CN110079860A - A kind of splicing growing method of large size single crystal diamond epitaxial wafer - Google Patents
A kind of splicing growing method of large size single crystal diamond epitaxial wafer Download PDFInfo
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- CN110079860A CN110079860A CN201910247096.4A CN201910247096A CN110079860A CN 110079860 A CN110079860 A CN 110079860A CN 201910247096 A CN201910247096 A CN 201910247096A CN 110079860 A CN110079860 A CN 110079860A
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- crystal diamond
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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
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/22—Sandwich processes
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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
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/04—Diamond
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- Chemical & Material Sciences (AREA)
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- General Chemical & Material Sciences (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The present invention prepares existing defect for the splicing of large size single crystal diamond in the prior art, a kind of splicing growing method of large size single crystal diamond epitaxial wafer is provided, pass through ion implanting and isolation technics first, the single-crystal diamond epitaxial wafer of multi-disc crystal orientation strict conformance is obtained after chemical vapor deposition, then after epitaxial wafer being arranged and is bonded on substrate along consistent crystal orientation, implement planarizing processing and ion implanting, finally by obtaining large-sized single-crystal diamond epitaxial wafer after chemical vapor deposition and separation, the present invention can get 1-6 inches of single-crystal diamond epitaxial wafer, and splice the crystal quality of interface epitaxial growth without significant degradation.
Description
Technical field
The invention belongs to large size single crystal technical field of diamond preparation, and in particular to outside a kind of large size single crystal diamond
Prolong the splicing growing method of piece.
Background technique
As the basic material that electric power, electron and information technology develop, exist by the first generation semiconductor material of representative of Si
The performance of the operating voltage of device, power loss, response device speed etc. is gradually close to theoretical limit, traditional Si half
Conductor device is faced with the progressive updating replacement.Application demand in fields such as high-power, low-loss, high temperature, high frequencies promotes
The appearance of the new a collection of semiconductor material with wide forbidden band such as SiC, GaN, diamond.Compared with Si semiconductor material, the forbidden band of diamond
Width, breakdown electric field, carrier mobility, thermal conductivity are the decades of times of Si, and far more than SiC material.Therefore, diamond is partly led
Body device high-power, low-loss, high temperature, in terms of application there is more significant advantage.
The matter of utmost importance that diamond semiconductor device exploitation solves is the preparation problem of large size single crystal diamond, micro-
Wave plasma chemical vapor deposition technique is the preparation of the large size single crystal diamond for the most advantage generally acknowledged in research field
Method.Technology has generally realized 8-10 mm high-quality (1332 cm of diamond at present-1Raman peak width is less than 2.6 cm-1) epitaxial growth of single crystal diamond flag answers but due to lacking the substrate of bigger seed crystal as single-crystal diamond epitaxial growth
Preparation for developing inch grade (> 1 inch) single-crystal diamond wafer of diamond semiconductor device is still faced with numerous difficulties.
Currently, generalling use in the preparation process of large size single crystal diamond by the single-crystal diamond of smaller size
According to the method for consistent crystal orientation splicing growth to obtain larger sized single-crystal diamond, if Yamada is in its research
The splicing growing method [1,2] of 1 inch and 2 inches single-crystal diamond has been reported respectively, it was confirmed that obtains large size single crystal Buddha's warrior attendant
The feasibility of stone material splicing growth, but due to the complexity and degree of difficulty of its technology, the system of large size single crystal diamond
Standby problem is not well solved yet at present.
Bibliography
[1] “Fabrication and fundamental characterizations of tiled clones of
single-crystal diamond with 1-inch size” H. Yamada*, A. Chayahara, H.
Umezawa, N. Tsubouchi, Y. Mokuno, and S. Shikata. Diamong & Related Materials
24 (2012) 29-33.
[2] “A 2-in. mosaic wafer made of a single-crystal diamond” H. Yamada*,
A. Chayahara, Y. Mokuno, Y. Kato, and S. Shikata. Applied Physics Letters
104, 102110(2014)。
Summary of the invention
The present invention prepares existing defect for the splicing of large size single crystal diamond in the prior art, provides a kind of large scale
The splicing growing method of single-crystal diamond epitaxial wafer can get 1-6 inches of single-crystal diamond epitaxial wafer, and splice outside interface
Prolong the crystal quality of growth without significant degradation.
