CN117721530A - Manufacturing method of diamond SiV color center regular array structure - Google Patents
Manufacturing method of diamond SiV color center regular array structure Download PDFInfo
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- CN117721530A CN117721530A CN202311034762.9A CN202311034762A CN117721530A CN 117721530 A CN117721530 A CN 117721530A CN 202311034762 A CN202311034762 A CN 202311034762A CN 117721530 A CN117721530 A CN 117721530A
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- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 63
- 239000010432 diamond Substances 0.000 title claims abstract description 63
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 54
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 26
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 26
- 230000012010 growth Effects 0.000 claims abstract description 20
- 229910052741 iridium Inorganic materials 0.000 claims abstract description 18
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 14
- 239000010703 silicon Substances 0.000 claims abstract description 14
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000011248 coating agent Substances 0.000 claims abstract description 12
- 238000000576 coating method Methods 0.000 claims abstract description 12
- 239000000758 substrate Substances 0.000 claims abstract description 9
- 229920002120 photoresistant polymer Polymers 0.000 claims description 32
- 238000000034 method Methods 0.000 claims description 25
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 24
- 239000013078 crystal Substances 0.000 claims description 21
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 238000000151 deposition Methods 0.000 claims description 16
- 239000010410 layer Substances 0.000 claims description 14
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 14
- 229910052786 argon Inorganic materials 0.000 claims description 12
- 238000009616 inductively coupled plasma Methods 0.000 claims description 12
- 230000008021 deposition Effects 0.000 claims description 11
- 238000005530 etching Methods 0.000 claims description 11
- 239000007789 gas Substances 0.000 claims description 11
- 238000005229 chemical vapour deposition Methods 0.000 claims description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 239000011241 protective layer Substances 0.000 claims description 8
- 238000004544 sputter deposition Methods 0.000 claims description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 7
- 239000001257 hydrogen Substances 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- 238000000137 annealing Methods 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims description 6
- 238000005498 polishing Methods 0.000 claims description 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 4
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 239000002131 composite material Substances 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 238000011161 development Methods 0.000 claims description 2
- 238000001312 dry etching Methods 0.000 claims description 2
- 238000002474 experimental method Methods 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 230000001276 controlling effect Effects 0.000 abstract description 7
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- 238000005481 NMR spectroscopy Methods 0.000 description 3
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- 239000002159 nanocrystal Substances 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- 238000005424 photoluminescence Methods 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
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- 230000007423 decrease Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002189 fluorescence spectrum Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
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- 150000002500 ions Chemical class 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- 239000002110 nanocone Substances 0.000 description 1
- 239000002061 nanopillar Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000001259 photo etching Methods 0.000 description 1
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- -1 silicon ion Chemical class 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
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- 239000010409 thin film Substances 0.000 description 1
Abstract
The invention relates to a manufacturing method of a diamond SiV color center regular array structure, which belongs to the technical field of quantum materials, combines an electron beam lithography technology to form a nano-scale patterned silicon dioxide/iridium mask on the surface of a diamond substrate, adjusts the thickness of a silicon dioxide mask layer, controls the position and depth of silicon ion permeation, and regulates and controls the thickness of an epitaxial layer with a vacancy center by controlling the condition of secondary growth and the growth time, thereby regulating and controlling the detection precision. According to the preparation method of the diamond silicon color center regular array, the silicon dioxide/iridium mixed mask structure is adopted, and the doping depth meets the set requirement by controlling the thickness of a coating film, so that the diamond SiV color center structure with the regular array is prepared.
Description
Technical Field
The invention belongs to the technical field of quantum materials, and particularly relates to a method for manufacturing a diamond color center regular array, which provides a basis for further realizing a semiconductor device based on diamond.
