CN109338459A - A kind of N doping method preparing low COP defect silicon single crystal - Google Patents
A kind of N doping method preparing low COP defect silicon single crystal Download PDFInfo
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- CN109338459A CN109338459A CN201811519495.3A CN201811519495A CN109338459A CN 109338459 A CN109338459 A CN 109338459A CN 201811519495 A CN201811519495 A CN 201811519495A CN 109338459 A CN109338459 A CN 109338459A
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- 239000013078 crystal Substances 0.000 title claims abstract description 54
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 44
- 239000010703 silicon Substances 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 37
- 230000007547 defect Effects 0.000 title claims abstract description 27
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 147
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 71
- 238000010494 dissociation reaction Methods 0.000 claims abstract description 51
- 230000005593 dissociations Effects 0.000 claims abstract description 51
- 239000007789 gas Substances 0.000 claims abstract description 23
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 239000007787 solid Substances 0.000 claims abstract description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 32
- 229910052757 nitrogen Inorganic materials 0.000 claims description 16
- 239000012298 atmosphere Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000919 ceramic Substances 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 6
- 238000005121 nitriding Methods 0.000 abstract description 6
- 239000012299 nitrogen atmosphere Substances 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000010923 batch production Methods 0.000 abstract description 2
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 5
- 125000004433 nitrogen atom Chemical group N* 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000000752 ionisation method Methods 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 238000007500 overflow downdraw method Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
Classifications
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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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/02—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt
- C30B15/04—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt adding doping materials, e.g. for n-p-junction
-
- 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
- C30B29/06—Silicon
-
- 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
- C30B31/00—Diffusion or doping processes for single crystals or homogeneous polycrystalline material with defined structure; Apparatus therefor
- C30B31/06—Diffusion or doping processes for single crystals or homogeneous polycrystalline material with defined structure; Apparatus therefor by contacting with diffusion material in the gaseous state
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a kind of N doping methods for preparing low COP defect silicon single crystal.During crystal for straight drawing monocrystal growth, increase ammonia thermal dissociation device, high-purity ammonia is passed through ammonia thermal dissociation device and generates N (g), N (g) is dissolved in silicon melt, and diffuse at crystal growth solid, liquid interface, then as the progress of growth course, into inside silicon single crystal, it realizes N doping process, inhibits silicon single crystal COP defect;Compared with traditional nitrogen atmosphere nitriding, ammonia dissociation temperature is low, dissociation efficiency is high, it is easy to accomplish nitrogen-doping effect helps to prepare the low COP defect silicon single crystal of vertical pulling method.Ammonia dissociation temperature is low to mean that heating power is lower, and ammonia dissociation efficiency height means that required gas source is less, and therefore, this will substantially reduce production cost, is applicable to the batch production of the low COP defect silicon single crystal of vertical pulling method.
Description
Technical field
The present invention relates to single crystal silicon semiconductor material preparation technology more particularly to a kind of prepare low COP defect silicon single crystal
N doping method.
Background technique
Semiconductor monocrystal silicon materials are the basic materials of the electronics industries such as semiconductor devices and integrated circuit.From raising silicon device
Part and ic yield, for reducing the angle of cost, the diameter for increasing silicon single crystal is still crystal for straight drawing monocrystal system from now on
The development trend of standby technology.Often there is Crystal Originated Particle (Crystal in the crystal for straight drawing monocrystal of major diameter
Originated Particls) defect, referred to as COP defect.When the size of COP defect reaches the scale of characteristic line breadth, it
It will seriously affect the gate oxide integrity of integrated circuit, and with the reduction of integrated circuit feature line width, its destructiveness
It will be increasing.
