CN116356426A - Heterogeneous integrated graphical gallium oxide and preparation method thereof - Google Patents

Heterogeneous integrated graphical gallium oxide and preparation method thereof Download PDF

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CN116356426A
CN116356426A CN202310277431.1A CN202310277431A CN116356426A CN 116356426 A CN116356426 A CN 116356426A CN 202310277431 A CN202310277431 A CN 202310277431A CN 116356426 A CN116356426 A CN 116356426A
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gallium oxide
single crystal
patterned
bonding
mask layer
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韩根全
贾晓乐
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Hangzhou Research Institute Of Xi'an University Of Electronic Science And Technology
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Hangzhou Research Institute Of Xi'an University Of Electronic Science And Technology
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L29/00—Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. PN junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof  ; Multistep manufacturing processes therefor
    • H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
    • H01L29/12—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed
    • H01L29/26—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed including, apart from doping materials or other impurities, elements provided for in two or more of the groups H01L29/16, H01L29/18, H01L29/20, H01L29/22, H01L29/24, e.g. alloys
    • H01L29/267—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed including, apart from doping materials or other impurities, elements provided for in two or more of the groups H01L29/16, H01L29/18, H01L29/20, H01L29/22, H01L29/24, e.g. alloys in different semiconductor regions, e.g. heterojunctions
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    • 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
    • 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
    • C30B29/16—Oxides
    • 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
    • C30B31/00—Diffusion or doping processes for single crystals or homogeneous polycrystalline material with defined structure; Apparatus therefor
    • C30B31/20—Doping by irradiation with electromagnetic waves or by particle radiation
    • C30B31/22—Doping by irradiation with electromagnetic waves or by particle radiation by ion-implantation
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    • 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
    • C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
    • C30B33/08—Etching
    • C30B33/12—Etching in gas atmosphere or plasma
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Abstract

The invention belongs to the technical field of semiconductor power devices, and particularly discloses heterogeneous integrated graphical gallium oxide and a preparation method thereof. In the preparation method, firstly, patterning is carried out on a gallium oxide monocrystal to be bonded, and then element injection is carried out on the patterned gallium oxide monocrystal; and then bonding the gallium oxide single crystal subjected to element injection with a heterogeneous substrate single crystal, and finally annealing to bond the patterned gallium oxide single crystal onto the heterogeneous substrate to obtain the heterogeneous integrated patterned gallium oxide.