Technical Field
The color center in diamond has attracted high attention in the fields of Quantum Information Processing (QIP), single photon sources (sps) for quantum computation, probes for weak magnetic field measurement, biosensing and the like due to the advantages of spin initialization, convenient operation, convenient optical readout, long coherence time in the environment and the like. There are two basic methods for forming color centers associated with impurities in diamond: the first method relies on ion implanted diamond doping to create a variety of optically active defects in this way, including NV, silicon vacancies (SiV), geV, tin vacancies (SnV), lead vacancies (PbV), and Cr centres; another method of forming the core is in situ doping during diamond synthesis using a high pressure-high temperature (HPHT) process or a Chemical Vapor Deposition (CVD) process. By adding selected doping elements to the crystallization medium, single-crystal or micro/nanocrystalline doped HPHT diamond can be obtained. However, HPHT technology does not allow the growth of thin films and fine structures, which can be achieved by CVD. Among the different CVD methods, microwave plasma CVD is considered to be the most suitable instrument for depositing epitaxial diamond films, polycrystalline films and separating micro/nanocrystals, because they provide very high diamond material purity (nitrogen impurity content less than 1 ppb) and allow for control of doping levels and film thickness. However, before the characteristic performance is fully developed, it is required to enhance the emission of a specific charge state, improve the collection efficiency of photons, and the like.
In general, diamond color centers are expected to be applied to nano-scale nuclear magnetic resonance, particularly nano-scale nuclear magnetic resonance, because they have high magnetic field sensitivity and nano-scale spatial resolution. One key factor is to reduce the distance between the diamond color center and the sensing target, as the magnetic field sensitivity of the color center decreases with the cube of the distance from the target. Shallow color centers with a depth of a few nanometers are necessary for nanometer-scale nuclear magnetic resonance. Currently, the mainstream scheme for realizing the structure in the industry is to prepare a nano-structure such as a nanowire array, a nano cone or a nano crystal diamond film material by etching. However, the etching defects or grain boundary defects introduced by the above scheme may reduce the detection performance. In addition, the overall uniformity is difficult to control due to the random spatial orientation created by the voids during growth.
Aiming at the difficulties, the patent provides a diamond color center structure for realizing high uniformity and low detection distance based on selective area growth. The nano-scale silicon oxide mask can be formed on the surface of the diamond substrate by combining an electron beam lithography technology, and an epitaxial layer with a silicon vacancy center can be formed due to penetration doping of the mask in the secondary growth process. The thickness of the epitaxial layer with the vacancy center can be regulated and controlled by controlling the secondary growth condition and the growth time, so that the detection precision is regulated and controlled. Compared with the technical scheme, the method realizes the nano-structure array based on the photoetching technology, so that the process with high uniformity and no etching damage is easier to obtain. On the other hand, since there is a silicon oxide mask under each nanostructure, voids of high uniformity can be realized and isolated from each other in space.
Disclosure of Invention
The invention aims to improve the coherence time and conversion rate of a diamond silicon color center structure, solve the technical problem of disordered inside the diamond SiV color center structure under normal conditions, and construct a diamond SiV color center structure convenient for accurate positioning. The sensor provided by the invention is provided with the diamond nano-pillar waveguide array to form a plurality of probes containing the silicon vacancy color centers, so that the efficiency and the service life of the silicon vacancy color center sensor are improved.
