CN114836832A - Gallium oxide-doped crystal and preparation method thereof - Google Patents
Gallium oxide-doped crystal and preparation method thereof Download PDFInfo
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- 239000013078 crystal Substances 0.000 title claims abstract description 113
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 title description 6
- 229910052733 gallium Inorganic materials 0.000 title description 6
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 claims abstract description 106
- 229910001195 gallium oxide Inorganic materials 0.000 claims abstract description 106
- 239000010955 niobium Substances 0.000 claims abstract description 17
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 11
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical group [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000004020 conductor Substances 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims description 50
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims description 31
- 229910000484 niobium oxide Inorganic materials 0.000 claims description 30
- 239000000463 material Substances 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 17
- 238000000137 annealing Methods 0.000 claims description 8
- 239000011812 mixed powder Substances 0.000 claims description 8
- 238000005245 sintering Methods 0.000 claims description 8
- 239000003960 organic solvent Substances 0.000 claims description 7
- 229910005191 Ga 2 O 3 Inorganic materials 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 4
- 238000003825 pressing Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000003746 solid phase reaction Methods 0.000 claims description 3
- 229910021478 group 5 element Inorganic materials 0.000 claims 1
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 16
- 239000002994 raw material Substances 0.000 description 6
- 235000019441 ethanol Nutrition 0.000 description 5
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- 229920001343 polytetrafluoroethylene Polymers 0.000 description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 3
- 239000003574 free electron Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
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- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
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- 230000001590 oxidative effect Effects 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 230000005355 Hall effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- 229910021480 group 4 element Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
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- 238000000746 purification Methods 0.000 description 1
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- 229920006395 saturated elastomer Polymers 0.000 description 1
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- 239000000758 substrate Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
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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
- C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
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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
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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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
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- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
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Abstract
The invention discloses a gallium oxide doped crystal and a preparation method thereof. The doped gallium oxide crystal provided by the invention is an N-type conductor formed by doping gallium oxide crystal, the doping element is niobium, and the doping concentration range is less than or equal to 0.8 mol%. The invention can obtain gallium oxide crystals with high carrier concentration and high conductivity, and can obtain gallium oxide crystals with different resistivities and carrier concentrations by controlling the doping concentration.
Description
The application is divisional application of invention patent application with the invention name of doped gallium oxide crystal and a preparation method thereof, the application date of which is 3 months and 3 days in 2017 and the application number of which is 201710124917.6.
Technical Field
The invention relates to the technical field of artificial crystals, in particular to a gallium oxide doped crystal and a preparation method thereof.
Background
β-Ga 2 O 3 (gallium oxide) is a direct band gap wide band gap semiconductor material, and the band gap is about 4.8-4.9 eV. The material has the advantages of large forbidden band width, high saturated electron drift speed, high thermal conductivity, high breakdown field strength, stable chemical property and the like, is transparent from Deep Ultraviolet (DUV) to Infrared (IR), and can be used for preparing a new generation of semiconductor photoelectric devices with shorter wavelength compared with the traditional transparent conductive materials (TCOs).
Pure beta-Ga 2 O 3 The crystal exhibits semi-insulating or weaker N-type conductivity, and the improvement of beta-Ga is known at present 2 O 3 The main method for the N-type conductivity of the crystal is to dope 4-valent ions, which mainly comprise Si, Hf, Ge, Sn, Zr, Ti and the like of a fourth main group and a fourth auxiliary group. In the case of Si, the main mechanism for increasing the carrier concentration is as follows
As can be seen from the above formula, the theoretical limit capacity of 4-valent element doping for providing free electrons is about 1:1, and as the doping concentration is increased, the difficulty of crystal crystallization is increased, and the degree of conductivity increase is limited.
Disclosure of Invention
The invention aims to provide a doped gallium oxide crystal and a preparation method thereof, which can improve the conductivity of the gallium oxide crystal and obtain the gallium oxide crystal with adjustable carrier concentration and resistivity.
In order to solve the above technical problems, the present invention provides a gallium oxide-doped crystal, wherein the gallium oxide crystal is doped to form an N-type conductor, the doping element is niobium, and the doping concentration range is not more than 0.8 mol%.
