0.1%.
According to the present invention, light float-zone method, czochralski method, EFG technique etc. can be used in the growth of above-mentioned semi-insulating gallium oxide crystal.
Preferably, preparation step is as follows:
(1) selection and processing of raw material
Select the Ga of 99.9% or more purity2O3, doped raw material is using CaO, ZnO, Ti2O3, NiO or above-mentioned element its
The oxide of his valence state, 99.9% or more purity；By Ga2O3It is uniformly mixed with above-mentioned one or more kinds of doped raw materials, using liquid
Press is pressed into pie or static pressure is waited to be pressed into column charge bar；The gallium oxide polycrystal material adulterated using solid sintering technology synthesized element；
Alternatively, directly to equipped with Ga2O3It is directly added into above-mentioned one or more kinds of doped raw materials in the crucible of raw material and directly carries out crystal life
It is long；
(2) crystal growth
Raw material will be pressed to be fitted into Iridium Crucible, or fixed in the furnace of light floating region；
Select<100>,<010>and<001>direction seed crystal；
The growth for carrying out gallium oxide single crystal is grown using light float-zone method, czochralski method or EFG technique.
Light float-zone method preferably uses pure oxygen atmosphere in the present invention, can reduce the Lacking oxygen defect of crystal kind and reduce crystalline substance
Concentration of background carriers in body.Oxygen atmosphere flowing velocity 0.5-6L/min.
The preferred iraurite of czochralski method or platinum pot containing 8-18% rhodium.Selecting iraurite pot is employed nitrogen as crystal life
Long atmosphere, select rhodium-containing platinum pot when using oxygen content 50%-100% oxygen+nitrogen atmosphere.
Iraurite or platinum pot and mold containing 8-18% rhodium are preferably used in EFG technique.Atmosphere and Czochralski grown gas
Atmosphere is identical.
Unless otherwise specified, state of the art is pressed.
Beneficial effects of the present invention:
The present invention is in β-Ga2O3Ca, Zn, Ti, Ni element are mixed in crystal, can effectively capture carrier, doped crystal has
Semiconductor devices electric leakage can be effectively reduced in higher electric resistivity.This method is not necessarily to high pure raw material, at low cost, suitable for mass production.
Detailed description of the invention
Fig. 1 is that Ca adulterates β-Ga in embodiment 12O3Crystal prototype photo
Fig. 2 is that Ca adulterates β-Ga in embodiment 12O3Crystal is infrared to penetrate spectrum
Fig. 3 is that Ca adulterates β-Ga in embodiment 12O3Crystal carrier concentration C-V test.
Specific embodiment
Below with reference to embodiment, the present invention will be further described, but not limited to this.
Embodiment 1:A=Ca, x=0.002, crystal-chemical formula is β-(Ga0.998Fe0.002)2O3
Crystal the preparation method is as follows:
(1) selection and processing of raw material
The Ga of purity 99.99% is weighed according to stoichiometric ratio2O3, purity 99.9% CaCO3, raw material is put into mixing
It is sufficiently mixed in machine 48 hours.After the completion of mixing, mixed raw material is pressed into pie with hydraulic press.Then material cake is put into corundum
It in crucible, is sintered 30 hours at 1250 DEG C, obtains calcium analysis gallium oxide polycrystal material.
(2) crystal growth
The raw material pressed is fitted into Iridium Crucible by a, carries out crystal growth using czochralski method.It is evacuated down to 1 × 10-3Pa,
It is filled with 1%O2Add 99% high-purity argon gas to an atmospheric pressure.Using mid-frequency induction heating Iridium Crucible, temperature programming keeps raw material slow
Slow fusing.
B regulates temperature of sowing, and<010>direction gallium oxide seed crystal is used slowly to contact bath surface, micro- to melt and receive neck.When
When seed crystal diameter is received carefully to 1.5mm, shouldering and isodiametric growth are carried out.The pull rate of crystal is 3mm/h.Crystal growth is to required
When size, after being gradually warmed up 10 DEG C, constant temperature 30 minutes, crystal is mentioned de-.
After c crystal growth, room temperature is cooled to the rate of 30 DEG C/h, is come out of the stove.