The technical scheme adopted by the invention is as follows:
a method for manufacturing a regular array structure of a diamond SiV color center combines an electron beam lithography technology to form a nano-scale patterned silicon dioxide/iridium mask on the surface of a diamond substrate, adjusts the thickness of a silicon dioxide mask layer, controls the position and depth of silicon ion penetration, and regulates and controls the thickness of an epitaxial layer with a vacancy center by controlling the condition of secondary growth and the growth time, thereby regulating and controlling the detection precision; the method specifically comprises the following steps:
step 1): pretreatment of diamond seed crystals
Selecting (100) oriented single crystal diamond as seed crystal, and precisely polishing the diamond seed crystal by adopting a method combining mechanical polishing and chemical polishing; then, the single crystal diamond seed crystal is treated by using boiled mixed solution of concentrated sulfuric acid and concentrated nitric acid with the volume ratio of 1:3 until bubbles are stopped to be generated on the surface of the substrate; then using hydrofluoric acid to treat the substrate to remove silicon impurities, then using deionized water to carry out ultrasonic cleaning, and then using acetone and alcohol to carry out ultrasonic cleaning alternately to remove impurities on the surface;
step 2): deposition of silicon dioxide masks
The experimental sample is prepared by adopting a radio frequency magnetron sputtering coating machine, the target is monocrystalline silicon, sputtering gas is argon with the purity of 99.9%, reactive gas is oxygen with the purity of 99.9%, the flow rates of the oxygen and the argon are respectively 10 sccm-20 sccm and 40 sccm-50 sccm, the thickness of silicon dioxide is 100 nm-600 nm, and the deposition temperature is 300-500 ℃;
step 3): deposition of metallic iridium protective layer
Sputtering a metal iridium protective layer with the thickness of 10 nm-30 nm on the surface of the silicon dioxide film to obtain a monocrystalline diamond seed crystal/silicon dioxide/iridium composite substrate; the annealing temperature is 700-900 ℃;
step 4): photoresist coating
Coating photoresist by using a photoresist homogenizing machine for experiments, wherein the rotating speed is 3000 r/s-5000 r/s, the photoresist homogenizing time is 30 s-50 s, and the photoresist with good uniformity of 1 mu m-2 mu m thickness is obtained;
step 5): alignment exposure
The exposure pattern is round holes with the diameter of 50 nm-200 nm and the interval between the round holes is 100 nm-2 mu m; wherein the exposure energy is 10 keV-30 keV, and the exposure dose of the round hole area is 200-400 mu C/cm 2 The exposure dose outside the round hole is 0.2-0.6 mu C/cm 2 ；
Step 6): post-development bake
Developing at room temperature for 50-70 s; post-baking at 100-120 deg.c for 5-15 min;
step 7): dry etching
An Inductively Coupled Plasma (ICP) etching process is adopted, and the volume ratio of 8mTorr to 15mTorr is 40: 1-40: CHF of 5 3 /O 2 The power of the gas mixture, the power of the radio frequency and the Inductively Coupled Plasma (ICP) are respectively 80W-100W and 300W-400W, and the etching rate is 1.5 mu m/min-3.5 mu m/min;
step 8): photoresist removal
Removing the residual photoresist by using acetone ultrasonic waves for 20-40 s;
step 9): growing single crystal diamond epitaxial layers
Putting the regular array mask prepared by the steps into plasma chemical vapor deposition (MPCVD) equipment to grow the diamond epitaxial layer, wherein the growth conditions are as follows: the epitaxial layer with the regularly arranged diamond silicon color center structure is obtained by the power of 2k W-3 k W, preferably 2.6 kW-2.8 k W, the pressure of 80-120 torr, preferably 90-105 torr, the temperature of 800-900 ℃, preferably 830-880 ℃, the hydrogen flow of 400-500 sccm, preferably 400-450 sccm, the methane flow of 20-36 sccm, preferably 20-28 sccm, the nitrogen flow of 0.01-0.03 sccm, preferably 0.01-0.02 sccm and the growth time of 20-40 h, preferably 22-30 h.
The beneficial effects are that:
according to the preparation method of the diamond silicon color center regular array, the silicon dioxide/iridium mixed mask structure is adopted, and the doping depth meets the set requirement by controlling the thickness of a coating film, so that the diamond SiV color center structure with the regular array is prepared.
Drawings
Fig. 1 is a process flow diagram of the regular array preparation of diamond silicon color centers according to the present invention.
Fig. 2 is a scan of a cross section of a sample of regular array structure of diamond SiV color centers prepared in example 1 of the present invention.
FIG. 3 is a fluorescence spectrum of a regular array structure of diamond SiV color centers prepared in example 1 of the present invention.
Detailed Description
For the purposes of promoting an understanding of the principles and advantages of the disclosure, reference will now be made to the embodiments illustrated in the drawings and specific language will be used to describe the same.