Optionally, for the doped gallium oxide crystal, the gallium oxide crystal is monoclinic beta-Ga 2 O 3 And (4) crystals.
Optionally, for the doped gallium oxide crystal, the doping concentration range of niobium is 0.0001-0.8 mol%.
Optionally, for the doped gallium oxide crystal, the resistivity of the doped gallium oxide crystal is 5.5 × 10 -3 ～3.6×10 2 Omega cm, carrier concentration of 9.55 × 10 16 ～1.8×10 19 /cm 3 。
The invention also provides a preparation method of the doped gallium oxide crystal, which comprises the following steps:
providing gallium oxide powder and niobium oxide powder, wherein the proportion of niobium oxide is less than or equal to 0.8 mol%;
and mixing the gallium oxide powder and the niobium oxide powder, and then carrying out crystal growth to obtain the gallium oxide doped crystal.
Optionally, in the preparation method of the doped gallium oxide crystal, the purity of the gallium oxide powder is more than 6N, and the purity of the niobium oxide powder is more than 4N.
Optionally, in the preparation method of the doped gallium oxide crystal, the ratio of niobium oxide in the gallium oxide powder and the niobium oxide powder is 0.0001-0.8 mol%.
Optionally, for the preparation method of the doped gallium oxide crystal, the gallium oxide powder and the niobium oxide powder are uniformly mixed in an organic solvent.
Optionally, for the preparation method of the doped gallium oxide crystal, the gallium oxide powder and the niobium oxide powder are uniformly mixed in an organic solvent for 12h to 24h in a ball mill under a sealed environment.
Optionally, for the preparation method of the doped gallium oxide crystal, performing crystal growth includes:
drying the mixed powder to remove the organic solvent;
pressing the mixed powder into a material rod;
sintering to enable gallium oxide and niobium oxide to generate solid-phase reaction to form a polycrystal material;
and providing seed crystals, and growing by using the polycrystalline material to obtain the gallium oxide doped crystal.
Optionally, for the preparation method of the doped gallium oxide crystal, the drying is baking for 3 to 6 hours at 80 to 100 ℃.
Optionally, for the preparation method of the doped gallium oxide crystal, the sintering is performed in a muffle furnace at 1400-1600 ℃ for 10-20 h.
Optionally, for the preparation method of the doped gallium oxide crystal, the seed crystal is a gallium oxide crystal.
Optionally, for the preparation method of the doped gallium oxide crystal, the growth speed is 2-6 mm/h, and the rotation speed is 5-15 rpm.
The doped gallium oxide crystal and the preparation method thereof provided by the invention are characterized in that the gallium oxide crystal is doped to form an N-type conductor, the doping element is niobium, more free electrons can be provided, and the doping concentration range is less than or equal to 0.8 mol%. The invention can obtain gallium oxide crystals with high carrier concentration and high conductivity, and can obtain gallium oxide crystals with different resistivities and carrier concentrations by controlling the doping concentration.
Drawings
FIG. 1 is a flow chart of a method for preparing a doped gallium oxide crystal according to an embodiment of the present invention;
FIG. 2 is a schematic diagram showing the change of the carrier and resistivity under different doping concentrations of Nb.
Detailed Description
The doped gallium oxide crystal and the method of making the same of the present invention will now be described in greater detail with reference to the schematic drawings, in which preferred embodiments of the invention are shown, it being understood that one skilled in the art may modify the invention herein described while still achieving the advantageous effects of the invention. Accordingly, the following description should be construed as broadly as possible to those skilled in the art and not as limiting the invention.
The invention is described in more detail in the following paragraphs by way of example with reference to the accompanying drawings. Advantages and features of the present invention will become apparent from the following description and from the claims. It is to be noted that the drawings are in a very simplified form and are not to precise scale, which is merely for the purpose of facilitating and distinctly claiming the embodiments of the present invention.
