CN115874282A - Method for improving splicing growth quality of large-area single crystal diamond - Google Patents
Method for improving splicing growth quality of large-area single crystal diamond Download PDFInfo
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- CN115874282A CN115874282A CN202211477959.5A CN202211477959A CN115874282A CN 115874282 A CN115874282 A CN 115874282A CN 202211477959 A CN202211477959 A CN 202211477959A CN 115874282 A CN115874282 A CN 115874282A
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- 239000013078 crystal Substances 0.000 title claims abstract description 87
- 239000010432 diamond Substances 0.000 title claims abstract description 68
- 238000000034 method Methods 0.000 title claims abstract description 38
- 229910003460 diamond Inorganic materials 0.000 title claims description 65
- 239000000758 substrate Substances 0.000 claims description 49
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 24
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 20
- 229910052739 hydrogen Inorganic materials 0.000 claims description 20
- 239000001257 hydrogen Substances 0.000 claims description 20
- 238000004140 cleaning Methods 0.000 claims description 10
- 238000005498 polishing Methods 0.000 claims description 9
- 238000000259 microwave plasma-assisted chemical vapour deposition Methods 0.000 claims 2
- 230000003746 surface roughness Effects 0.000 claims 1
- 239000012535 impurity Substances 0.000 abstract description 7
- 238000005229 chemical vapour deposition Methods 0.000 abstract description 5
- 230000007547 defect Effects 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 5
- 229910017604 nitric acid Inorganic materials 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000005034 decoration Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004050 hot filament vapor deposition Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- 230000007123 defense Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
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Abstract
The invention provides a method for improving the splicing growth quality of large-area single crystal diamonds, and belongs to the technical field of crystal growth. The method comprises the steps of pre-growing in an MPCVD (microwave plasma chemical vapor deposition) device, and then selecting pre-grown samples with similar step flow growth directions for splicing growth, thereby improving the splicing efficiency, reducing the defect density in the splicing growth process, improving the stress distribution at the splicing seams and improving the crystal quality of the splicing growth. The method is simple and effective to implement, can give consideration to both growth rate and crystal quality, does not introduce other impurity atoms in the growth process, has uniform texture at the joint, gradually merges step flows, has relatively gentle integral growth surface, and obviously improves the subsequent growth quality of the integral material.
Description
Technical Field
The invention relates to the technical field of crystal growth, in particular to a method for improving the splicing growth quality of single crystal diamond.
Background
Diamond is known as a final semiconductor material due to its excellent mechanical properties, such as large forbidden bandwidth, large hole and electron mobility, effective radiation resistance, etc., and has higher speed, lower power consumption and higher intrinsic mobility than the conventional semiconductor, especially has significant advantages and huge development potential in the fields of 6G era, deep ultraviolet photoelectric devices, high-voltage high-power electronic devices, etc. in the future, and has become a hot spot of international competition. With the development of the fields of semiconductor devices, microelectronics, nuclear energy, aerospace, national defense war industry and the like, the demand of large-area single crystal diamond is more and more urgent, and the natural diamond can not meet the demand of people, so that the artificial synthesis method is hopeful to prepare the high-quality large-area single crystal diamond material.
The proposal of the mosaic splicing technology indicates a road for preparing large-area single crystal diamond, but how to solve the problems of dislocation and uneven stress distribution generated on splicing seams in the splicing process is still a hotspot of research. Shinya Ohmagari et al perform tungsten element doping by HFCVD (hot filament chemical vapor deposition) growth technology, so that edge effect is reduced in the splicing process, and the influence of growth dislocation on the uniformity of the splicing sheet is reduced.
Disclosure of Invention
The invention aims to provide a method for improving the splicing growth quality of single crystal diamond, which can reduce the defect density in the splicing growth process, improve the stress distribution at a splicing seam and improve the crystal quality of splicing growth on the premise of not introducing impurity elements.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for improving the splicing growth quality of single crystal diamond, which comprises the following steps:
placing a plurality of single crystal diamond substrates into an MPCVD device, and pre-growing single crystal diamond films on the upper surfaces to obtain a plurality of pre-grown samples; the thickness difference of any two single crystal diamond substrates in the plurality of single crystal diamond substrates is within 10 mu m;
observing the growth directions of step flows on the upper surfaces of the plurality of pre-growth samples, and selecting samples with similar growth directions of the step flows to obtain samples to be spliced; controlling the deviation included angle of the surface step flows of any two pre-growth samples in the samples to be spliced to be 0-10 degrees;
mosaic splicing is carried out on the samples to be spliced according to a mode that the step flow directions are close to each other, and spliced samples are obtained; the deviation included angle of the surface step flows of any two samples in the spliced samples is controlled to be 0-10 degrees;
and putting the spliced sample into MPCVD equipment for mosaic splicing growth.