The present invention adopts the following technical scheme:
A kind of splicing growing method of large size single crystal diamond epitaxial wafer, comprising the following steps:
Step 1, single-crystal diamond is chosen as substrate 1, after substrate 1 is cut and polished along (100) crystal plane direction, in substrate 1
Main surface carry out ion implanting formed ion implanted layer, the ion implanted layer surface chemistry be vapor-deposited single crystal diamond
Then stone epitaxial layer 1 separates outside to get single-crystal diamond single-crystal diamond substrate 1 with epitaxial layer 1 along ion implanted layer
Prolong piece, obtains the single-crystal diamond epitaxial wafer of multi-disc crystal orientation strict conformance after repeating this step；
Step 2, step 1 gained multi-disc single-crystal diamond epitaxial wafer along (100) crystal plane direction orientations and is bonded in substrate 3
On, integral grinding and polishing treatment then are carried out to the surface of single-crystal diamond epitaxial wafer made of arrangement；
Step 3, gained single-crystal diamond epitaxial wafer is arranged as substrate 2 using step 2, carries out ion implanting in the main surface of substrate 2
Ion implanted layer is formed, in the surface chemistry vapor deposition single-crystal diamond epitaxial layer 2 of the ion implanted layer, then along ion
Implanted layer separates single-crystal diamond substrate 2 with epitaxial layer 2, outside the large size single crystal diamond for so far obtaining splicing growth
Prolong piece.
Preferably, in step 1, the substrate 1 is the non-nuclear density gauge that high temperature and high pressure method or chemical vapour deposition technique synthesize,
And dislocation density is lower than 5000/cm2Single-crystal diamond.Crystal is no more than ± 1 ° in strict accordance with (100) crystal plane direction and error
It is cut into the square crystal of sheet,
Preferably, in step 1, the polishing is required so that crystal upper and lower major surfaces roughness is no more than 5nm, and 4 sides are coarse
Degree is no more than 100nm.
Preferably, in step 1 and step 3, the ion implanting be the main surface of substrate 1 or substrate 2 injection carbon from
Son, Implantation Energy 100-300keV, implantation dosage are 1 × 1015-17ions/cm2, the injection depth of carbon ion layer is 0.1-
0.5μm。
Preferably, in step 1 and step 3, the chemical vapor deposition single-crystal diamond epitaxial layer 1 has with epitaxial layer 2
Body uses MPCVD method, operating condition are as follows: and 800-1200 DEG C of temperature, air pressure 10-14kPa, 500-
1000sccmH2, 30-60sccmCH4, 0.1-1sccmN2。
Preferably, in step 1 and step 3, the separation method of the substrate 1 and epitaxial layer 1 and substrate 2 and epitaxial layer 2
It is electrochemical erosion method, in the electrochemical erosion method, electrolyte selects such as deionized water high resistant solution, and electrode two terminates
Enter the alternating current greater than 1000V and carry out electrochemical corrosion, for removing the damage of the carbon ion between diamond substrate and epitaxial layer
Layer, until substrate is separated with epitaxial layer.
Preferably, in step 2, the substrate 3 selects surface roughness to be no more than 5nm and thermally expands system with single-crystal diamond
The close material of number, such as monocrystalline silicon piece, quartz glass plate or polycrystalline diamond flag, the integral grinding make with polishing treatment
The surface roughness of single-crystal diamond epitaxial wafer made of must arranging is no more than 2nm.
Preferably, in step 2, the bonding specifically: the titanium film layer of thickness 5-30nm is deposited on the surface of substrate 3 first,
Then multi-disc single-crystal diamond epitaxial wafer is orientated close-packed arrays, and single crystal diamond along (100) crystal plane direction on the titanium film layer
Gap maximum between stone epitaxial wafer is no more than 500 μm, and in 800-1200 DEG C of vacuum annealing 5-30min.
Preferably, the size range of the large size single crystal diamond epitaxial wafer is 1 ~ 6 inch.