Description

Heterogeneous integrated graphical gallium oxide and preparation method thereof
Technical Field
The invention belongs to the technical field of semiconductor power devices, and particularly relates to a method for preparing heterogeneous integrated patterned gallium oxide, which can be used for manufacturing high-power devices.
Background
Gallium oxide (Ga) 2 O 3 ) Is a third generation wide band gap semiconductor material, the forbidden band width is 4.5 eV-4.9 eV, the theoretical breakdown field strength reaches 8MV/cm, and the theoretical breakdown field strength is far greater than 2.5MV/cm of silicon carbide (SiC) and 3.3MV/cm of gallium nitride (GaN). In addition, gallium oxide has a Barbally figure of merit (3214) that is 10 times that of SiC and 4 times that of GaN, and thereforeGallium oxide is very suitable for manufacturing ultra-high power devices.
Although gallium oxide materials have the advantages of large forbidden bandwidth, high breakdown electric field and the like compared with materials such as silicon carbide, gallium nitride and the like, and have great application potential in the field of power electronic power devices, the thermal conductivity of the gallium oxide materials is only one tenth of that of GaN materials and one twentieth of that of SiC materials, so that the gallium oxide devices manufactured on patterned gallium oxide substrates at present cannot effectively dissipate heat generated in the working process, extremely serious self-heating effect is generated, and the application of the gallium oxide devices in the fields of power and radio frequency is limited.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a heterogeneous integrated patterned gallium oxide and a preparation method thereof so as to obtain patterned gallium oxide with good heat conduction performance.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a method of preparing heterogeneous integrated patterned gallium oxide comprising the steps of:
(1) Providing a gallium oxide single crystal and a heterogeneous substrate single crystal to be bonded; at least one surface of each of the gallium oxide single crystal and the heterogeneous substrate single crystal is a bonding surface;
(2) Forming a mask layer on the bonding surface of the gallium oxide monocrystal, and performing graphical treatment on the mask layer to obtain a graphical mask layer; the patterned mask layer is of a mesa unit structure;
(3) Etching the gallium oxide single crystal on the bonding surface, which is not covered by the patterned mask layer, and removing the patterned mask layer to obtain the patterned gallium oxide single crystal;
(4) Performing element injection on the patterned gallium oxide single crystal, and forming an element enrichment layer parallel to a bonding surface in the patterned gallium oxide single crystal; the depth from the bonding surface of the gallium oxide single crystal to the element enrichment layer in the step (4) is less than or equal to the etched depth of the gallium oxide single crystal in the step (3);
(5) Bonding the bonding surface of the patterned gallium oxide monocrystal with the bonding surface of the heterogeneous substrate monocrystal to obtain a composite structure;
(6) And annealing the composite structure to break the patterned gallium oxide monocrystal at the element enrichment layer, so as to finally obtain the heterogeneous integrated patterned gallium oxide.
Optionally, in step (1), the gallium oxide single crystal and the hetero-substrate single crystal are 1 μm to 1mm in thickness and 2 inches to 12 inches in size, respectively.
Optionally, in step (1), the heterogeneous substrate single crystal includes at least one of a silicon single crystal, a silicon carbide single crystal, and a diamond single crystal.
Optionally, in step (2), the method for forming the mask layer includes at least one of Chemical Vapor Deposition (CVD), physical Vapor Deposition (PVD), atomic Layer Deposition (ALD), magnetron sputtering (sputtering), spin coating.
Optionally, in the step (2), the thickness of the mask layer is 50nm-1000nm.
In the step (2), the mask layer is made of Photoresist (PR) or silicon dioxide (SiO 2 ) Silicon nitride (Si) 3 N 4 ) At least one of them.
Optionally, in step (2), the patterning method includes wet etching.
Optionally, in the step (2), the minimum dimension of the mesa unit structure is greater than or equal to 1 μm, and a gap is formed between adjacent mesa unit structures, and the gap is less than or equal to 10 μm.
Optionally, in step (2), the mesa unit structures are regularly arranged.
Optionally, in step (3), the method of etching treatment includes at least one of inductively coupled plasma etching (ICP) and Reactive Ion Etching (RIE).
Optionally, in step (3), the method for removing the patterned mask layer includes soaking with a buffered oxide etching solution (BOE solution).
Optionally, in step (4), the type of the element implantation is at least one of hydrogen element, nitrogen element and helium element.
Optionally, in step (4), the element is implanted at an energy of 10keV-200keV, at a dose of 1×10 15 ions/cm 2 -1×10 19 ions/cm 2 The temperature is 20-200 ℃.
Optionally, in step (5), the bonding method includes at least one of surface activated bonding, metal bonding, hydrophilic bonding, and anodic bonding.
Optionally, in step (5), the bonding vacuum is 5×10 -8 Pa-5×10 -7 Pa, the pressure is 5MPa-25MPa, and the temperature is 20-30 ℃.
Optionally, in step (6), the annealing temperature is 200 ℃ to 600 ℃.
Compared with the prior art, the invention has the following beneficial effects: the heterogeneous substrate bonding technology is used for transferring the patterned gallium oxide to the heterogeneous substrate with good heat conduction performance, so that the heterogeneous integrated patterned gallium oxide is prepared, the self-heating effect of a gallium oxide device manufactured by the heterogeneous substrate integrated patterned gallium oxide can be effectively relieved, and the method has great significance for the development of future gallium oxide devices.
Drawings
FIG. 1 is a schematic flow chart of a method for preparing heterogeneous integrated patterned gallium oxide according to the present invention.
Fig. 2 is a schematic diagram of a gallium oxide wafer after deposition of a mask layer according to embodiments 1-3 of the present invention.
Fig. 3 is a schematic diagram of the embodiment 1-3 of the present invention after patterning the mask layer.
Fig. 4 is a schematic diagram of the gallium oxide wafer etched according to the embodiment 1-3 of the present invention.
Fig. 5 is a schematic diagram of a gallium oxide wafer according to example 1-3 after patterning.
Fig. 6 is a schematic diagram of the patterned gallium oxide wafer of embodiments 1-3 after specific element implantation to form a specific element enriched layer.
