CN109796223A - The method that silicon vacancy defect and GR1 neutrality vacancy defect mutually convert in diamond - Google Patents
The method that silicon vacancy defect and GR1 neutrality vacancy defect mutually convert in diamond Download PDFInfo
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- CN109796223A CN109796223A CN201910062973.0A CN201910062973A CN109796223A CN 109796223 A CN109796223 A CN 109796223A CN 201910062973 A CN201910062973 A CN 201910062973A CN 109796223 A CN109796223 A CN 109796223A
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Abstract
The present invention relates to the methods that silicon vacancy defect in diamond and GR1 neutrality vacancy defect mutually convert, belong to semiconductor material and diamond post-processing technique field, solve the technical issues of migrating and converting based on defect, this method the following steps are included: S1, will be pre-processed after diamond cut to diamond sample, be made surface cleaning diamond sample remain after walk and use；S2, the pretreated diamond sample of step S1 is subjected to electron irradiation, silicon vacancy defect is converted into GR1 neutrality vacancy defect after diamond irradiation；S3, the diamond sample in step S2 is annealed in heating furnace, the GR1 neutrality vacancy defect that diamond is generated through step S2 is converted into silicon vacancy defect.The present invention can control silicon vacancy defect and GR1 neutrality vacancy defect concentration in diamond, provide the microcosmic intrinsic defect of various concentration for the different macroscopical use condition of diamond.
Description
Technical field
The invention belongs to semiconductor materials and diamond post-processing technique field, in particular to a kind of to utilize electron irradiation
Diamond is handled with annealing to make the method that silicon vacancy and GR1 neutrality vacancy mutually convert in diamond.
Background technique
Optical centre in diamond, such as nitrogen vacancy (NV), silicon vacancy (Si-V), chromium or nickel correlating center, due to narrow spectrum
Line, Gao Guangzi emissivity and optical states have longer coherence time, therefore can be used as quantum information and generate, store and process
Candidate centers.Since the Si-V defect excitation service life is short (~ 1ns), Zero-Phonon Transitions are strong, line width (~ 1.6nm), non-homogeneous exhibition
Width is small (0.015 nm), therefore the center Si-V has very strong photism and zero-phonon line (ZPL) at 738nm.These characteristics
It can be used for quantum optices technology.The photoluminescence property at the center Si-V is had studied, and as emitter lower
Injection range.Many of document reports the track for describing the center Si-V and electron spin coherence and quantum state
Relevant control technology, to be applied in quantum information is handled.
During chemical vapor deposition (CVD), silicon can be prepared using two methods of energetic ion injection and doping in situ
Doped diamond.After electron irradiation, intrinsic defect is introduced into silicon doped diamond, and annealing will lead to intrinsic defect migration.
In the processing of some pairs of diamond latent defects, few methods for migrating and converting based on defect.
Summary of the invention
In order to overcome the shortcomings of the prior art, silicon vacancy defect and GR1 neutrality vacancy in a kind of diamond are provided and lacked
The method mutually converted is fallen into, the concentration of different defects is controlled diamond post-processing using electron irradiation and annealing, makes Buddha's warrior attendant
Silicon vacancy is mutually converted with GR1 neutrality vacancy in stone.
The present invention is achieved by the following technical programs.
The method that silicon vacancy defect and GR1 neutrality vacancy defect mutually convert in diamond, comprising the following steps:
S1, diamond cutting is cut into having a size of long 2mm × wide 2mm × thickness 1mm sample, diamond sample is pre-processed,
The pretreatment includes pickling, cutting, polishing and ultrasonic cleaning, and the ultrasonic cleaning time is 30 ~ 60min, and it is clear that surface is made
Clean diamond sample is walked after remaining and is used；
S2, the pretreated diamond sample of step S1 is carried out to electron irradiation, irradiation voltage is 150 ~ 300KeV, irradiation dose
It is 1 × 1017~5×1020e·cm2, irradiation diameter is 80-150 μm, and the diamond after irradiation is carried out photoluminescence characterization, gold
Silicon vacancy defect is converted into GR1 neutrality vacancy defect after hard rock irradiation；
S3, the diamond sample in step S2 is annealed in heating furnace, the annealing temperature is 700-900 DEG C, soaking time
It is 30-60 minutes, GR1 neutrality vacancy defect concentration reduces, and silicon vacancy defect concentration increases, and diamond is generated through step S2
GR1 neutrality vacancy defect is converted into silicon vacancy defect.
Further, diamond sample in the step S1 are as follows: synthesized by microwave plasma assistant chemical vapor phase deposition
The colourless silicon doped diamond of 0.1 millimeters thick, nitrogen concentration are less than 10ppm, and it further includes other can not ignore that silicon concentration, which is less than 15ppm,
Impurity is micro.
Compared with prior art the invention has the benefit that
The method that silicon vacancy defect and GR1 neutrality vacancy defect mutually convert in a kind of diamond provided by the invention, can control
Silicon vacancy defect and GR1 neutrality vacancy defect concentration in diamond processed, provide difference for the different macroscopical use condition of diamond
The microcosmic intrinsic defect of concentration.