Inhibit COP defect generate method first is that N doping method.Existing correlative study shows for vertical pulling method silicon list
Crystalline substance, N doping can reduce COP flaw size, reduce COP defect concentration.There are many implementations, including nitrogen for N doping technique
Gas atmosphere nitriding, Si3N4Fusion method and ion implanting etc..Wherein, nitrogen atmosphere nitriding employs nitrogen as growth atmosphere,
Nitrogen molecular in nitrogen dissociates into nitrogen-atoms at high temperature, and nitrogen-atoms is dissolved in melt silicon and diffuses to crystal growth solid, liquid boundary
At face, it will enter inside silicon single crystal as growth course carries out nitrogen-atoms, and realize N doping process.Nitrogen atmosphere nitriding exists
Main problem be N doping low efficiency, this is because nitrogen molecular is not easy to dissociate into nitrogen-atoms.In fact, nitrogen molecular is known
Most stable of in diatomic molecule, the NoN key in nitrogen molecular has very high dissociation energy (about 941 kJ × mol-1), or even heating
Only 0.1% rate of dissociation when to 3000 DEG C of high temperature.In the relatively low silicon monocrystal growth environment of temperature, nitrogen molecular from
Solution rate is lower.In order to improve the low problem of the nitrogen rate of dissociation, often using the method for increasing nitrogen flow, but this will lead to life
Long air pressure is excessively high, in some instances it may even be possible to the heating electrode of monocrystal stove be brought the negative effect such as to strike sparks.
In conclusion in traditional crystal for straight drawing monocrystal technique, the nitrogen thermal dissociation efficiency of nitrogen atmosphere nitriding
It is low, N doping effect is poor, be not easy to realize the inhibiting effect to silicon single crystal COP defect.
Summary of the invention
To the prior art, there are the analyses of technical problem in view of above-mentioned, the present invention is intended to provide a kind of prepare low COP defect
The N doping method of silicon single crystal, to solve N doping effect in the prior art it is poor, to the inhibiting effect of silicon single crystal COP defect not
Strong technical problem.
The purpose of the present invention is mainly achieved through the following technical solutions: a kind of nitrogen preparing low COP defect silicon single crystal
Doping method, which is characterized in that this method has following steps:
(1), during crystal for straight drawing monocrystal growth, high-purity ammonia is passed through thermal dissociation device and generates N (g), ammonia flow
Range is 0.01 ~ 0.05 SLM.
(2), N (g) is dissolved in silicon melt, and diffuses at crystal growth solid, liquid interface, then as growth course
Progress, into inside silicon single crystal, realize N doping process, inhibit silicon single crystal COP defect.
(3), emission-control equipment is first passed through before tail gas enters and evacuates pipeline, emission-control equipment includes the mistake of low temperature
Structure is filtered, which makes ammonia dissociation product react generation ammonia, nitrogen and hydrogen at low temperature, then passes in water,
Ammonia is set to be dissolved in water, the tail gas for removing ammonia enters evacuation pipeline and puts side by side into atmosphere.
Present invention ammonia thermal dissociation device as described in step (1) is in entrance area, intermediate region and exit region point
Netted dissociation area is not set, for increasing the circulation path of ammonia, improves the contact area of ammonia and thermal environment, makes ammonia air-flow
It is sufficiently heated;Heater is respectively set in position outside gas pipeline around netted dissociation area, at high temperature for ammonia
Dissociation;Heater is respectively I heater, II heater, III heater, and wherein I heater is around setting in gas
The entrance area of pipeline external;II heater surrounds the intermediate region being arranged in outside gas pipeline;III heater surrounds
Exit region outside gas pipeline is set;The temperature of three region settings is different, i.e. the intermediate region entrance area temperature >
Temperature > exit region temperature.
The ammonia thermal dissociation device is mounted on the middle part of monocrystal stove inner cavity chamber by the present invention, and setting heater enters
Mouth region domain, intermediate region, exit region temperature are successively are as follows: 1200 ~ 1300 DEG C, 1100 ~ 1200 DEG C, 1000 ~ 1100 DEG C.
The ammonia thermal dissociation device is mounted on the lower part of monocrystal stove inner cavity chamber by the present invention, i.e., adds close to graphite
Hot device position, setting calorifier inlets region, intermediate region, exit region temperature successively are as follows: 800 ~ 900 DEG C, 700 ~ 800 DEG C,
600~700℃。
Netted dissociation area of the present invention is made of similar spongiform high temperature resistant, chemically inert porous ceramic film material
Airflow channel.