Example 1:
(1) And (3) performing magnetron sputtering on the surface of the precisely polished and cleaned monocrystalline diamond seed crystal, wherein monocrystalline silicon is used as a target, the flow rates of oxygen and argon are respectively 20sccm and 50sccm, the deposition temperature is 400 ℃, the preparation time is 10min, and a layer of silicon dioxide with the thickness of 100nm is obtained. (2) Sputtering an iridium protective layer with the thickness of 10nm on the surface of compact silicon dioxide at the temperature of 400 ℃ and the argon flow of 50sccm, and then annealing at the temperature of 800 ℃. (3) Coating photoresist by using a photoresist homogenizing machine, wherein the rotating speed is 3500r/s, the photoresist homogenizing time is 30s, the photoresist with the thickness of 2 mu m is obtained, the exposure pattern is round holes, the diameter is 100nm, and the interval between the round holes is 200nm; wherein the exposure dose of the round hole area is 350 muC/cm 2 The exposure dose outside the round hole was 0.5. Mu.C/cm 2 Developing at room temperature for 60s; post-baking at 100deg.C for 10min; an Inductively Coupled Plasma (ICP) etching process was used with a volume ratio of 10mTorr of 40: CHF of 3 3 /O 2 And (3) removing the residual photoresist by using acetone ultrasonic for 40 seconds to obtain a circular hole-shaped silicon dioxide/iridium mask, wherein the power of the gas mixture, the power of radio frequency and Inductively Coupled Plasma (ICP) are 80W and 300W respectively. (4) And depositing diamond on the surface of the mask prepared by adopting a microwave plasma chemical vapor deposition system, wherein the power of the growth process is 2.8k W, the pressure is 100torr, the temperature is 850 ℃, the hydrogen flow is 400sccm, the methane flow is 20sccm, the nitrogen flow is 0.01sccm, and the growth time is 30 hours, so that the diamond SiV color center structure with the regular array is obtained. A scanning electron microscope of the cross section of the sample is shown in fig. 2. Photoluminescence (PL) spectra were measured using a raman spectrometer with a laser wavelength of 532 nm. The results of testing the above window of the sample section obtained in example 1 and the diamond window respectively are shown in fig. 3, and illustrate that the diamond SiV color center structure with the regular array is prepared.
Example 2:
(1) And (3) performing magnetron sputtering on the surface of the precisely polished and cleaned monocrystalline diamond seed crystal, wherein monocrystalline silicon is used as a target, the flow rates of oxygen and argon are respectively 20sccm and 50sccm, the deposition temperature is 400 ℃, the preparation time is 10min, and a layer of silicon dioxide with the thickness of 200nm is obtained. (2) Sputtering an iridium protective layer with the thickness of 10nm on the surface of compact silicon dioxide at the temperature of 400 ℃ and the argon flow of 50sccm, and then annealing at the temperature of 800 ℃. (3) Coating photoresist by using a photoresist homogenizing machine, wherein the rotating speed is 3500r/s, the photoresist homogenizing time is 30s, the photoresist with the thickness of 2 mu m is obtained, the exposure pattern is round holes, the diameter is 100nm, and the interval between the round holes is 200nm; wherein the exposure dose of the round hole area is 350 muC/cm 2 The exposure dose outside the round hole was 0.5. Mu.C/cm 2 Developing at room temperature for 60s; post-baking at 100deg.C for 10min; an Inductively Coupled Plasma (ICP) etching process was used with a volume ratio of 10mTorr of 40: CHF of 3 3 /O 2 And (3) removing the residual photoresist by using acetone ultrasonic for 40 seconds to obtain a circular hole-shaped silicon dioxide/iridium mask, wherein the power of the gas mixture, the power of radio frequency and Inductively Coupled Plasma (ICP) are 80W and 300W respectively. (4) And depositing diamond on the surface of the mask prepared by adopting a microwave plasma chemical vapor deposition system, wherein the power of the growth process is 2.8k W, the pressure is 100torr, the temperature is 850 ℃, the hydrogen flow is 400sccm, the methane flow is 20sccm, the nitrogen flow is 0.01sccm, and the growth time is 30 hours, so that the diamond SiV color center structure with the regular array is obtained.