The invention provides a gallium oxide-doped crystal, wherein the gallium oxide crystal is doped to form an N-type conductor, the doping element is niobium, and the doping concentration range is less than or equal to 0.8 mol%. Therefore, the invention can obtain the gallium oxide crystal with high carrier concentration and high conductivity, and can obtain the gallium oxide crystal with different resistivity and carrier concentration by controlling the doping concentration.
The main reaction mechanism of the invention is as follows:
as can be seen from the comparison of formula 2 with formula 1 in the prior art, the +5 Nb (niobium) element doping can provide more free electrons than the +4 Nb element with respect to the group IV element, thereby achieving the effect of the present invention.
The gallium oxide crystal is monoclinic beta-Ga 2 O 3 Crystal, space group is C2/m. The niobium doping concentration range may be further 0.0001 to 0.8 mol%. The resistivity of the doped gallium oxide crystal is 5.5 multiplied by 10 -3 ～3.6×10 2 Omega cm, carrier concentration of 9.55 × 10 16 ～1.8×10 19 /cm 3 . Fig. 1 shows the change of the carrier and resistivity at a part of the doping concentration of niobium.
The present invention may contain elements that the conventionally available raw materials inevitably contain during the purification process and impurities that are inevitably mixed in the process. The above elements and the above impurities are preferably 10ppm or less with respect to the entire constituent components in order to ensure that the properties of the obtained doped gallium oxide crystal are not affected.
The doped gallium oxide crystal of the present invention can be prepared by using an optical float zone method, and it is understood that those skilled in the art can appropriately select other methods to prepare the doped gallium oxide crystal based on the disclosure of the present invention, such as a czochralski method, a Bridgman method, a guided mode method, etc.
Referring to fig. 1, the method for preparing a doped gallium oxide crystal of the present invention includes:
first, step S11 is performed to provide gallium oxide (Ga) 2 O 3 ) Powder and niobium oxide (Nb) 2 O 5 ) Powder, gallium oxide in a proportion of 0.8 mol% or less, for example, 0.0001 to 0.8 mol%; preferably, the purity of the niobium oxide powder is 4N (99.99 m%) or more and the purity of the gallium oxide powder is 6N (99.9999 m%) or more in the raw materials used in order to reduce the influence of impurities as much as possible. In one embodiment, the raw material ratio of the gallium oxide powder and the niobium oxide powder is measured according to a molar ratio of 0.99999999: 0.000001, and in other embodiments, the molar ratio of the niobium oxide powder is x, and the molar ratio of the gallium oxide powder is 1-x, wherein x is greater than 0 and less than or equal to 0.008, such as 0.00001, 0.0001, 0.002, 0.005, 0.008 and the like.
Next, step S12 is performed, so that the gallium oxide powder and the niobium oxide powder are mixed and then subjected to crystal growth, to obtain a gallium oxide-doped crystal.
Step S12 specifically includes: and step S121, mixing materials. The gallium oxide powder and the niobium oxide powder can be mixed by a wet method, the used solvent and the used amount are not particularly limited, and the gallium oxide powder and the niobium oxide powder can be uniformly mixed and are easy to remove subsequently. For example, an organic solvent such as ethanol, methanol, or isopropanol is selected. In the embodiment of the invention, absolute ethyl alcohol is selected, and the gallium oxide powder and the niobium oxide powder are uniformly mixed in the ethyl alcohol in a sealed environment. In the step S121, the gallium oxide powder and the niobium oxide powder are put into a clean polytetrafluoroethylene ball mill, high-purity corundum balls are put into the clean polytetrafluoroethylene ball mill, a proper amount of absolute ethyl alcohol is poured into the clean polytetrafluoroethylene ball mill, the clean polytetrafluoroethylene ball mill is sealed and then put into a ball mill, and the materials are mixed for 12 to 24 hours, so that the gallium oxide powder and the niobium oxide powder can be uniformly mixed.
And step S122, drying. Drying the mixed powder to remove ethanol; specifically, the step can be that the ball milling pot is placed in an oven and baked for 3 to 6 hours at the temperature of 80 to 100 ℃ until the ethanol is completely volatilized. According to the actual situation, if the ethanol is agglomerated after volatilization, the agglomerated raw materials can be continuously placed in a ball mill for ball milling for about 10 minutes to grind the dried massive raw materials into powder.