Ammonia is passed through in single crystal growth process, ammonia dissociates at high temperature, and reaction process is with following reversible chemical reaction
Formula description:
NH3 (g) « NH2(g) (1)+H (g);
NH2(g) (2) NH (g)+H (g);
NH (g) N (g)+H (g) (3).
In chemical equation (3), N (g) can be dissolved in silicon melt, and diffuse to crystal growth solid, liquid interface
Into inside silicon single crystal, N doping process is realized then as the progress of growth course in place.
The rate of dissociation of ammonia is higher.It is estimated according to chemical equilibrium theory, when temperature is up to 1000 DEG C, the rate of dissociation of ammonia can
Up to 99% or more, this, which means that be dissociated with less ammonia, generates enough N (g), to meet nitrogen-doping
Demand.
It illustrates, NH3Although successively dismantling the energy needed for them there are three N-H key of equal value in molecule
It is different, i.e. NH3、NH2, the dissociation energy of NH it is different.Studies have shown that NH3、NH2, NH dissociation energy successively reduce, respectively
435 kJ×mol-1、397 kJ×mol-1、339 kJ×mol-1Left and right.So ammonia thermal dissociation device may be designed as difference
Temperature range, this may advantageously facilitate chemical equation and carries out to the right, improve ammonia dissociation efficiency.
The present invention has the beneficial effect that:
1, the present invention provides a kind of N doping methods for preparing low COP silicon single crystal.Lead to during crystal for straight drawing monocrystal growth
Enter ammonia, N (g) obtained by ammonia thermal dissociation, compared with traditional nitrogen atmosphere nitriding, ammonia dissociation temperature is low, from
It solves high-efficient, it is easy to accomplish nitrogen-doping effect helps to prepare the low COP defect silicon single crystal of vertical pulling method.
2, using the N doping method provided by the invention for preparing low COP silicon single crystal, ammonia dissociation temperature is low to be meaned to add
Thermal power is lower, and ammonia dissociation efficiency height means that required gas source is less, and therefore, this will substantially reduce production cost, applicable
In the batch production of the low COP defect silicon single crystal of vertical pulling method.
Detailed description of the invention
Fig. 1 is the ammonia thermal dissociation device schematic side view used in the embodiment of the present invention.
The ammonia thermal dissociation device schematic elevation view used in Fig. 2 embodiment of the present invention;
Fig. 3 is the crystal for straight drawing monocrystal furnace schematic diagram that the embodiment of the present invention 1 has ammonia high temperature ionization device;
Fig. 4 is the crystal for straight drawing monocrystal furnace schematic diagram that the embodiment of the present invention 2 has ammonia high temperature ionization device.
Specific embodiment
Present invention will be further explained below with reference to the attached drawings and examples:
As depicted in figs. 1 and 2, ammonia thermal dissociation device of the invention is distinguished in entrance area, intermediate region and exit region
Netted dissociation area 5 is set, for increasing the circulation path of ammonia, improves the contact area of ammonia and thermal environment, makes ammonia air-flow
It is sufficiently heated;Netted dissociation area 5 is made of similar spongiform air-flow high temperature resistant, chemically inert porous ceramic film material and leads to
Road.Heater is respectively set in position outside gas pipeline 4 around netted dissociation area 5, dissociates at high temperature for ammonia;Add
Hot device is respectively I heater 1, II heater 2, III heater 3, and wherein I heater is around setting in gas pipeline
Entrance area outside 4;II heater 2 surrounds the intermediate region being arranged in outside gas pipeline 4;III heater 3 surrounds
Exit region outside gas pipeline 4 is set;The temperature of three region settings is different, i.e. the intermediate region entrance area temperature >
Temperature > exit region temperature.
In view of NH3、NH2, NH dissociation energy successively reduce, ammonia thermal dissociation device is designed as different temperatures section.If
The I heter temperature for setting ammonia thermal dissociation device portal region is relatively high, the II heter temperature phase of intermediate region
To lower, the temperature of the III heater of exit region is minimum.Such thermal field design, improves ammonia dissociation efficiency, and drop
Low heating power reduces energy consumption.