Detailed description of the invention
Fig. 1 is luminescence generated by light spot scan figure of the diamond in predose.
Fig. 2 is the luminescence generated by light spot scan figure after one electron irradiation of embodiment.
Fig. 3 be irradiation after Si-V vacancy defect irradiation zone intensity distribution.
Fig. 4 be irradiation after GR1 neutrality vacancy defect irradiation zone intensity distribution.
Sectional view of the Si-V vacancy defect in irradiation zone depth direction after Fig. 5 anneals for 800 DEG C.
Sectional view of the GR1 neutrality vacancy defect in irradiation zone depth direction after Fig. 6 anneals for 800 DEG C.
Specific embodiment
The present invention is described in further detail with reference to the accompanying drawings and examples.
Embodiment one
The diamond selected in the present embodiment one is provided by Xi'an Communications University, what which was synthesized by MPCVD
The colourless silicon doped diamond of 0.1 millimeters thick, nitrogen concentration are less than 10ppm, and it further includes other can not ignore that silicon concentration, which is less than 15ppm,
Impurity is micro；
Transmission electron microscope is Jeol Ltd. JEM-2100, and maximum voltage is 200 KeV；Heating furnace model
RT-1200, size of burner hearth 4*6mm.
The method that silicon vacancy defect and GR1 neutrality vacancy defect mutually convert in diamond, comprising the following steps:
S1, diamond cutting is cut into having a size of long 2mm × wide 2mm × thickness 1mm sample, diamond sample is pre-processed,
The pretreatment includes pickling, cutting, polishing and ultrasonic cleaning, and the ultrasonic cleaning time is 30 ~ 60min, and it is clear that surface is made
Clean diamond sample is walked after remaining and is used；
S2, the pretreated diamond sample of step S1 is subjected to electron irradiation, irradiation dose in transmission electron microscope JEM-2100
It is 1 × 1017 e·cm2, irradiation voltage is 200KeV, and irradiation diameter is 80 μm, and the diamond after irradiation is carried out luminescence generated by light
Characterization, silicon vacancy defect is converted into GR1 neutrality vacancy defect after diamond irradiation；
S3, the diamond sample in step S2 is annealed in RT-1200 heating furnace, the annealing temperature is 800 DEG C, when annealing
Using silicon carbide as gasket, soaking time is 30 minutes, and GR1 neutrality vacancy defect concentration reduces, and silicon vacancy defect concentration increases,
The GR1 neutrality vacancy defect that diamond is generated through step S2 is converted into silicon vacancy defect.
Embodiment two
The diamond selected in this example two is provided by Xi'an Communications University, the diamond sample synthesized by MPCVD 0.1
The colourless silicon doped diamond of millimeters thick, nitrogen concentration are less than 10ppm, silicon concentration be less than 15ppm, further include it is other can not ignore it is miscellaneous
Matter is micro；
Transmission electron microscope is Philips EM430, and maximum voltage is 300 KeV；Heating furnace model LinkamTS1200,
Burner hearth is having a size of 4*6mm.
The method that silicon vacancy defect and GR1 neutrality vacancy defect mutually convert in diamond, comprising the following steps:
S1, diamond cutting is cut into having a size of long 2mm × wide 2mm × thickness 1mm sample, diamond sample is pre-processed,
The pretreatment includes pickling, cutting, polishing and ultrasonic cleaning, and the ultrasonic cleaning time is 30min, and surface cleaning is made
Diamond sample is walked after remaining and is used；
S2, the pretreated diamond sample of step S1 is subjected to electron irradiation in transmission electron microscope Philips EM430, irradiated
Dosage is 1 × 1017 e·cm2, irradiation voltage is 250KeV, and irradiation diameter is 100 μm, the diamond after irradiation is carried out photic
Shine characterization, and silicon vacancy defect is converted into GR1 neutrality vacancy defect after diamond irradiation；
S3, the diamond sample in step S2 is annealed in RT-1200 heating furnace, the annealing temperature is 900 DEG C, when annealing
Using silicon carbide as gasket, soaking time is 30 minutes, and GR1 neutrality vacancy defect concentration reduces, and silicon vacancy defect concentration increases,
The GR1 neutrality vacancy defect that diamond is generated through step S2 is converted into silicon vacancy defect.
Embodiment three
The diamond selected in this example three is provided by Xi'an Communications University, the diamond sample synthesized by MPCVD 0.1
The colourless silicon doped diamond of millimeters thick, nitrogen concentration are less than 10ppm, and it further includes that other can not ignore impurity that silicon concentration, which is less than 15ppm,
It is micro；
Transmission electron microscope is Philips EM430, and maximum voltage is 300 KeV；Irradiation dose is 5 × 1020 e·cm2；
Heating furnace model RT-1200, burner hearth are having a size of 4 × 6mm.