Fig. 7 is a schematic diagram of bonding a gallium oxide wafer with specific element implantation to a heterogeneous substrate in embodiments 1-3 of the present invention.
Fig. 8 is a schematic diagram showing separation of a gallium oxide single crystal thin film bonded to a hetero-substrate from a gallium oxide wafer in examples 1 to 3 of the present invention.
Detailed Description
The invention will be described in further detail with reference to the drawings and examples in order to make the objects and advantages of the invention more apparent.
Referring to fig. 1, the present invention provides a method for preparing heterogeneous integrated patterned gallium oxide, and the following 3 specific examples are given.
Example 1
The method for preparing the silicon-based heterogeneous integrated graphical gallium oxide by injecting hydrogen elements comprises the following steps:
(1) As shown in fig. 2, a 2-inch gallium oxide wafer and a 4-inch silicon substrate wafer to be bonded are provided, and a photoresist mask layer with the thickness of 500nm is formed on the bonding surface of the gallium oxide wafer by a spin coating method;
(2) As shown in fig. 3, the photoresist mask layer is patterned to form rectangular mesa unit structures which are regularly arranged, wherein the length and the width of each mesa unit structure are larger than 1 μm, and gaps are formed between adjacent mesa unit structures, and the gaps are not larger than 10 μm;
(3) As shown in fig. 4, the gallium oxide wafer is subjected to ICP etching treatment, and the etching depth is 500nm; soaking and removing the photoresist mask layer by using a buffer oxide etching solution (BOE solution) to obtain a patterned gallium oxide wafer, as shown in FIG. 5;
(4) As shown in FIG. 6, the bonding surface of the gallium oxide wafer was implanted with an energy of 20KeV at a dose of 1X 10 17 ions/cm 2 Forming a hydrogen element enrichment layer parallel to the bonding surface in the gallium oxide wafer, wherein the depth from the bonding surface of the gallium oxide wafer to the hydrogen element enrichment layer is 300nm;
(5) As shown in FIG. 7, the bonding technique was performed under a pressure of 10MPa and a vacuum of 1X 10 -7 Bonding the gallium oxide wafer with a heterogeneous substrate wafer under the condition of Pa to prepare a composite structure;
(6) As shown in fig. 8, the composite structure is annealed at 200 ℃, and the gallium oxide wafer is broken at the hydrogen element enrichment layer, so as to obtain the hetero-substrate integrated patterned gallium oxide.
Example 2
The method for preparing the silicon carbide-based heterogeneous integrated graphical gallium oxide by injecting nitrogen element comprises the following steps:
(a) As shown in fig. 2, a 2 inch gallium oxide wafer and a 2 inch silicon carbide substrate wafer to be bonded are provided, and a silicon dioxide mask layer with the thickness of 300nm is formed on the bonding surface of the gallium oxide wafer by a physical vapor deposition method;
(b) As shown in fig. 3, the silicon dioxide mask layer is patterned to form rectangular mesa unit structures which are regularly arranged, wherein the length and the width of each mesa unit structure are larger than 1 μm, and gaps are formed between every two adjacent mesa unit structures, and are not larger than 10 μm;
(c) As shown in fig. 4, the gallium oxide wafer was subjected to ICP etching treatment to an etching depth of 1 μm. Soaking by using a buffer oxide etching solution (BOE solution), and removing the silicon dioxide mask layer to obtain a patterned gallium oxide wafer, as shown in fig. 5;
(d) As shown in FIG. 6, the bonding surface of the gallium oxide wafer was implanted with an energy of 30KeV at a dose of 5X 10 17 ions/cm 2 Forming a nitrogen element enrichment layer parallel to the bonding surface in the gallium oxide wafer, wherein the depth from the bonding surface of the gallium oxide wafer to the nitrogen element enrichment layer is 500nm;
(e) As shown in FIG. 7, the bonding technique was performed under a pressure of 15MPa and a vacuum of 2X 10 -7 Bonding the gallium oxide wafer with a heterogeneous substrate wafer under the condition of Pa to prepare a composite structure;
(f) As shown in fig. 8, the composite structure is annealed at 350 ℃, and the gallium oxide wafer is broken at the nitrogen element enrichment layer, so as to obtain the hetero-substrate integrated patterned gallium oxide.
Example 3
Helium is injected to prepare the diamond-based heterogeneous integrated patterned gallium oxide, which comprises the following steps:
(I) As shown in fig. 2, a 2 inch gallium oxide wafer and a 2 inch diamond substrate wafer to be bonded are provided, and a silicon nitride mask layer with the thickness of 300nm is formed on the bonding surface of the gallium oxide wafer by a chemical vapor deposition method;
(II) as shown in FIG. 3, patterning the silicon nitride mask layer to form square mesa unit structures which are regularly arranged, wherein the length and the width of each mesa unit structure are larger than 1 mu m, and gaps are formed between adjacent mesa unit structures, and the gaps are not larger than 10 mu m;
(III) As shown in FIG. 4, the gallium oxide wafer was subjected to RIE etching treatment with an etching depth of 500nm. Removing the silicon nitride mask layer to obtain a patterned gallium oxide wafer, as shown in fig. 5;
(IV) As shown in FIG. 6, the bonding surface of the gallium oxide wafer was implanted with an energy of 20KeV at a dose of 1X 10 18 ions/cm 2 Forming a helium element enrichment layer parallel to the bonding surface in the gallium oxide wafer, wherein the depth from the bonding surface of the gallium oxide wafer to the helium element enrichment layer is 300nm;
(V) As shown in FIG. 7, the bonding technique was performed under a pressure of 20MPa and a vacuum of 5X 10 -7 Bonding the gallium oxide wafer with a heterogeneous substrate wafer under the condition of Pa to prepare a composite structure;
(VI) as shown in FIG. 8, annealing the composite structure at 300 ℃, wherein the gallium oxide wafer breaks at the helium element enrichment layer, so as to obtain the heterogeneous substrate integrated patterned gallium oxide.
According to the invention, the gallium oxide wafer is subjected to patterning and then is subjected to subsequent bonding, so that the stress in the gallium oxide wafer can be reduced, the phenomenon of brittle fracture of the integrated gallium oxide of the heterogeneous substrate is reduced, and the yield and reliability of the integrated gallium oxide of the heterogeneous substrate are improved.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted equally without departing from the spirit and scope of the technical solution of the present invention.