Fig. 1 adulterates β-Ga for the Ca obtained after cutting and polishing2O3Crystal prototype photo.The penetrating quality of crystal is higher.Fig. 2 is
Ca adulterates β-Ga2O3Crystal is infrared to penetrate spectrum, it can be seen that crystal illustrates crystal in infrared band transmitance with higher
Middle free carrier concentration is lower, and crystal lacks conducting carriers at room temperature.It is tested by high resistant tester, obtains crystal resistance
Rate is up to 2 × 10 at room temperature11Ω cm, it was demonstrated that crystal is semi-insulating crystal or high-resistance crystalline.Fig. 3 is that Ca adulterates β-
Ga2O3Crystal carrier concentration C-V test curve, crystal C-V curve are a straight line, cumulative curve do not occur, illustrate that chip is in
It is existing semi-insulating.
Embodiment 2:A=Zn, x=0.001, crystal-chemical formula is β-(Ga0.999Ca0.001)2O3
Crystal the preparation method is as follows:
(1) selection and processing of raw material
The Ga of purity 99.99% is weighed according to stoichiometric ratio2O3, purity 99.99% ZnO, raw material is put into batch mixer
In be sufficiently mixed 48 hours.After the completion of mixing, by the raw material mixed be fitted into rubber tube by etc. static pressure suppressions at charge bar.It will material
Stick is sintered 30 hours at 1300 DEG C, obtains zinc doping gallium oxide polycrystalline charge bar.
(2) crystal growth
A is fixed in the furnace of floating region by fuel rod, is evacuated down to 1 × 10-2Pa is passed through high purity oxygen gas flowing atmosphere, flow velocity
0.5L/min.Heating melts raw material slowly.
B regulates temperature of sowing, and uses<010>direction gallium oxide seed crystal induced crystal growth.Heating power is controlled, seed is worked as
When brilliant diameter is received carefully to 1mm, shouldering and isodiametric growth are carried out.The pull rate of crystal is 6mm/h, seed crystal and charge bar rotation speed
It is set as 10r/min.When crystal growth to required size, crystal and charge bar high speed are pulled.
After c crystal growth, heating power is progressively closed off, is come out of the stove.
Embodiment 3:A=Zn, x=0.002, crystal-chemical formula is β-(Ga0.998Zn0.002)2O3
Crystal the preparation method is as follows:
(1) selection and processing of raw material
According to stoichiometric ratio, to equipped with pure Ga2O399.99% ZnO powder is added in the crucible of polycrystal material.
(2) crystal growth
A places iraurite mold, carries out crystal growth using EFG technique.It is evacuated down to 1 × 10-3Pa is filled with high-purity argon gas extremely
One atmospheric pressure.Using mid-frequency induction heating Iridium Crucible, temperature programming melts raw material slowly, and to raw material, all fusing is subsequent
10 DEG C of temperature of continuing rising, constant temperature drops back to former temperature, 1-2 hour of constant temperature after 0.5 hour.
B regulates temperature of sowing, and<010>direction gallium oxide seed crystal is used slowly to contact iraurite die surface, micro- to melt and receive
Neck.When seed crystal diameter is received carefully to 1mm, shouldering and isodiametric growth are carried out.The pull rate of crystal is 15mm/h.Crystal growth is extremely
When required size, after 5 DEG C, constant temperature 30 minutes of heating, crystal is mentioned de-.
Embodiment 4:A=Ni, x=0.001, crystal-chemical formula is β-(Ga0.999Ni0.001)2O3
Crystal the preparation method is as follows:
(1) selection and processing of raw material
The Ga of purity 99.99% is weighed according to stoichiometric ratio2O3, purity 99.9% NiO.
(2) crystal growth
A places platinum-rhodium crucible and mold, carries out crystal growth using EFG technique.It is evacuated down to 1 × 10-3Pa is filled with 50%
Nitrogen and 50% oxygen are to an atmospheric pressure.Using mid-frequency induction heating, temperature programming melts raw material slowly, to raw material whole
10 DEG C of subsequent temperature of continuing rising is melted, constant temperature drops back to former temperature, 1-2 hour of constant temperature after 0.5 hour.
