CN113564701A - Method for processing monocrystal diamond seed crystal - Google Patents
Method for processing monocrystal diamond seed crystal Download PDFInfo
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- CN113564701A CN113564701A CN202110775318.7A CN202110775318A CN113564701A CN 113564701 A CN113564701 A CN 113564701A CN 202110775318 A CN202110775318 A CN 202110775318A CN 113564701 A CN113564701 A CN 113564701A
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- 239000013078 crystal Substances 0.000 title claims abstract description 125
- 239000010432 diamond Substances 0.000 title claims abstract description 57
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000012545 processing Methods 0.000 title claims abstract description 18
- 230000007547 defect Effects 0.000 claims abstract description 42
- 238000009616 inductively coupled plasma Methods 0.000 claims abstract description 31
- 238000004140 cleaning Methods 0.000 claims abstract description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 76
- 239000007789 gas Substances 0.000 claims description 57
- 230000001590 oxidative effect Effects 0.000 claims description 48
- 229910052786 argon Inorganic materials 0.000 claims description 38
- 230000010287 polarization Effects 0.000 claims description 28
- 230000005284 excitation Effects 0.000 claims description 10
- 239000011248 coating agent Substances 0.000 claims description 9
- 238000000576 coating method Methods 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 230000003213 activating effect Effects 0.000 claims description 5
- 239000000460 chlorine Substances 0.000 claims description 5
- 229910052801 chlorine Inorganic materials 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 229910052681 coesite Inorganic materials 0.000 claims description 3
- 229910052906 cristobalite Inorganic materials 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 229910052682 stishovite Inorganic materials 0.000 claims description 3
- 229910052905 tridymite Inorganic materials 0.000 claims description 3
- 238000000259 microwave plasma-assisted chemical vapour deposition Methods 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 description 5
- 238000005498 polishing Methods 0.000 description 5
- 230000008878 coupling Effects 0.000 description 4
- 238000010168 coupling process Methods 0.000 description 4
- 238000005859 coupling reaction Methods 0.000 description 4
- 230000002950 deficient Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000001939 inductive effect Effects 0.000 description 4
- 238000001237 Raman spectrum Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 238000003698 laser cutting Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000004439 roughness measurement Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
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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
- C30B25/18—Epitaxial-layer growth characterised by the substrate
- C30B25/186—Epitaxial-layer growth characterised by the substrate being specially pre-treated by, e.g. chemical or physical means
-
- 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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- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention provides a method for processing single crystal diamond seed crystals, which solves the problem of surface defect enrichment of the seed crystals in the existing MPCVD growth by cleaning the single crystal diamond seed crystals, preparing a shielding shelter, placing a sample according to certain requirements and then processing the sample by inductively coupled plasma, and can effectively improve the quality of epitaxially grown diamond.
Description
Technical Field
The present invention relates to a method of treating a single crystal diamond seed.
Background
The single crystal diamond has high hardness, high thermal conductivity, excellent optical transmittance, radiation resistance and corrosion resistance, and is widely applied to the fields of precision machining, high-frequency communication, aerospace and the like. The diamond prepared by the method has more impurities, higher defect density, poorer quality and small size, and cannot meet the related application requirements, so that the HPHT diamond has narrower application range, is downstream in the industry, has low profit and low competitiveness.
Compared with the prior art, the microwave plasma-assisted chemical vapor deposition (MPCVD) method is the currently accepted best method for preparing the large-size single-crystal diamond, and the single-crystal diamond prepared by the method has the advantages of low impurity concentration, wide transmission waveband, low defect density, large size and controllable growth rate. When the MPCVD method is used for growing CVD diamond, a single-crystal HPHT or natural diamond piece is mostly used as a seed crystal for growing. Single crystal diamond seeds require pre-growth processing, but because of the extreme hardness and wear resistance of diamond, high power lasers must be used to cut the stone. The high heat effect of the laser leads to severe graphitization and amorphous phase on the cut surface, so that a polishing process is also required. Mechanical polishing can remove the graphite and amorphous phase layers produced by laser processing to a large extent, but can cause a large number of defects and dislocations on the surface of the seed crystal after processing. Epitaxial growth is carried out on the seed crystal rich in defects, grown crystal lattices can continue and amplify the original defects, so that the grown CVD diamond contains a large number of defects, the quality of the material is seriously deteriorated, even a single crystal phase can not grow, and the reliability of material preparation and the yield of products are influenced.