Beneficial effects of the present invention are as follows:
1. under the conditions of the prior art, the epitaxial growth size of single-crystal diamond is difficult to more than 10mm, and technical solution of the present invention can be real
The preparation of existing inch grade (1-6 inches) single-crystal diamond, largely improves the dimension limit of single-crystal diamond；
2. under the conditions of the prior art, the crystal quality of the single-crystal diamond splicing interface epitaxial growth after splicing growth has not
With the degeneration of degree, technical solution of the present invention single-crystal diamond splices the crystal quality of interface epitaxial growth without significant degradation；
3. under the conditions of the prior art, there are biggish residual stress inside the single-crystal diamond after splicing growth, being easy to appear outer
Prolong the cracking of piece and be crushed, technical solution of the present invention single-crystal diamond internal residual stress is small, epitaxial wafer cracking and broken probability
It is low.
Detailed description of the invention
Fig. 1 is the process flow chart of embodiment；
Fig. 2 is 21 × 35mm obtained by embodiment2Optical microscope after single-crystal diamond splicing growth；
Fig. 3 is 21 × 35mm obtained by embodiment2Single-crystal diamond splices single-crystal diamond 1332 in ± 20 μ m of interface
cm-1Raman peak width figure.
Specific embodiment
In order to keep technical purpose of the invention, technical scheme and beneficial effects clearer, with reference to the accompanying drawing and specifically
Embodiment is further illustrated technical solution of the present invention.
The specific preparation process of the present invention as shown in Figure 1, first select chemical vapour deposition technique synthesis non-nuclear density gauge,
And dislocation density is lower than 5000/cm2Single-crystal diamond as substrate 1, substrate 1 is cut and is polished, cut surface with
(100) crystal plane direction error is no more than ± 1 °, is cut into having a size of 7 × 7mm2, the sheet square crystal of thickness 0.5mm.It is right
Substrate 1 after cutting is ground and is polished, and crystal upper and lower major surfaces roughness is no more than 5nm, 4 side roughness after polishing
No more than 100nm.
One of main surface injection carbon ion of substrate 1 after a polish forms carbon ion implantation layer, and Implantation Energy is
300keV, implantation dosage are 1 × 1017ions/cm2, injection depth is 0.3 μm.
In the ion implanting face chemical vapor deposition single-crystal diamond epitaxial layer 1 of substrate 1, using microwave plasma chemical
Vapour deposition process, sedimentary condition are as follows: 1100 DEG C of temperature, air pressure 12kPa, 700sccmH2, 30sccmCH4, 0.3sccmN2, until
Epitaxial layer 1 with a thickness of 0.5mm
Thickness preferably 0.2 ~ 0.5mm of epitaxial layer 1 of the present invention, in the present embodiment, the thickness of epitaxial layer 1 is selected specifically to
0.5mm。
Substrate 1 is separated along carbon ion implantation layer with single-crystal diamond epitaxial layer 1 using electrochemical erosion method, is electrolysed
The deionized water high resistant solution that 1:10 is mixed by volume that liquid selects the concentrated sulfuric acid and resistance to be not less than 10 megaohms, electrode two
The alternating current (voltage of alternating current preferably 1000 ~ 1500V) terminated into 1000V corrodes carbon ion damaging layer, up to substrate 1 and outside
Prolong the separation of layer 1 to get single-crystal diamond epitaxial wafer.
It repeats the above steps to obtain the 7 × 7mm of size of 15 crystal orientation strict conformances2, the single crystal diamond of thickness 0.5mm
Stone epitaxial wafer.
21 × 35mm of preferred dimension2, as substrate 3,3 surface roughness 5nm of substrate is used the monocrystalline silicon piece of thickness 1mm
The titanium film of one layer of 15nm thickness is deposited in electron beam evaporation method on substrate 3, along above-mentioned 15 of (100) high preferred orientation arrangement on titanium film
Single-crystal diamond epitaxial wafer is bonded the parting surface of epitaxial wafer with titanium film, and the gap maximum between epitaxial wafer is no more than 100 μm,
Then in 1000 DEG C of vacuum annealing 30min, it is bonded realization between monocrystalline silicon piece and single-crystal diamond epitaxial wafer.
The surface of single-crystal diamond epitaxial wafer after para-linkage carries out integral grinding and polishing, the single-crystal diamond after polishing
The surface roughness 2nm of epitaxial wafer.
, as substrate 2, to inject carbon ion through treated single-crystal diamond epitaxial wafer on 2 surface of substrate, inject energy
Amount is 300keV, and implantation dosage is 1 × 1017ions/cm2, injection depth is 0.3 μm.