B regulates temperature of sowing, and<001>direction gallium oxide seed crystal is used slowly to contact iraurite die surface, micro- to melt and receive
Neck.When seed crystal diameter is received carefully to 1mm, shouldering and isodiametric growth are carried out.The pull rate of crystal is 15mm/h.Crystal growth is extremely
When required size, after 5 DEG C, constant temperature 30 minutes of heating, crystal is mentioned de-.
Embodiment 5:A=Ti, x=0.02, crystal-chemical formula is β-(Ga0.98Ti0.02)2O3
Crystal the preparation method is as follows:
(2) selection and processing of raw material
The Ga of purity 99.99% is weighed according to stoichiometric ratio2O3, purity 99.9% Ti2O3, raw material is put into mixing
It is sufficiently mixed in machine 48 hours.After the completion of mixing, mixed raw material is pressed into pie with hydraulic press.Then material cake is put into corundum
It in crucible, is sintered 30 hours at 1250 DEG C, obtains Fe2O3 doping gallium oxide polycrystal material.
(2) crystal growth
The raw material pressed is fitted into Iridium Crucible by a, carries out crystal growth using czochralski method.It is evacuated down to 1 × 10-3Pa,
It is filled with 1%O2Add 99% high-purity argon gas to an atmospheric pressure.Using mid-frequency induction heating Iridium Crucible, temperature programming keeps raw material slow
Slow fusing.
B regulates temperature of sowing, and<010>direction gallium oxide seed crystal is used slowly to contact bath surface, micro- to melt and receive neck.When
When seed crystal diameter is received carefully to 1.5mm, shouldering and isodiametric growth are carried out.The pull rate of crystal is 3mm/h.Crystal growth is to required
When size, after being gradually warmed up 10 DEG C, constant temperature 30 minutes, crystal is mentioned de-.
After c crystal growth, room temperature is cooled to the rate of 30 DEG C/h, is come out of the stove.
Comparative example 1
As described in Example 1, unlike: the doping ratio of Ca element is 1%.That is: crystal-chemical formula is β-
(Ga0.99Ca0.01)2O3。
Ca doping concentration is excessively high, and growth obtains crystal as polycrystalline and contains a large amount of crackles, and crystal is not available.
Comparative example 2
As described in Example 2, unlike: the doping ratio of Zn element is 1%.That is: crystal-chemical formula is β-
(Ga0.99Zn0.01)2O3。
Zn doping concentration is excessively high, and ZaGa is formed in crystal2O4Miscellaneous phase, crystal quality are lower.
Comparative example 3
As described in Example 4, unlike: the doping ratio of Ni element is 1%.That is: crystal-chemical formula is β-
(Ga0.99Ni0.01)2O3。
Ni doping concentration is excessively high, and due to Ni is different from Ga valence state, crystal generates a large amount of packages, furthermore coloring of crystal
Obviously, application of the crystal in terms of power device and opto-electronic device is affected.
Comparative example 5
As described in Example 2, unlike: doping Al element.That is: crystal-chemical formula is β-(Ga0.999Al0.001)2O3。
After Al element mixes crystal, the free carrier in crystal can not be reduced, and prohibit since doping causes crystal
Bandwidth increases.Additionally due to Al element radius is smaller, crystal generates a degree of distortion of lattice, and generates electronics, phonon
The thermal conductivity of the obvious crystal of scattering meeting.It is unfavorable for the heat dissipation of semiconductor devices.
Comparative example 6
As described in Example 5, unlike: doping Co element, doping ratio are constant.That is: crystal-chemical formula is β-
(Ga0.98Co0.02)2O3。
Crystal mixes Co element, rather than when Ti element.The miscellaneous phase of a large amount of CoO is generated in crystal, crystal generates serious
Wrappage, although crystal is in high resistant, crystal structure quality is greatly reduced, and is not able to satisfy device and thin film epitaxy requirement.
Through the foregoing embodiment with the comparative illustration of comparative example, the doped chemical of screening must be specific, and doping concentration is necessary
It can be only achieved the effect for reducing carrier concentration well and improving resistivity in suitable range.
Claims (7)
1. a kind of semi-insulating gallium oxide crystal, which is characterized in that the crystal molecule formula is β-(Ga1-xAx)2O3, A represent Ca, Zn,
Ti or Ni element, 0.0001≤x≤0.2.