Disclosure of Invention
The invention provides a method for processing single crystal diamond seed crystals, which solves the problem of surface defect enrichment of the seed crystals in the existing MPCVD growth by cleaning the single crystal diamond seed crystals, preparing a shielding shelter, placing a sample according to certain requirements and then processing the sample by inductively coupled plasma, and can effectively improve the quality of epitaxially grown diamond.
A method of processing a single crystal diamond seed comprising the steps of:
firstly, cleaning monocrystalline diamond seed crystals:
under the condition that the ultrasonic power is 500W-1000W, sequentially placing a plurality of monocrystalline diamond seed crystals in acetone, deionized water and absolute ethyl alcohol, respectively cleaning for 20 min-30 min, and then drying in a vacuum drying oven at the temperature of 30-70 ℃ to obtain clean seed crystals;
secondly, preparing a shielding shelter:
shielding the part which is not required to be processed on the clean seed crystal by using an oxide coating, and leaving the surface defect part exposed to obtain the seed crystal shielded and masked;
thirdly, placing a sample:
placing a plurality of seed crystals of the shielding shelter on a cabin sample tray of the inductively coupled plasma equipment in order, wherein the distance between the seed crystals of each shielding shelter is 20-50 mm;
fourthly, closing the cabin:
the sample platform is moved into the cabin, and the cabin door of the cabin body is closed;
fifthly, vacuumizing:
after closing the cabin, vacuumizing the cabin body to make the vacuum degree in the cabin body reach 1.0 multiplied by 10-6mbar～1.0×10- 5mbar；
Sixthly, inductively coupled plasma treatment:
firstly, starting a program, introducing argon, setting the flow of the argon to be 10 sccm-100 sccm, enabling the air pressure of a cabin body to be 0.5 Pa-30 Pa, starting an excitation power supply, and activating inductively coupled plasma;
secondly, adjusting the air pressure of the cabin body to be 3-40 Pa, and adjusting the incident power of the plasma to be 200-800W, so that the inductively coupled plasma reaches a preheating state;
thirdly, controlling the seed crystal temperature of the shielding shelter to be 400K-900K;
opening an oxidizing gas valve, introducing oxidizing gas, setting the flow rate of the oxidizing gas to be 2 sccm-40 sccm, keeping the pressure in the chamber to be 2 Pa-50 Pa, and after the oxidizing gas and the argon plasma atmosphere are uniformly mixed, adjusting the incident power of the plasma to be 300W-2200W and the polarization power to be 300W-2200W so that the inductively coupled plasma reaches a working state;
the oxidizing gas is oxygen or chlorine;
fifthly, processing for 1h to 50h under the conditions that the argon flow is 10sccm to 100sccm, the oxidizing gas flow is 2sccm to 40sccm, the pressure in the cabin is 2Pa to 50Pa, the plasma incident power is 300W to 2200W, the polarization power is 300W to 200W, and the seed crystal temperature of the shielding shelter is 400K to 900K;
closing the oxidizing gas valve and stopping introducing the oxidizing gas;
keeping the argon flow at 1 sccm-100 sccm, reducing the plasma incident power and the polarization power at the speed of 100-200W/min until the plasma incident power and the polarization power are respectively reduced to be lower than 100W, and cooling the treated seed crystal to room temperature;
eighthly, closing the excitation power supply and extinguishing plasma glow;
ninthly, stopping introducing the argon gas, and vacuumizing the cabin;
and opening the cabin to take out a sample to finish the method for treating the surface defects of the single crystal diamond seed crystal by using the inductive coupling plasma technology.