And step S123, pressing the rod. Pressing the mixed powder into a material rod; specifically, the step may be to place the mixed powder into an organic mold, and press the mixed powder into a material rod by using an isostatic press.
And step S124, sintering. Sintering to enable gallium oxide and niobium oxide to perform solid-phase reaction to form a polycrystalline material; specifically, the step can be sintering for 10 to 20 hours in a muffle furnace at 1400 to 1600 ℃. In this way, water possibly existing in the material rod can be removed, so that the quality of the generated polycrystalline material is improved. For example, in one embodiment, sintering may be at 1500 ℃ for 10 hours.
And step S125, growing. And providing seed crystals, and growing by using the polycrystalline material to obtain the gallium oxide doped crystal. The growth atmosphere is inert atmosphere or oxidizing atmosphere to ensure the stable valence state of high valence ions. Specifically, for the optical float zone method, sintered polycrystalline material can be loaded into a float zone furnace as a feeding rod, gallium oxide crystals are placed below the floating zone furnace as seed crystals, and for example, the <010> direction, <100> can be selected; direction or <001 >; gallium oxide crystals of directions and the like are used as seed crystals, preferably gallium oxide crystals of <010> directions, so as to be beneficial to obtaining gallium oxide single crystals with better quality. And raising the temperature to melt the seed crystal, and then contacting the seed crystal with the feeding rod to start the growth of the crystal after the seed crystal is stabilized. The stable growth speed of the crystal is preferably 2-6 mm/h, such as 3mm/h, 4.5mm/h and the like, the rotation speed is preferably 5-15 rpm, such as 8rpm, 12rpm and the like, and the growth atmosphere in one embodiment of the invention is air. Stopping the descending of the feeding rod after the crystal growth is finished, gradually separating the melting zone through the natural descending of the lower crystal, naturally and slowly cooling to the room temperature for 1-3h, and taking out the crystal. For example, in one embodiment of the present invention, the crystal growth may be performed at a speed of 5mm/h, the rotation speed is 10rpm, and after the growth is completed, the temperature is naturally reduced to room temperature for 2 h.
The gallium oxide-doped crystal obtained by the method is complete and has no crack and uniform color.
The invention also carries out electrical property measurement on the obtained doped gallium oxide crystal. For example, regarding the doped gallium oxide crystal obtained after the molar ratio of the gallium oxide powder to the niobium oxide powder is 0.999999:0.000001, the doped gallium oxide crystal is cut into samples of 5mm × 5mm × 0.3mm (length, width and height), indium electrodes are manufactured on four corners, and then the detection is performed by using a hall effect tester, so that the conductive type of the doped gallium oxide crystal can be measured to be N type, and the carrier concentration is 2.01 × 10 18 /cm 3 Resistivity of 7.7X 10 -2 Ω · cm, further, considering that growth under an air atmosphere (or an oxidizing atmosphere) causes oxygen vacancies in the crystal, the sample can be annealed at 1000 ℃ for 3 hours under an air atmosphere to eliminate the influence of oxygen vacancies, and measurement is continued, and a carrier concentration of 9.6 × 10 can be obtained 16 /cm 3 The resistivity was 36.63. omega. cm.
As can be seen from fig. 2 and table 1 below, gallium oxide crystals having different resistivity and carrier concentration can be obtained for other raw material ratios. Wherein the doping concentration is 10 -6 And 10 -5 In the case of (2), the data are shown after annealing, doping to 0 representing pure beta-Ga 2 O 3 Crystals, as a control.
TABLE 1
As can be seen in fig. 2, the carrier concentration is higher after doping and increases substantially with increasing doping concentration, for which the carrier concentration decreases after annealing compared to before annealing, but still remains at a higher level. The resistivity after doping is lower and basically decreases with the increase of the doping concentration, after annealing, the resistivity is increased compared with that before annealing, but is still obviously improved compared with pure gallium oxide, and after annealing, the resistivity is increased and can be regulated and controlled in a larger range, so that the method has a wider application range.