Preferably, the conditions for pre-growth include: the growth temperature is 800-1000 ℃, the growth pressure is 120-160 torr, the hydrogen flow is 300-500 sccm, the methane flow is 2-10% of the hydrogen flow, and the growth time is 1-4 h.
Preferably, the mosaic splicing growth conditions include: the growth temperature is 800-1000 ℃, the growth pressure is 120-160 torr, the hydrogen flow is 300-500 sccm, and the methane flow is 2-10% of the hydrogen flow.
Preferably, observing the growth direction of the step flow on the upper surface of the plurality of pre-growth samples is performed under a microscope.
Preferably, the crystal planes of the upper surfaces of the plurality of single crystal diamond substrates are in the same orientation, and the crystal plane orientation of the upper surface is (100), (110) or (111); the lateral orientations are all (100); the degrees of deviation of the crystal planes of the upper surface and the side surface of the multi-piece single crystal diamond substrate are within 3 degrees.
Preferably, the height difference between any two of the spliced samples is within 3 μm.
Preferably, the distance between any two adjacent samples in the spliced sample is less than 150 μm.
Preferably, before mosaic splicing, the side surface of the sample to be spliced is polished and cleaned, so that the roughness of the side surface of the spliced sample is within 200 nm.
Preferably, before the pre-growing of the single crystal diamond film, polishing and cleaning are further performed on the plurality of single crystal diamond substrates.
The invention provides a method for improving the splicing growth quality of single crystal diamond, which comprises the following steps: placing a plurality of single crystal diamond substrates into an MPCVD device, and pre-growing single crystal diamond films on the upper surfaces to obtain a plurality of pre-grown samples; the thickness difference of any two single crystal diamond substrates in the plurality of single crystal diamond substrates is within 10 mu m; observing the growth directions of the step flows on the upper surfaces of the plurality of pre-growth samples, and selecting the samples with similar growth directions of the step flows to obtain samples to be spliced; controlling the deviation included angle of the surface step flows of any two pre-growth samples in the samples to be spliced to be 0-10 degrees; mosaic splicing is carried out on the samples to be spliced according to a mode that the step flow directions are close to each other, and spliced samples are obtained; the deviation included angle of step flow on the surfaces of any two samples in the spliced samples is controlled to be 0-10 degrees; and putting the spliced sample into MPCVD equipment for mosaic splicing growth.
The method comprises the steps of pre-growing in an MPCVD (microwave plasma chemical vapor deposition) device, and then selecting pre-grown samples with similar step flow growth directions for splicing growth, thereby improving the splicing efficiency, reducing the defect density in the splicing growth process, improving the stress distribution at the splicing seams and improving the crystal quality of the splicing growth.
The method is simple, convenient and effective, can give consideration to both growth rate and crystal quality, does not introduce other impurity atoms in the growth process, has uniform texture at the joint, gradually merges step flows, has smoother overall growth surface performance, and obviously improves the subsequent growth quality of the overall material.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a surface topography of the single crystal diamond grown by splicing in example 2.
Detailed Description
The invention provides a method for improving the splicing growth quality of single crystal diamond, which comprises the following steps:
placing a plurality of single crystal diamond substrates into an MPCVD device, and pre-growing single crystal diamond films on the upper surfaces to obtain a plurality of pre-grown samples; the thickness difference of any two single crystal diamond substrates in the plurality of single crystal diamond substrates is within 10 mu m;
observing the growth directions of step flows on the upper surfaces of the plurality of pre-growth samples, and selecting samples with similar growth directions of the step flows to obtain samples to be spliced; the deviation included angle of the step flow on the surfaces of any two pre-growth samples in the samples to be spliced is controlled to be 0-10 degrees;
mosaic splicing is carried out on the samples to be spliced according to a mode that the step flow directions are close to each other, and spliced samples are obtained; the deviation included angle of the surface step flows of any two samples in the spliced samples is controlled to be 0-10 degrees;
and putting the spliced sample into an MPCVD device for mosaic splicing growth.