The invention has the beneficial effects that:
1. the method treats the surface of the seed crystal through the bombardment effect of the inductively coupled plasma, and solves the problems that effective mechanical polishing is difficult to carry out due to the extremely high hardness of diamond, and even defects are further introduced in the polishing;
2. selectively exposing the defective part of the seed crystal surface through the oxide coating as a shielding mask and treating the defective part by plasma bombardment treatment;
3. the uniformity of the inductively coupled plasma can reach the nanometer level, so that the high uniformity of the treated part is ensured;
4. the treated seed crystal has greatly raised crystal quality and use reliability owing to the treatment defect.
The invention is used for a method for processing the surface defects of the single crystal diamond seed crystal by utilizing the inductive coupling plasma technology.
Drawings
FIG. 1 is a photograph of a single crystal diamond seed prior to treatment of a surface defect;
FIG. 2 is a photograph of a single crystal diamond seed crystal treated for surface defects prepared in example one;
FIG. 3 is a photograph of an untreated surface defect single crystal diamond seed after growing CVD diamond;
FIG. 4 is a photograph of a single crystal diamond seed crystal treated for surface defects prepared in example one after growth of CVD diamond;
fig. 5 is a raman spectrum, 1 is a single crystal diamond seed crystal without surface defects treated, and 2 is a single crystal diamond seed crystal with surface defects treated prepared in example one.
FIG. 6 is an atomic force microscope test of a single crystal diamond seed crystal treated for surface defects, showing a roughness measurement of 1.4nm, indicating a uniformity of 1 nanometer after treatment.
Detailed Description
The technical solution of the present invention is not limited to the specific embodiments listed below, and includes any combination of the specific embodiments.
The first embodiment is as follows: a method of processing a single crystal diamond seed according to this embodiment includes the steps of:
firstly, cleaning monocrystalline diamond seed crystals:
under the condition that the ultrasonic power is 500W-1000W, sequentially placing a plurality of monocrystalline diamond seed crystals in acetone, deionized water and absolute ethyl alcohol, respectively cleaning for 20 min-30 min, and then drying in a vacuum drying oven at the temperature of 30-70 ℃ to obtain clean seed crystals;
secondly, preparing a shielding shelter:
shielding the part which is not required to be processed on the clean seed crystal by using an oxide coating, and leaving the surface defect part exposed to obtain the seed crystal shielded and masked;
thirdly, placing a sample:
placing a plurality of seed crystals of the shielding shelter on a cabin sample tray of the inductively coupled plasma equipment in order, wherein the distance between the seed crystals of each shielding shelter is 20-50 mm;
fourthly, closing the cabin:
the sample platform is moved into the cabin, and the cabin door of the cabin body is closed;
fifthly, vacuumizing:
after closing the cabin, vacuumizing the cabin body to make the vacuum degree in the cabin body reach 1.0 multiplied by 10-6mbar～1.0×10- 5mbar；
Sixthly, inductively coupled plasma treatment:
firstly, starting a program, introducing argon, setting the flow of the argon to be 10 sccm-100 sccm, enabling the air pressure of a cabin body to be 0.5 Pa-20 Pa, starting an excitation power supply, and activating inductively coupled plasma;
secondly, adjusting the air pressure of the cabin body to be 3-40 Pa, and adjusting the incident power of the plasma to be 200-800W, so that the inductively coupled plasma reaches a preheating state;
thirdly, controlling the seed crystal temperature of the shielding shelter to be 400K-900K;
opening an oxidizing gas valve, introducing oxidizing gas, setting the flow rate of the oxidizing gas to be 2 sccm-40 sccm, keeping the pressure in the chamber to be 2 Pa-50 Pa, and after the oxidizing gas and the argon plasma atmosphere are uniformly mixed, adjusting the incident power of the plasma to be 300W-2200W and the polarization power to be 300W-2200W so that the inductively coupled plasma reaches a working state;
the oxidizing gas is oxygen or chlorine;
fifthly, processing for 1h to 50h under the conditions that the argon flow is 10sccm to 100sccm, the oxidizing gas flow is 2sccm to 40sccm, the pressure in the cabin is 2Pa to 50Pa, the plasma incident power is 300W to 2200W, the polarization power is 300W to 2200W and the seed crystal temperature of the shielding shelter is 400K to 900K;
closing the oxidizing gas valve and stopping introducing the oxidizing gas;
keeping the argon flow at 10-100 sccm, reducing the plasma incident power and the polarization power at the speed of 100-200W/min until the plasma incident power and the polarization power are respectively reduced to be lower than 100W, and cooling the treated seed crystal to room temperature;
eighthly, closing the excitation power supply and extinguishing plasma glow;
ninthly, stopping introducing the argon gas, and vacuumizing the cabin;
and opening the cabin to take out a sample to finish the method for treating the surface defects of the single crystal diamond seed crystal by using the inductive coupling plasma technology.