In the ion implanting face chemical vapor deposition single-crystal diamond epitaxial layer 2 of substrate 2, using microwave plasma chemical
Vapour deposition process, sedimentary condition are as follows: 1100 DEG C of temperature, air pressure 12kPa, 700sccmH2, 30sccmCH4, 0.3sccmN2, until
Epitaxial layer 2 with a thickness of 0.5mm；
Thickness preferably 0.5 ~ 1.0mm of epitaxial layer 2 of the present invention, in the present embodiment, the thickness of epitaxial layer 2 is selected specifically to
0.5mm。
Single-crystal diamond substrate 2 is separated with epitaxial layer 2 along ion implanted layer using electrochemical erosion method, electrolyte
The concentrated sulfuric acid and resistance is selected to be not less than 10 megaohms of the deionized water high resistant solution that 1:10 is mixed by volume, electrode both ends
The exchange galvano-cautery carbon ion damaging layer of 1000V is accessed, until substrate 2 is separated with epitaxial layer 2 to get large size single crystal diamond
Epitaxial wafer.
As shown in Figure 2 and Figure 3, the size that splicing growth is obtained after separation is 21 × 35mm2Single-crystal diamond epitaxial wafer,
Splice 1332 cm of single-crystal diamond in ± 20 μ m of interface-1Raman peak width 2.41-2.55 cm-1, splice interface
The single-crystal diamond crystals quality of epitaxial growth is without significant degradation.
It should be noted last that: technical solution of the present invention that the above embodiments are only illustrative and not limiting is any right
The equivalent replacement and do not depart from the modification of spirit and scope of the invention or locally replace that the present invention carries out, should all cover in this hair
Within bright protective scope of the claims.
Claims (9)
1. a kind of splicing growing method of large size single crystal diamond epitaxial wafer, which comprises the following steps:
Step 1, single-crystal diamond is chosen as substrate 1, after substrate 1 is cut and polished along (100) crystal plane direction, in substrate 1
Main surface carry out ion implanting formed ion implanted layer, the ion implanted layer surface chemistry be vapor-deposited single crystal diamond
Then stone epitaxial layer 1 separates outside to get single-crystal diamond single-crystal diamond substrate 1 with epitaxial layer 1 along ion implanted layer
Prolong piece, obtains the single-crystal diamond epitaxial wafer of multi-disc crystal orientation strict conformance after repeating this step；
Step 2, step 1 gained multi-disc single-crystal diamond epitaxial wafer along (100) crystal plane direction orientations and is bonded in substrate 3
On, integral grinding and polishing treatment then are carried out to the surface of single-crystal diamond epitaxial wafer made of arrangement；
Step 3, gained single-crystal diamond epitaxial wafer is arranged as substrate 2 using step 2, carries out ion implanting in the main surface of substrate 2
Ion implanted layer is formed, in the surface chemistry vapor deposition single-crystal diamond epitaxial layer 2 of the ion implanted layer, then along ion
Implanted layer separates single-crystal diamond substrate 2 with epitaxial layer 2, outside the large size single crystal diamond for so far obtaining splicing growth
Prolong piece.
2. the splicing growing method of large size single crystal diamond epitaxial wafer according to claim 1, which is characterized in that step
In 1, the substrate 1 is the non-nuclear density gauge that high temperature and high pressure method or chemical vapour deposition technique synthesize, and dislocation density is lower than 5000/
cm2Single-crystal diamond.
3. the splicing growing method of large size single crystal diamond epitaxial wafer according to claim 1, which is characterized in that step
In 1, the polishing is required so that crystal upper and lower major surfaces roughness is no more than 5nm, and 4 side roughness are no more than 100nm.
4. the splicing growing method of large size single crystal diamond epitaxial wafer according to claim 1, which is characterized in that step
1 with step 3, and the ion implanting is to inject carbon ion, Implantation Energy 100- in the main surface of substrate 1 or substrate 2
300keV, implantation dosage are 1 × 1015-17ions/cm2, the injection depth of carbon ion layer is 0.1-0.5 μm.