The method that silicon vacancy defect and GR1 neutrality vacancy defect mutually convert in diamond, comprising the following steps:
S1, diamond cutting is cut into having a size of long 2mm × wide 2mm × thickness 1mm sample, diamond sample is pre-processed,
The pretreatment includes pickling, cutting, polishing and ultrasonic cleaning, and the ultrasonic cleaning time is 30min, and surface cleaning is made
Diamond sample is walked after remaining and is used；
S2, the pretreated diamond sample of step S1 is irradiated in transmission electron microscope Philips EM430, irradiation dose
It is 5 × 1020 e·cm2, irradiation voltage is 300KeV, and irradiation diameter is 120 μm, and the diamond after irradiation is carried out luminescence generated by light
Characterization, silicon vacancy defect is converted into GR1 neutrality vacancy defect after diamond irradiation；
S3, the diamond sample in step S2 is annealed in RT-1200 heating furnace, the annealing temperature is 900 DEG C, when annealing
Using silicon carbide as gasket, soaking time is 60 minutes, and GR1 neutrality vacancy defect concentration reduces, and silicon vacancy defect concentration increases,
The GR1 neutrality vacancy defect that diamond is generated through step S2 is converted into silicon vacancy defect.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
It is familiar with those skilled in the art in the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of, should all contain
Lid is within protection scope of the present invention.Therefore, protection scope of the present invention should be based on the protection scope of the described claims.
Claims (2)
1. the method that silicon vacancy defect and GR1 neutrality vacancy defect mutually convert in diamond, it is characterised in that including following step
It is rapid:
S1, diamond cutting is cut into having a size of long 2mm × wide 2mm × thickness 1mm sample, diamond sample is pre-processed,
The pretreatment includes pickling, cutting, polishing and ultrasonic cleaning, and the ultrasonic cleaning time is 30 ~ 60min, and it is clear that surface is made
Clean diamond sample is walked after remaining and is used；
S2, the pretreated diamond sample of step S1 is carried out to electron irradiation, irradiation voltage is 150 ~ 300KeV, irradiation dose
It is 1 × 1017~5×1020e·cm2, irradiation diameter is 80-150 μm, and the diamond after irradiation is carried out photoluminescence characterization, gold
Silicon vacancy defect is converted into GR1 neutrality vacancy defect after hard rock irradiation；
S3, the diamond sample in step S2 is annealed in heating furnace, the annealing temperature is 700-900 DEG C, soaking time
It is 30-60 minutes, GR1 neutrality vacancy defect concentration reduces, and silicon vacancy defect concentration increases, and diamond is generated through step S2
GR1 neutrality vacancy defect is converted into silicon vacancy defect.
2. the method that silicon vacancy defect and GR1 neutrality vacancy defect mutually convert in diamond according to claim 1,
It is characterized in that: diamond sample in the step S1 are as follows: 0.1 millimeters thick synthesized by microwave plasma assistant chemical vapor phase deposition
Colourless silicon doped diamond, nitrogen concentration are less than 10ppm, and silicon concentration is less than 15ppm, further include that other to can not ignore impurity micro.
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| CN201910062973.0A CN109796223A (en) | 2019-01-23 | 2019-01-23 | The method that silicon vacancy defect and GR1 neutrality vacancy defect mutually convert in diamond |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111344440A (en) * | 2017-09-18 | 2020-06-26 | 普林斯顿大学 | Synthetic diamond material with spinning impurities and method of making the same |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102939261A (en) * | 2010-06-03 | 2013-02-20 | 六号元素有限公司 | Diamond tools |
| CN104870697A (en) * | 2012-12-13 | 2015-08-26 | 六号元素技术有限公司 | Synthetic diamond materials for quantum and optical applications and methods of making the same |
| US20180080145A1 (en) * | 2015-03-26 | 2018-03-22 | Element Six (Uk) Limited | Highly fluorescent diamond particles and methods of fabricating the same |
| CN109152998A (en) * | 2016-05-17 | 2019-01-04 | 六号元素(英国)有限公司 | Diamond tool part |
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2019
- 2019-01-23 CN CN201910062973.0A patent/CN109796223A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102939261A (en) * | 2010-06-03 | 2013-02-20 | 六号元素有限公司 | Diamond tools |
| CN104870697A (en) * | 2012-12-13 | 2015-08-26 | 六号元素技术有限公司 | Synthetic diamond materials for quantum and optical applications and methods of making the same |
| US20180080145A1 (en) * | 2015-03-26 | 2018-03-22 | Element Six (Uk) Limited | Highly fluorescent diamond particles and methods of fabricating the same |
| CN109152998A (en) * | 2016-05-17 | 2019-01-04 | 六号元素(英国)有限公司 | Diamond tool part |
Non-Patent Citations (1)
| Title |
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| 王凯悦等: "金刚石中GR1中心的光致发光特性研究", 《物理学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111344440A (en) * | 2017-09-18 | 2020-06-26 | 普林斯顿大学 | Synthetic diamond material with spinning impurities and method of making the same |
| CN111344440B (en) * | 2017-09-18 | 2022-05-27 | 普林斯顿大学理事会 | Synthetic diamond material with spinning impurities and method of making the same |
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