In the second step of the embodiment, the oxide coating is used for shielding the parts of the seed crystals which do not need to be treated, only the parts which need to be treated are left to be exposed, and the specific treatment part is determined according to the distribution condition of the defects on the surfaces of the diamonds.
The beneficial effects of the embodiment are as follows: 1. the embodiment treats the surface of the seed crystal through the bombardment effect of the inductively coupled plasma, and solves the problems that effective mechanical polishing is difficult to carry out due to the extremely high hardness of diamond, and even defects are further introduced in the polishing;
2. selectively exposing the defective part of the seed crystal surface through the oxide coating as a shielding mask and treating the defective part by plasma bombardment treatment;
3. the uniformity of the inductively coupled plasma can reach the nanometer level, so that the high uniformity of the treated part is ensured;
4. the treated seed crystal has greatly raised crystal quality and use reliability owing to the treatment defect.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: opening a procedure, introducing argon, setting the flow of the argon to be 10 sccm-100 sccm, enabling the air pressure of the cabin to be 0.5 Pa-30 Pa, starting an excitation power supply, and activating the inductively coupled plasma. The rest is the same as the first embodiment.
The third concrete implementation mode: this embodiment is different from the first or second embodiment in that: sixthly, adjusting the incident power of the plasma to 200-1000W. The other is the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: and sixthly, controlling the seed crystal temperature of the shielding shelter to be 400-900K. The others are the same as the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: in the sixty-four step, when the oxidizing gas is oxygen, the flow rate of the oxidizing gas is set to be 10 sccm-50 sccm, the pressure in the chamber is kept to be 2 Pa-50 Pa, and after the oxidizing gas and the argon plasma atmosphere are uniformly mixed, the incident power of the plasma is adjusted to be 1000W-2000W and the polarization power is adjusted to be 1000W-2200W. The rest is the same as the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is: in the sixty-four step, when the oxidizing gas is chlorine, the flow rate of the oxidizing gas is set to be 2 sccm-40 sccm, the pressure in the chamber is kept to be 2 Pa-50 Pa, and after the oxidizing gas and the argon plasma atmosphere are uniformly mixed, the incident power of the plasma is adjusted to be 800W-2000W and the polarization power is adjusted to be 800W-2000W. The rest is the same as the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: in the sixth fifth step, the seed crystal is treated for 10 to 50 hours under the conditions that the flow of argon is 1 to 50sccm, the flow of oxidizing gas is 10 to 50sccm, the pressure in the cabin is 2 to 50Pa, the incident power of plasma is 1000 to 2200W, the polarization power is 1000 to 2200W and the temperature of the seed crystal for shielding the mask is 400 to 900K. The others are the same as the first to sixth embodiments.