Example 3:
(1) And (3) performing magnetron sputtering on the surface of the precisely polished and cleaned monocrystalline diamond seed crystal, wherein monocrystalline silicon is used as a target, the flow rates of oxygen and argon are respectively 20sccm and 50sccm, the deposition temperature is 400 ℃, the preparation time is 10min, and a layer of silicon dioxide with the thickness of 300nm is obtained. (2) Sputtering an iridium protective layer with the thickness of 10nm on the surface of compact silicon dioxide at the temperature of 400 ℃ and the argon flow of 50sccm, and then annealing at the temperature of 800 ℃. (3) Coating photoresist with a photoresist homogenizing machine at 3500r/s for 30s to obtain 2 μm thick photoresistThe exposure pattern is round holes with the diameter of 100nm and the interval between the round holes is 200nm; wherein the exposure dose of the round hole area is 350 muC/cm 2 The exposure dose outside the round hole was 0.5. Mu.C/cm 2 Developing at room temperature for 60s; post-baking at 100deg.C for 10min; an Inductively Coupled Plasma (ICP) etching process was used with a volume ratio of 10mTorr of 40: CHF of 3 3 /O 2 And (3) removing the residual photoresist by using acetone ultrasonic for 40 seconds to obtain a circular hole-shaped silicon dioxide/iridium mask, wherein the power of the gas mixture, the power of radio frequency and Inductively Coupled Plasma (ICP) are 80W and 300W respectively. (4) And depositing diamond on the surface of the mask prepared by adopting a microwave plasma chemical vapor deposition system, wherein the power of the growth process is 2.8k W, the pressure is 100torr, the temperature is 850 ℃, the hydrogen flow is 400sccm, the methane flow is 20sccm, the nitrogen flow is 0.01sccm, and the growth time is 30 hours, so that the diamond SiV color center structure with the regular array is obtained.
Example 4:
(1) And (3) performing magnetron sputtering on the surface of the precisely polished and cleaned monocrystalline diamond seed crystal, wherein monocrystalline silicon is used as a target, the flow rates of oxygen and argon are respectively 20sccm and 50sccm, the deposition temperature is 400 ℃, the preparation time is 10min, and a layer of silicon dioxide with the thickness of 400nm is obtained. (2) Sputtering an iridium protective layer with the thickness of 10nm on the surface of compact silicon dioxide at the temperature of 400 ℃ and the argon flow of 50sccm, and then annealing at the temperature of 800 ℃. (3) Coating photoresist by using a photoresist homogenizing machine, wherein the rotating speed is 3500r/s, the photoresist homogenizing time is 30s, the photoresist with the thickness of 2 mu m is obtained, the exposure pattern is round holes, the diameter is 100nm, and the interval between the round holes is 200nm; wherein the exposure dose of the round hole area is 350 muC/cm 2 The exposure dose outside the round hole was 0.5. Mu.C/cm 2 Developing at room temperature for 60s; post-baking at 100deg.C for 10min; an Inductively Coupled Plasma (ICP) etching process was used with a volume ratio of 10mTorr of 40: CHF of 3 3 /O 2 And (3) removing the residual photoresist by using acetone ultrasonic for 40 seconds to obtain a circular hole-shaped silicon dioxide/iridium mask, wherein the power of the gas mixture, the power of radio frequency and Inductively Coupled Plasma (ICP) are 80W and 300W respectively. (4) Chemical gas using microwave plasmaAnd depositing diamond on the surface of the mask prepared by the phase deposition system, wherein the power of the growth process is 2.8k W, the pressure is 100torr, the temperature is 850 ℃, the hydrogen flow is 400sccm, the methane flow is 20sccm, the nitrogen flow is 0.01sccm, and the growth time is 30 hours, so that the diamond SiV color center structure with a regular array is obtained.