The invention puts a plurality of single crystal diamond substrates into MPCVD equipment, pre-grows single crystal diamond films on the upper surface, and obtains a plurality of pre-grown samples.
The number of the single crystal diamond substrates is not specially required, and more or less single crystal diamond substrates can be selected according to the requirement. The present invention does not require the dimensions of each single crystal diamond substrate, and may be of any dimensions known in the art. In the present invention, the size of each single crystal diamond substrate is preferably the same. In the present invention, the difference in thickness between any two of the plurality of single crystal diamond substrates is within 10 μm. The invention controls the thickness of the single crystal diamond substrate to meet the conditions and ensures that mosaic splicing is finished. In the present invention, the crystal plane orientations of the upper surfaces of the plurality of pieces of single crystal diamond substrates are preferably uniform, and the crystal plane orientation of the upper surfaces is (100), (110), or (111); the lateral orientations are all (100); the degrees of deviation of the crystal planes of the upper surface and the side surface of the multi-piece single crystal diamond substrate are both preferably within 3 °. The invention controls the orientation of the multiple single crystal diamond substrates to meet the conditions, ensures that the two substrates are spliced, and realizes the transverse growth of the single crystal diamond film.
Before the pre-growth of the single crystal diamond film, the invention preferably polishes and cleans a plurality of single crystal diamond substrates. The present invention has no particular requirements for the polishing and cleaning process, and may employ polishing and cleaning processes well known in the art. The invention reduces height difference and surface impurities by polishing and cleaning. In the present invention, the cleaning is preferably performed by sequentially using a mixed solution of concentrated sulfuric acid and concentrated nitric acid at a volume ratio of 1:3, hydrofluoric acid, acetone, and alcohol. The invention has no special requirement on the concentration of the concentrated sulfuric acid and the concentrated nitric acid, and the concentrated sulfuric acid and the concentrated nitric acid which are well known in the field can be used.
In the present invention, the conditions for the pre-growth preferably include: the growth temperature is 800-1000 ℃, the growth pressure is 120-160 torr, the hydrogen flow is 300-500 sccm, the methane flow is 2-10% of the hydrogen flow, and the growth time is 1-4 h; more preferably, the growth temperature is more preferably 850 to 950 ℃; the growth pressure is more preferably 130 to 150torr; the hydrogen flow rate is more preferably 350 to 450sccm; the flow rate of the methane is preferably 3-8% of the flow rate of the hydrogen; the growth time is preferably 2 to 3 hours.
After a plurality of pre-growth samples are obtained, observing the growth directions of step flows on the upper surfaces of the pre-growth samples, and selecting samples with similar growth directions of the step flows to obtain samples to be spliced; and the deviation included angle of the step flow on the surfaces of any two pre-grown samples in the samples to be spliced is controlled to be 0-10 degrees.
The invention preferably observes the growth direction of the step flow on the upper surface of the plurality of pre-growth samples under a microscope; preferably, the photographing is carried out by measuring with an angle ruler to select samples with similar step flow growth directions.
After the samples to be spliced are obtained, the samples to be spliced are subjected to mosaic splicing according to a mode that the step flow directions are close to each other, and spliced samples are obtained.
In the invention, the distance between any two adjacent samples in the spliced samples is less than 150 μm; the height difference of any two spliced samples is within 3 mu m. Before mosaic splicing, the side surface of the sample to be spliced is polished and cleaned, so that the roughness of the side surface of the spliced sample is within 200 nm. In the invention, the included angle between the step flow directions of any two samples in the spliced samples is controlled to be 0-10 degrees.
After the spliced sample is obtained, the spliced sample is put into MPCVD equipment for mosaic splicing growth. In the present invention, the conditions for mosaic growth preferably include: the growth temperature is 800-1000 deg.C, the growth pressure is 120-160 torr, the hydrogen flow is 300-500 sccm, and the methane flow is 2-10% of the hydrogen flow. The growth temperature is more preferably 850-950 ℃; the growth pressure is more preferably 130 to 150torr; the hydrogen flow rate is more preferably 350 to 450sccm; the methane flow rate is more preferably 3 to 8% of the hydrogen flow rate. The invention has no special requirement on the growth time, and the proper growth time is selected according to the thickness of the target single crystal diamond.