2. semi-insulating gallium oxide crystal according to claim 1, which is characterized in that A represents Ti element, 0.005≤x≤
0.15。
3. semi-insulating gallium oxide crystal according to claim 1, which is characterized in that A represents Ca or Zn element, 0.0001≤
x≤0.01。
4. semi-insulating gallium oxide crystal according to claim 1, which is characterized in that A represents Ni element, 0.0001≤x≤
0.001。
5. the preparation method of the described in any item semi-insulating gallium oxide crystal of claim 1-4, comprises the following steps that
(1) selection and processing of raw material
Select the Ga of 99.9% or more purity2O3, doped raw material is using CaO, ZnO, Ti2O3, NiO or above-mentioned element other valence states
Oxide, 99.9% or more purity；By Ga2O3It is uniformly mixed with above-mentioned one or more kinds of doped raw materials, using hydraulic press pressure
At pie or static pressure is waited to be pressed into column charge bar；The gallium oxide polycrystal material adulterated using solid sintering technology synthesized element；Alternatively, straight
It connects to equipped with Ga2O3It is directly added into above-mentioned one or more kinds of doped raw materials in the crucible of raw material and directly carries out crystal growth；
(2) crystal growth
Raw material will be pressed to be fitted into Iridium Crucible, or fixed in the furnace of light floating region；
Select<100>,<010>and<001>direction seed crystal；
The growth for carrying out gallium oxide single crystal is grown using light float-zone method, czochralski method or EFG technique.
6. preparation method according to claim 5, which is characterized in that in step (2) crystal growth, when using light float-zone method
When growth, using pure oxygen atmosphere, oxygen atmosphere flowing velocity 0.5-6L/min.
7. preparation method according to claim 5, which is characterized in that in step (2) crystal growth, when using czochralski method or
When EFG technique is grown, grown using iraurite or the platinum pot containing 8-18% rhodium, using nitrogen atmosphere or nitrogen and oxygen
The mixed atmosphere of composition is as crystal growth atmosphere.
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Cited By (5)
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| CN112834700A (en) * | 2020-12-31 | 2021-05-25 | 杭州富加镓业科技有限公司 | Quality prediction method, preparation method and system of high-resistance gallium oxide based on deep learning and guided mode method |
| CN112853468A (en) * | 2020-12-31 | 2021-05-28 | 杭州富加镓业科技有限公司 | Conductive gallium oxide preparation method based on deep learning and heat exchange method |
| CN114108088A (en) * | 2021-11-26 | 2022-03-01 | 北京铭镓半导体有限公司 | Beta-gallium oxide crystal and growth method and application thereof |
| CN114214720A (en) * | 2021-12-15 | 2022-03-22 | 上海应用技术大学 | Bivalent metal ion doped beta-gallium oxide crystal growth fluxing agent and crystal growth method based on fluxing agent |
| WO2022141758A1 (en) * | 2020-12-31 | 2022-07-07 | 杭州富加镓业科技有限公司 | High-resistance gallium oxide mass prediction method, and preparation method and system based on deep learning and czochralski method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112834700A (en) * | 2020-12-31 | 2021-05-25 | 杭州富加镓业科技有限公司 | Quality prediction method, preparation method and system of high-resistance gallium oxide based on deep learning and guided mode method |
| CN112853468A (en) * | 2020-12-31 | 2021-05-28 | 杭州富加镓业科技有限公司 | Conductive gallium oxide preparation method based on deep learning and heat exchange method |
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| CN114108088B (en) * | 2021-11-26 | 2022-12-20 | 北京铭镓半导体有限公司 | Beta-gallium oxide crystal and growth method and application thereof |
| CN114214720A (en) * | 2021-12-15 | 2022-03-22 | 上海应用技术大学 | Bivalent metal ion doped beta-gallium oxide crystal growth fluxing agent and crystal growth method based on fluxing agent |
| CN114214720B (en) * | 2021-12-15 | 2024-01-16 | 上海应用技术大学 | Fluxing agent for growth of beta-gallium trioxide crystal doped with divalent metal ions and crystal growth method based on fluxing agent |
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