The specific implementation mode is eight: the present embodiment differs from one of the first to seventh embodiments in that: in the sixth fifth step, the seed crystal is treated for 10 to 50 hours under the conditions that the flow of argon is 1 to 50sccm, the flow of oxidizing gas is 10 to 50sccm, the pressure in the cabin is 2 to 50Pa, the incident power of plasma is 800 to 2000W, the polarization power is 800 to 2000W and the temperature of the seed crystal of the shielding mask is 300 to 800K. The rest is the same as the first to seventh embodiments.
The specific implementation method nine: the present embodiment differs from the first to eighth embodiments in that: sixthly, keeping the argon flow at 10-50 sccm, reducing the plasma incident power and the polarization power at a speed of 10-200W/min until the plasma incident power and the polarization power are respectively reduced to be lower than 100W, and cooling the treated seed crystal to room temperature. The other points are the same as those in the first to eighth embodiments.
The detailed implementation mode is ten: the present embodiment differs from one of the first to ninth embodiments in that: the oxide coating in the second step is SiO2. The other points are the same as those in the first to ninth embodiments.
The following examples were used to demonstrate the beneficial effects of the present invention:
the first embodiment is as follows:
a method for processing the surface defects of the monocrystalline diamond seed crystal by utilizing the inductively coupled plasma technology is carried out according to the following steps:
firstly, cleaning monocrystalline diamond seed crystals:
sequentially placing a plurality of monocrystalline diamond seed crystals in acetone, deionized water and absolute ethyl alcohol under the condition that the ultrasonic power is 300W, respectively cleaning for 10min, and then drying in a vacuum drying oven at the temperature of 60 ℃ to obtain clean seed crystals;
secondly, preparing a shielding shelter:
by SiO2The oxide coating shields the part which is not required to be processed on the clean seed crystal, and the part with surface defects is left to be exposed to obtain the seed crystal shielded;
thirdly, placing a sample:
placing a plurality of seed crystals of the shielding shelter on a cabin sample tray of the inductively coupled plasma equipment in order, wherein the distance between the seed crystals of each shielding shelter is 30 mm;
fourthly, closing the cabin:
the sample platform is moved into the cabin, and the cabin door of the cabin body is closed;
fifthly, vacuumizing:
after closing the cabin, vacuumizing the cabin body to make the vacuum degree in the cabin body reach 5.0 multiplied by 10-6mbar；
Sixthly, inductively coupled plasma treatment:
firstly, starting a program, introducing argon, setting the flow of the argon to be 10sccm, enabling the air pressure of a cabin body to be 10Pa, starting an excitation power supply, and activating inductively coupled plasma;
secondly, adjusting the air pressure of the cabin body to be 10Pa, and adjusting the incident power of the plasma to be 500W, so that the inductively coupled plasma reaches a preheating state;
thirdly, controlling the seed crystal temperature of the shielding shelter to be 800K;
opening an oxidizing gas valve, introducing oxidizing gas, setting the flow of the oxidizing gas to be 10sccm, keeping the pressure in the chamber to be 10Pa, and after the oxidizing gas and the argon plasma atmosphere are uniformly mixed, adjusting the incident power of the plasma to be 1000W and the polarization power to be 1000W so that the inductively coupled plasma reaches a working state;
the oxidizing gas is oxygen;
fifthly, processing for 10 hours under the conditions that the flow of argon gas is 10sccm, the flow of oxidizing gas is 10sccm, the pressure in the cabin is 10Pa, the incident power of plasma is 1000W, the polarization power is 1000W and the temperature of seed crystals for shielding the shelter is 800K;
closing the oxidizing gas valve and stopping introducing the oxidizing gas;
keeping the argon flow at 10sccm, reducing the plasma incident power and the polarization power at a speed of 100W/min until the plasma incident power and the polarization power are respectively reduced to be lower than 100W, and cooling the treated seed crystal to room temperature;
eighthly, closing the excitation power supply and extinguishing plasma glow;
ninthly, stopping introducing the argon gas, and vacuumizing the cabin;
and opening the cabin to take out a sample at the R part to obtain the single crystal diamond seed crystal for treating the surface defect, namely completing the method for treating the surface defect of the single crystal diamond seed crystal by using the inductive coupling plasma technology.