FIG. 1 is a process flow diagram of the present invention. As can be seen from FIG. 1, the present invention puts a plurality of single crystal diamond substrates into MPCVD equipment, pre-grows single crystal diamond films on the upper surface, and obtains a plurality of pre-grown samples; observing the growth directions of the step flows on the upper surfaces of the plurality of pre-growth samples, and selecting the samples with similar growth directions of the step flows to obtain samples to be spliced; mosaic splicing is carried out on the samples to be spliced according to a mode that the step flow directions are close to each other, and spliced samples are obtained; and finally, putting the spliced sample into MPCVD equipment for mosaic splicing growth.
The method comprises the steps of pre-growing in an MPCVD (microwave plasma chemical vapor deposition) device, and then selecting pre-grown samples with similar step flow growth directions for splicing growth, thereby improving the splicing efficiency, reducing the defect density in the splicing growth process, improving the stress distribution at the splicing seams and improving the crystal quality of the splicing growth.
The method for improving the quality of the single crystal diamond joint growth provided by the invention is described in detail with reference to the following examples, but the method is not to be construed as limiting the scope of the invention.
Example 1
Selecting 2 single crystal diamond substrates with the crystal plane orientation of the upper surface and the lower surface of each wafer being (100), the crystal plane orientation of the side surface being (100) and the crystal plane deviation degree being within 2 degrees, polishing the upper surface and the lower surface of the selected single crystal diamond substrates, controlling the height difference to be within 10 micrometers, and sequentially cleaning by using mixed solution of concentrated sulfuric acid (18 mol/L) and concentrated nitric acid (16 mol/L), hydrofluoric acid, acetone and alcohol with the volume ratio of 1:3 to remove surface impurities.
Putting the treated substrate into an MPCVD device for pre-growth at 850 ℃, 120torr of growth pressure, 200sccm of hydrogen flow, 3% of methane concentration and 2h of growth time to obtain a plurality of pre-growth samples;
placing the pre-grown sample under a microscope to observe the growth direction of the step flow of the sample, selecting 2 single crystal diamond substrates with the step flow included angle smaller than 10 degrees to carry out side polishing, and controlling the side roughness to be smaller than 200nm;
selecting 2 processed single crystal diamond substrates, cleaning, then placing the substrates in order according to a mode that the growth directions of step flows are similar, controlling the distance between any two single crystal diamonds to be less than 150 mu m, using the substrates as splicing substrates, and placing the substrates into MPCVD (multi-phase plasma chemical vapor deposition) for mosaic splicing growth; the growth temperature is controlled at 900 ℃, the growth pressure is 120torr, the hydrogen flow is controlled at 600sccm, the methane concentration is 5%, and the growth time is 24h.
Example 2
Selecting 4 monocrystalline diamond substrates with crystal face orientations of the upper surface and the lower surface of the sheet and side surfaces of the sheet being (100) and crystal face deviation degree within 3 degrees, polishing the upper surface and the lower surface of the selected monocrystalline diamond substrates, controlling the height difference within 10 mu m, and sequentially cleaning by using a mixed solution of concentrated sulfuric acid (18 mol/L) and concentrated nitric acid (16 mol/L), hydrofluoric acid, acetone and alcohol with a volume ratio of 1:3 to remove surface impurities;
putting the processed substrate into an MPCVD device for pre-growth at the same time, wherein the growth temperature is controlled at 900 ℃, the growth pressure is 140torr, the hydrogen flow is controlled at 400sccm, the methane concentration is 2%, and the growth time is 2h;
placing the pre-grown sample under a microscope to observe the growth direction of the sample step flow, selecting 4 single crystal diamond substrates with the step flow included angle smaller than 10 degrees for side polishing, controlling the side roughness to be smaller than 200nm,
cleaning 4 single crystal diamond substrates which are selected and processed, then placing the substrates in order according to a mode that the growth directions of step flows are close, controlling the distance between any two single crystal diamonds to be less than 150 mu m, using the substrates as a splicing substrate, placing the substrates into MPCVD (multi-phase plasma chemical vapor deposition) for mosaic splicing growth, controlling the growth temperature to be 950 ℃, the growth pressure to be 140torr, controlling the hydrogen flow to be 600sccm, controlling the methane concentration to be 5% and controlling the growth time to be 24h.