Claims (2)
1. The manufacturing method of the diamond SiV color center regular array structure comprises the following steps:
step 1): pretreatment of diamond seed crystals
Selecting (100) oriented single crystal diamond as seed crystal, and precisely polishing the diamond seed crystal by adopting a method combining mechanical polishing and chemical polishing; then, the single crystal diamond seed crystal is treated by using boiled mixed solution of concentrated sulfuric acid and concentrated nitric acid with the volume ratio of 1:3 until bubbles are stopped to be generated on the surface of the substrate; then using hydrofluoric acid to treat the substrate to remove silicon impurities, then using deionized water to carry out ultrasonic cleaning, and then using acetone and alcohol to carry out ultrasonic cleaning alternately to remove impurities on the surface;
step 2): deposition of silicon dioxide masks
The experimental sample is prepared by adopting a radio frequency magnetron sputtering coating machine, the target is monocrystalline silicon, sputtering gas is argon with the purity of 99.9%, reactive gas is oxygen with the purity of 99.9%, the flow rates of the oxygen and the argon are respectively 10 sccm-20 sccm and 40 sccm-50 sccm, the thickness of silicon dioxide is 100 nm-600 nm, and the deposition temperature is 300-500 ℃;
step 3): deposition of metallic iridium protective layer
Sputtering a metal iridium protective layer with the thickness of 10 nm-30 nm on the surface of the silicon dioxide film to obtain a monocrystalline diamond seed crystal/silicon dioxide/iridium composite substrate; the annealing temperature is 700-900 ℃;
step 4): photoresist coating
Coating photoresist by using a photoresist homogenizing machine for experiments, wherein the rotating speed is 3000 r/s-5000 r/s, the photoresist homogenizing time is 30 s-50 s, and the photoresist with good uniformity of 1 mu m-2 mu m thickness is obtained;
step 5): alignment exposure
The exposure pattern is round hole with diameter50 nm-200 nm, and the distance between the round holes is 100 nm-2 μm; wherein the exposure energy is 10 keV-30 keV, and the exposure dose of the round hole area is 200-400 mu C/cm 2 The exposure dose outside the round hole is 0.2-0.6 mu C/cm 2 ；
Step 6): post-development bake
Developing at room temperature for 50-70 s; post-baking at 100-120 deg.c for 5-15 min;
step 7): dry etching
An inductively coupled plasma etching process is adopted, and the volume ratio of 8mTorr to 15mTorr is 3 to 5: CHF of 10 3 /O 2 The power of the gas mixture, the power of the radio frequency and the power of the inductively coupled plasma are respectively 80W-100W and 300W-400W, and the etching rate is 1.5 mu m/min-3.5 mu m/min;
step 8): photoresist removal
Removing the residual photoresist by using acetone ultrasonic waves for 20-40 s;
step 9): growing single crystal diamond epitaxial layers
Putting the regular array mask prepared by the steps into plasma chemical vapor deposition equipment to grow a diamond epitaxial layer, wherein the growth conditions are as follows: the power is 2k W-3 k W, the pressure is 80-120 torr, the temperature is 800-900 ℃, the hydrogen flow is 400-500 sccm, the methane flow is 20-36 sccm, the nitrogen flow is 0.01-0.03 sccm, and the growth time is 20-40 h, so that the epitaxial layer with the regularly arranged diamond silicon color center structure is obtained.
2. The method for manufacturing a regular array structure of diamond SiV color centers according to claim 1, wherein in step 9), the growth conditions are: the power is 2.6-k W-2.8 k W, the pressure is 90-105 torr, the temperature is 830-880 ℃, the hydrogen flow is 400-450 sccm, the methane flow is 20-28 sccm, the nitrogen flow is 0.01-0.02 sccm, and the growth time is 22-30 h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202311034762.9A CN117721530A (en) | 2023-08-16 | 2023-08-16 | Manufacturing method of diamond SiV color center regular array structure |
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| CN202311034762.9A CN117721530A (en) | 2023-08-16 | 2023-08-16 | Manufacturing method of diamond SiV color center regular array structure |
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