FIG. 1 is a photograph of a single crystal diamond seed prior to treatment of a surface defect; as can be seen, the surface is dark and uneven, indicating defects caused by laser cutting;
FIG. 2 is a photograph of a single crystal diamond seed crystal treated for surface defects prepared in example one; as can be seen, the surface is white and even, indicating that the defect has been treated;
FIG. 3 is a photograph of an untreated surface defect single crystal diamond seed after growing CVD diamond; as can be seen, the surface is significantly polycrystallized;
FIG. 4 is a photograph of a single crystal diamond seed crystal treated for surface defects prepared in example one after growth of CVD diamond; as can be seen from the figure, the surface is bright and smooth, and is a typical single crystal growth morphology.
Fig. 5 is a raman spectrum, 1 is a single crystal diamond seed crystal without surface defects treated, and 2 is a single crystal diamond seed crystal with surface defects treated prepared in example one. As can be seen from the figure, after the defects were treated, the grown layer was a high-quality single crystal, and polycrystalline and amorphous characteristic peaks appeared in the untreated defects.
According to the embodiment, the exposed part with the defect on the surface of the seed crystal is removed through the bombardment treatment effect of the inductively coupled plasma, so that the quality and the reliability of the crystal are improved, the crystal has more excellent material properties and application values, and the defect-free high-quality monocrystalline diamond epitaxial layer can be more easily grown by removing the defect seed crystal through the inductively coupled plasma according to the appearance after CVD growth and the Raman spectrum result.
Claims (10)
1. A method of processing a single crystal diamond seed, the method comprising the steps of:
firstly, cleaning monocrystalline diamond seed crystals:
under the condition that the ultrasonic power is 500W-1000W, sequentially placing a plurality of monocrystalline diamond seed crystals in acetone, deionized water and absolute ethyl alcohol, respectively cleaning for 20 min-30 min, and then drying in a vacuum drying oven at the temperature of 30-70 ℃ to obtain clean seed crystals;
secondly, preparing a shielding shelter:
shielding the part which is not required to be processed on the clean seed crystal by using an oxide coating, and leaving the surface defect part exposed to obtain the seed crystal shielded and masked;
thirdly, placing a sample:
placing a plurality of seed crystals of the shielding shelter on a cabin sample tray of the inductively coupled plasma equipment in order, wherein the distance between the seed crystals of each shielding shelter is 20-50 mm;
fourthly, closing the cabin:
the sample platform is moved into the cabin, and the cabin door of the cabin body is closed;
fifthly, vacuumizing:
after closing the cabin, vacuumizing the cabin body to make the vacuum degree in the cabin body reach 1.0 multiplied by 10-6mbar～1.0×10-5mbar；
Sixthly, inductively coupled plasma treatment:
firstly, starting a program, introducing argon, setting the flow of the argon to be 10 sccm-100 sccm, enabling the air pressure of a cabin body to be 0.5 Pa-30 Pa, starting an excitation power supply, and activating inductively coupled plasma;
secondly, adjusting the air pressure of the cabin body to be 3-40 Pa, and adjusting the incident power of the plasma to be 200-800W, so that the inductively coupled plasma reaches a preheating state;
thirdly, controlling the seed crystal temperature of the shielding shelter to be 400K-900K;
opening an oxidizing gas valve, introducing oxidizing gas, setting the flow rate of the oxidizing gas to be 2 sccm-40 sccm, keeping the pressure in the chamber to be 2 Pa-50 Pa, and after the oxidizing gas and the argon plasma atmosphere are uniformly mixed, adjusting the incident power of the plasma to be 300W-2200W and the polarization power to be 300W-2200W so that the inductively coupled plasma reaches a working state;
the oxidizing gas is oxygen or chlorine;
fifthly, processing for 1h to 50h under the conditions that the argon flow is 10sccm to 100sccm, the oxidizing gas flow is 2sccm to 40sccm, the pressure in the cabin is 2Pa to 50Pa, the plasma incident power is 300W to 2200W, the polarization power is 300W to 2200W and the seed crystal temperature of the shielding shelter is 400K to 900K;
closing the oxidizing gas valve and stopping introducing the oxidizing gas;
keeping the argon flow at 10-100 sccm, reducing the plasma incident power and the polarization power at a speed of 100-200W/min until the plasma incident power and the polarization power are respectively reduced to be lower than 100W, and cooling the treated seed crystal to room temperature;
eighthly, closing the excitation power supply and extinguishing plasma glow;
ninthly, stopping introducing the argon gas, and vacuumizing the cabin;
and opening the cabin to obtain a sample.