Claims (10)

1. The preparation method of the heterogeneous integrated patterned gallium oxide is characterized by comprising the following steps of:
(1) Providing a gallium oxide single crystal and a heterogeneous substrate single crystal to be bonded; at least one surface of each of the gallium oxide single crystal and the heterogeneous substrate single crystal is a bonding surface;
(2) Forming a mask layer on the bonding surface of the gallium oxide monocrystal, and performing graphical treatment on the mask layer to obtain a graphical mask layer; the patterned mask layer is of a mesa unit structure;
(3) Etching the gallium oxide single crystal on the bonding surface, which is not covered by the patterned mask layer, and removing the patterned mask layer to obtain the patterned gallium oxide single crystal;
(4) Performing element injection on the patterned gallium oxide single crystal, and forming an element enrichment layer parallel to a bonding surface in the patterned gallium oxide single crystal; the depth from the bonding surface of the gallium oxide single crystal to the element enrichment layer in the step (4) is less than or equal to the etched depth of the gallium oxide single crystal in the step (3);
(5) Bonding the bonding surface of the patterned gallium oxide monocrystal with the bonding surface of the heterogeneous substrate monocrystal to obtain a composite structure;
(6) And annealing the composite structure to break the patterned gallium oxide monocrystal at the element enrichment layer, so as to finally obtain the heterogeneous integrated patterned gallium oxide.
2. The method of claim 1, wherein in step (2), the mesa unit structure has a minimum dimension of 1 μm or more, and a gap of 10 μm or less is provided between adjacent mesa unit structures.
3. The method of preparing a heterogeneous integrated patterned gallium oxide according to claim 1 or 2, wherein in step (2), the mesa unit structures are regularly arranged.
4. The method of claim 1, wherein in step (4), the element is implanted at an energy of 10keV to 200keV, at a dose of 1 x 10 15 ions/cm 2 -1×10 19 ions/cm 2 The temperature is 20-200 ℃.
5. The method for preparing heterogeneous integrated patterned gallium oxide according to claim 1, wherein in the step (4), the type of the element implantation is at least one of hydrogen element, nitrogen element and helium element.
6. The method for preparing heterogeneous integrated patterned gallium oxide according to claim 1, wherein in step (6), the annealing temperature is 200 ℃ to 600 ℃; in the step (5), the bonding method comprises at least one of surface activation bonding, metal bonding, hydrophilic bonding and anodic bonding.
7. The method of claim 1, wherein in step (2), the mask layer is made of at least one of photoresist, silicon dioxide, and silicon nitride; in the step (2), the patterning method comprises wet etching; in the step (2), the method for forming the mask layer comprises at least one of chemical vapor deposition, physical vapor deposition, atomic layer deposition, magnetron sputtering and spin coating; in the step (2), the thickness of the mask layer is 50nm-1000nm.
8. The method for preparing heterogeneous integrated patterned gallium oxide according to claim 1, wherein in the step (3), the etching treatment method comprises at least one of inductively coupled plasma etching and reactive ion etching; in the step (1), the thickness of the gallium oxide single crystal and the thickness of the heterogeneous substrate single crystal are respectively 1 mu m-1 mm, and the sizes are respectively 2 inches-12 inches.
9. The method as claimed in claim 1The preparation method of the heterogeneous integrated patterned gallium oxide is characterized in that in the step (5), the bonding vacuum degree is 5 multiplied by 10 -8 Pa-5×10 -7 Pa, the pressure is 5MPa-25MPa, and the temperature is 20-30 ℃; in the step (1), the hetero-substrate single crystal includes at least one of a silicon single crystal, a silicon carbide single crystal, and a diamond single crystal; in the step (3), the method for removing the patterned mask layer comprises soaking by using a buffer oxide etching solution.
10. The hetero-integrated patterned gallium oxide according to any one of claims 1-9.
CN202310277431.1A 2023-03-17 2023-03-17 Heterogeneous integrated graphical gallium oxide and preparation method thereof Pending CN116356426A (en)

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