Based on the parameters, the doped gallium oxide crystal provided by the invention can be applied to a plurality of fields, such as power electronic devices, optoelectronic devices, conductive substrates and the like.
In summary, the doped gallium oxide crystal provided by the present invention is an N-type conductor formed by doping gallium oxide crystal, the doping element is niobium, and the doping concentration range is not more than 0.8 mol%. The invention can obtain gallium oxide crystals with high carrier concentration and high conductivity, and can obtain gallium oxide crystals with different resistivities and carrier concentrations by controlling the doping concentration.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (9)
1. A preparation method of a doped gallium oxide crystal, the gallium oxide crystal is doped by the preparation method to form an N-type electric conductor, wherein a doping element is niobium of a V group element, and the resistivity of the doped gallium oxide crystal after annealing is 5.5 x 10 -3 ～3.6×10 2 Omega cm, the carrier concentration of the doped gallium oxide crystal after annealing is 9.55 multiplied by 10 16 ～1.8×10 19 /cm 3 The preparation method comprises the following steps:
providing gallium oxide powder and niobium oxide powder, wherein the ratio of the niobium oxide powder in the gallium oxide powder to the niobium oxide powder is 0.0001-0.8 mol%, and the niobium oxide powder is niobium pentoxide powder;
uniformly mixing the gallium oxide powder and the niobium oxide powder in an organic solvent;
and after uniformly mixing the gallium oxide powder and the niobium oxide powder, performing crystal growth to obtain a doped gallium oxide crystal, wherein the performing crystal growth comprises:
drying the mixed powder to remove the organic solvent;
pressing the mixed powder into a material rod;
sintering to enable gallium oxide and niobium oxide to perform solid-phase reaction to form a polycrystalline material;
providing seed crystals, and growing by using the polycrystalline material to obtain a doped gallium oxide crystal, wherein the molecular formula of the doped gallium oxide crystal is Ga 2(1-x) Nb 2x O 3 。
2. The method for producing a doped gallium oxide crystal according to claim 1, wherein the gallium oxide powder has a purity of 6N or more, and the niobium oxide powder has a purity of 4N or more.
3. The method for preparing a doped gallium oxide crystal according to claim 1, wherein the gallium oxide powder and the niobium oxide powder are mixed uniformly in an organic solvent in a ball mill in a sealed environment for 12h to 24 h.
4. The method for preparing a doped gallium oxide crystal according to any one of claims 1 to 3, wherein the drying is baking at 80 ℃ to 100 ℃ for 3h to 6 h.
5. The method for preparing a doped gallium oxide crystal according to any one of claims 1 to 3, wherein the sintering is carried out in a muffle furnace at 1400 ℃ to 1600 ℃ for 10h to 20 h.
6. The method for producing a doped gallium oxide crystal according to any one of claims 1 to 3, wherein the seed crystal is a gallium oxide crystal.
7. The method for preparing a doped gallium oxide crystal according to any one of claims 1 to 3, wherein the growth rate is 2 to 6mm/h and the rotation speed is 5 to 15 rpm.
8. A doped gallium oxide crystal prepared by the preparation method according to any one of claims 1 to 7, wherein the doped concentration of the group V element niobium is in the range of 0.0001 to 0.8 mol%, and the formula of the doped gallium oxide crystal is Ga 2(1-x) Nb 2x O 3 。
9. The doped gallium oxide crystal of claim 8, wherein the doped gallium oxide crystal is monoclinic β -Ga 2 O 3 And (4) crystals.
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| JP2011190127A (en) * | 2010-03-12 | 2011-09-29 | Namiki Precision Jewel Co Ltd | Gallium oxide single crystal and method for producing the same |
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| JP2011190127A (en) * | 2010-03-12 | 2011-09-29 | Namiki Precision Jewel Co Ltd | Gallium oxide single crystal and method for producing the same |
| CN103469299A (en) * | 2013-09-05 | 2013-12-25 | 大连理工大学 | Preparation method of gallium oxide-doped membrane and gallium oxide-doped membrane |
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