5. the splicing growing method of large size single crystal diamond epitaxial wafer according to claim 1, which is characterized in that step
1 with step 3, and the chemical vapor deposition single-crystal diamond epitaxial layer 1 specifically uses microwave plasma with epitaxial layer 2
Learn vapour deposition process, operating condition are as follows: 800-1200 DEG C of temperature, air pressure 10-14kPa, 500-1000sccmH2, 30-
60sccmCH4, 0.1-1sccmN2。
6. the splicing growing method of large size single crystal diamond epitaxial wafer according to claim 1, which is characterized in that step
1 with step 3, and the separation method of the substrate 1 and epitaxial layer 1 and substrate 2 and epitaxial layer 2 is electrochemical erosion method.
7. the splicing growing method of large size single crystal diamond epitaxial wafer according to claim 1, which is characterized in that step
In 2, the substrate 3 selects surface roughness to be no more than 5nm and the material close with single-crystal diamond thermal expansion coefficient, described whole
Body grinding makes the surface roughness of single-crystal diamond epitaxial wafer made of arrangement be no more than 2nm with polishing treatment.
8. the splicing growing method of large size single crystal diamond epitaxial wafer according to claim 1, which is characterized in that step
In 2, the bonding specifically:, then will be more on the titanium film layer first in the titanium film layer of the surface of substrate 3 vapor deposition thickness 5-30nm
Piece single-crystal diamond epitaxial wafer is orientated close-packed arrays along (100) crystal plane direction, and the gap between single-crystal diamond epitaxial wafer is most
It is big to be no more than 500 μm, and in 800-1200 DEG C of vacuum annealing 5-30min.
9. the splicing growing method of large size single crystal diamond epitaxial wafer according to claim 1, which is characterized in that described
The size range of large size single crystal diamond epitaxial wafer is 1 ~ 6 inch.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110541199A (en) * | 2019-10-11 | 2019-12-06 | 山东大学 | Preparation method of high-quality SiC seed crystal with diameter of 8 inches or more |
| CN111733454A (en) * | 2020-05-20 | 2020-10-02 | 西南科技大学 | Separation method of CVD homoepitaxy diamond large single crystal based on boron-doped transition layer |
| CN111962148A (en) * | 2020-08-04 | 2020-11-20 | 中国科学院上海微系统与信息技术研究所 | Preparation method of single crystal diamond film |
| CN112164976A (en) * | 2020-09-29 | 2021-01-01 | 北京大学东莞光电研究院 | High-heat-dissipation GaN single crystal substrate and preparation method thereof |
| CN112430803A (en) * | 2020-11-16 | 2021-03-02 | 北京科技大学 | Preparation method of self-supporting ultrathin diamond film |
| CN114318531A (en) * | 2022-01-06 | 2022-04-12 | 济南金刚石科技有限公司 | Stripping method applied to MPCVD large-size diamond polycrystal |
| CN115261982A (en) * | 2022-08-01 | 2022-11-01 | 北京科技大学 | Method for growing large-size single crystal diamond based on side bonding splicing |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110541199A (en) * | 2019-10-11 | 2019-12-06 | 山东大学 | Preparation method of high-quality SiC seed crystal with diameter of 8 inches or more |
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| CN111962148A (en) * | 2020-08-04 | 2020-11-20 | 中国科学院上海微系统与信息技术研究所 | Preparation method of single crystal diamond film |
| CN112164976A (en) * | 2020-09-29 | 2021-01-01 | 北京大学东莞光电研究院 | High-heat-dissipation GaN single crystal substrate and preparation method thereof |
| CN112430803A (en) * | 2020-11-16 | 2021-03-02 | 北京科技大学 | Preparation method of self-supporting ultrathin diamond film |
| CN112430803B (en) * | 2020-11-16 | 2022-04-01 | 北京科技大学 | Preparation method of self-supporting ultrathin diamond film |
| CN114318531A (en) * | 2022-01-06 | 2022-04-12 | 济南金刚石科技有限公司 | Stripping method applied to MPCVD large-size diamond polycrystal |
| CN115261982A (en) * | 2022-08-01 | 2022-11-01 | 北京科技大学 | Method for growing large-size single crystal diamond based on side bonding splicing |
| CN115261982B (en) * | 2022-08-01 | 2024-01-26 | 北京科技大学 | Method for growing large-size monocrystalline diamond based on side bonding and splicing |
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