2. The method as claimed in claim 1, wherein the process is started in step six, argon gas is introduced, the flow rate of the argon gas is set to 10sccm to 100sccm, the air pressure of the chamber body is set to 0.5Pa to 30Pa, the excitation power supply is started, and the inductively coupled plasma is activated.
3. The method of claim 1, wherein the incident power of the plasma in step six is adjusted to 200W to 800W.
4. The method of claim 1, wherein the seed temperature of the shelter is controlled to be 400K to 900K in the sixth step.
5. The method according to claim 1, wherein in the sixty-four step, when the oxidizing gas is oxygen, the flow rate of the oxidizing gas is set to be 2sccm to 40sccm, the pressure in the chamber is kept to be 2Pa to 50Pa, and after the oxidizing gas and the argon plasma atmosphere are uniformly mixed, the plasma incident power is adjusted to be 1000W to 2000W and the polarization power is adjusted to be 1000W to 2000W.
6. The method according to claim 1, wherein in the sixty-four step, when the oxidizing gas is chlorine, the flow rate of the oxidizing gas is set to 10sccm to 50sccm, the pressure in the chamber is maintained to 2Pa to 50Pa, and after the oxidizing gas and the argon plasma atmosphere are uniformly mixed, the plasma incident power is adjusted to 800W to 2000W and the polarization power is adjusted to 800W to 2000W.
7. The method as claimed in claim 1, wherein the seed crystal is treated for 10 to 50 hours in the sixteenth step under the conditions that the flow rate of argon gas is 1 to 50sccm, the flow rate of oxidizing gas is 10 to 50sccm, the pressure of the cabin air is 2 to 50Pa, the incident power of plasma is 1000 to 2000W, the polarization power is 1000 to 2000W, and the temperature of the seed crystal for covering the mask is 300 to 800K.
8. The method as claimed in claim 1, wherein the seed crystal is treated for 5 to 50 hours in the sixteenth step under the conditions that the flow rate of argon gas is 1 to 50sccm, the flow rate of oxidizing gas is 10 to 50sccm, the pressure of the cabin is 2 to 50Pa, the incident power of plasma is 800 to 2000W, the polarization power is 800 to 2000W, and the temperature of the seed crystal for covering the mask is 300 to 800K.
9. The method as claimed in claim 1, wherein in step sixthly, the argon flow is maintained at 10sccm to 50sccm, the plasma incident power and the polarization power are reduced at a rate of 150W/min until the plasma incident power and the polarization power are respectively reduced to less than 100W, and the temperature of the treated seed crystal is reduced to room temperature.
10. The method of claim 1, wherein the oxide coating in step two is SiO2。
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| CN109183146A (en) * | 2018-10-17 | 2019-01-11 | 哈尔滨工业大学 | A method of single crystal diamond seed crystal surface defect is eliminated using inductively coupled plasma body technique |
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| CN109183146A (en) * | 2018-10-17 | 2019-01-11 | 哈尔滨工业大学 | A method of single crystal diamond seed crystal surface defect is eliminated using inductively coupled plasma body technique |
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| Title |
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| 张楷亮;王莎莎;王芳;吴小国;孙大智;: "基于电感耦合氧等离子体金刚石膜表面修饰的功率优化", 光电子.激光, no. 07, pages 1034 - 1037 * |
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