FIG. 2 is a surface topography of the single crystal diamond grown by tiling of example 2. The 5 pictures in fig. 2 represent the center position of the final sample and the 4 positions where the splice seam exists two by two, respectively. As can be seen from FIG. 2, the method of the present invention can reduce the defect density in the splicing growth process without introducing impurity elements, the texture of the joint is uniform, the step flows are gradually merged, the integral growth surface is more gentle, and the quality of the crystal grown by splicing is improved.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (9)
1. A method for improving the splicing growth quality of single crystal diamond is characterized by comprising the following steps:
placing a plurality of single crystal diamond substrates into an MPCVD device, and pre-growing single crystal diamond films on the upper surfaces to obtain a plurality of pre-grown samples; the thickness difference of any two single crystal diamond substrates in the plurality of single crystal diamond substrates is within 10 mu m;
observing the growth directions of the step flows on the upper surfaces of the plurality of pre-growth samples, and selecting the samples with similar growth directions of the step flows to obtain samples to be spliced; controlling the deviation included angle of the surface step flows of any two pre-growth samples in the samples to be spliced to be 0-10 degrees;
mosaic splicing is carried out on the samples to be spliced according to a mode that the step flow directions are close to each other, and spliced samples are obtained; the deviation included angle of the surface step flows of any two samples in the spliced samples is controlled to be 0-10 degrees;
and putting the spliced sample into an MPCVD device for mosaic splicing growth.
2. The method of claim 1, wherein the pre-growth conditions comprise: the growth temperature is 800-1000 ℃, the growth pressure is 120-160 torr, the hydrogen flow is 300-500 sccm, the methane flow is 2-10% of the hydrogen flow, and the growth time is 1-4 h.
3. The method according to claim 1, wherein the conditions for mosaic growth comprise: the growth temperature is 800-1000 deg.C, the growth pressure is 120-160 torr, the hydrogen flow is 300-500 sccm, and the methane flow is 2-10% of the hydrogen flow.
4. The method of claim 1, wherein observing the growth direction of the step flow on the upper surface of the plurality of pre-grown samples is performed under a microscope.
5. The method according to claim 1, wherein the plurality of single crystal diamond substrates have a uniform orientation of upper surface crystal planes, the orientation of the upper surface crystal planes being (100), (110) or (111); the lateral orientations are all (100); the degrees of deviation of the crystal planes of the upper surface and the side surface of the multi-piece single crystal diamond substrate are within 3 degrees.
6. The method of claim 1, wherein the difference in height between any two of the spliced samples is within 3 μ ι η.
7. The method of claim 1, wherein the distance between any two adjacent samples in the stitched sample is less than 150 μ ι η.
8. The method according to claim 1, wherein before mosaic splicing, the side surfaces of the samples to be spliced are polished and cleaned so that the side surface roughness of the spliced samples is within 200 nm.
9. The method according to claim 1, wherein before pre-growing the single crystal diamond film, polishing and cleaning the plurality of single crystal diamond substrates are further performed.
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| CN110184653A (en) * | 2019-06-04 | 2019-08-30 | 北京科技大学 | A method of improving large size single crystal diamond seam quality |
| CN113463192A (en) * | 2021-07-02 | 2021-10-01 | 吉林大学 | Method for splicing and growing diamond single crystal |
| WO2021200203A1 (en) * | 2020-03-30 | 2021-10-07 | アダマンド並木精密宝石株式会社 | Diamond crystal substrate and method for producing diamond crystal substrate |
| CN114032613A (en) * | 2021-10-14 | 2022-02-11 | 吉林大学 | Method for improving quality of joint seam of diamond monocrystal grown by splicing method |
| CN114150376A (en) * | 2021-10-14 | 2022-03-08 | 吉林大学 | Large-size single crystal diamond splicing growth method |
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- 2022-11-23 CN CN202211477959.5A patent/CN115874282A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110184653A (en) * | 2019-06-04 | 2019-08-30 | 北京科技大学 | A method of improving large size single crystal diamond seam quality |
| WO2021200203A1 (en) * | 2020-03-30 | 2021-10-07 | アダマンド並木精密宝石株式会社 | Diamond crystal substrate and method for producing diamond crystal substrate |
| CN113463192A (en) * | 2021-07-02 | 2021-10-01 | 吉林大学 | Method for splicing and growing diamond single crystal |
| CN114032613A (en) * | 2021-10-14 | 2022-02-11 | 吉林大学 | Method for improving quality of joint seam of diamond monocrystal grown by splicing method |
| CN114150376A (en) * | 2021-10-14 | 2022-03-08 | 吉林大学 | Large-size single crystal diamond splicing growth method |
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