Embodiment 1: the N doping method for preparing low COP defect silicon single crystal has following steps:
(1) as shown in figure 3, increasing ammonia high temperature ionization device 11 in the middle part of crystal for straight drawing monocrystal furnace chamber;In vertical pulling method silicon list
In brilliant 6 growth courses, high-purity ammonia is passed through ammonia thermal dissociation device and generates N (g), ammonia flow 0.03SLM.This implementation
Example setting calorifier inlets region, intermediate region, exit region temperature are successively are as follows: 1250 DEG C, 1150 DEG C, 1050 DEG C.
(2) N (g) is dissolved in silicon melt 7, and diffuses at crystal growth solid, liquid interface, then as growth course
Progress, into inside silicon single crystal, realize N doping process, inhibit silicon single crystal COP defect.
(3) emission-control equipment 9 is first passed through before tail gas enters and evacuates pipeline 10, emission-control equipment 9 includes low temperature
Filter structure, which react ammonia dissociation product at low temperature to generate ammonia, nitrogen and hydrogen, then pass to water
In, so that ammonia is dissolved in water, remove the tail gas of ammonia, into evacuation pipeline 10, and is emitted into atmosphere.It is passed through vertical pulling method silicon list
The ammonia flow very little of brilliant furnace, therefore the content of nitrogen and hydrogen is also very small in treated tail gas, to the shadow of external environment
Sound is very little, can be directly entered and evacuate pipeline 10, and be emitted into atmosphere.
Ammonia is behind netted dissociation area 5, and dissociation generates N (g) under high temperature action, subsequently into crystal for straight drawing monocrystal
Inside furnace chamber.N (g) will be dissolved in silicon melt 7 and diffuse at crystal growth solid, liquid interface, then as growth course
Progress, into inside silicon single crystal 6, realize N doping process.The ammonia rate of dissociation is high in the present invention, so ammonia in actual production
Throughput is smaller, flow 0.03SLM.In order to avoid containing vapor in ammonia, gas purifier should be matched (such as to miscellaneous
Matter oxygen has higher requirements, and can also increase oxygen-eliminating device in purifier).
Embodiment 2: the N doping method for preparing low COP defect silicon single crystal has following steps:
As shown in figure 4, the present embodiment is unlike the first embodiment: it is high to increase ammonia in the chamber lower portion of crystal for straight drawing monocrystal furnace
Warm ionization device 11, i.e., close to graphite heater position;The present embodiment sets calorifier inlets region, intermediate region, outlet area
Domain temperature is successively are as follows: 850 DEG C, 750 DEG C, 650 DEG C.
Since ammonia high temperature ionization device 11 is placed near graphite heater 8, adding for graphite heater 8 can use
The high temperature ionization process of ammonia is completed in heat effect, therefore compared with Example 1, the present embodiment can significantly reduce the heating of heater
Power.
Claims (4)
1. a kind of N doping method for preparing low COP defect silicon single crystal, which is characterized in that this method has following steps:
(1), during crystal for straight drawing monocrystal growth, high-purity ammonia is passed through thermal dissociation device and generates N (g), ammonia flow
Range is 0.01 ~ 0.05 SLM;
(2), N (g) is dissolved in silicon melt, and diffuse at crystal growth solid, liquid interface, then as growth course into
Row realizes N doping process into inside silicon single crystal, inhibits silicon single crystal COP defect;
(3), emission-control equipment is first passed through before tail gas enters and evacuates pipeline, emission-control equipment includes the filtering knot of low temperature
Structure, the filter structure make ammonia dissociation product react generation ammonia, nitrogen and hydrogen at low temperature, then pass in water, make ammonia
Gas is dissolved in water, and the tail gas for removing ammonia enters evacuation pipeline and puts side by side into atmosphere;
Ammonia thermal dissociation device as described in step (1) is respectively set netted in entrance area, intermediate region and exit region
Area is dissociated, for increasing the circulation path of ammonia, the contact area of ammonia and thermal environment is improved, adds ammonia air-flow sufficiently
Heat;Heater is respectively set in position outside gas pipeline around netted dissociation area, dissociates at high temperature for ammonia;Heating
Device is respectively I heater, II heater, III heater, and wherein I heater is around setting outside gas pipeline
Entrance area;II heater surrounds the intermediate region being arranged in outside gas pipeline;III heater is around setting in gas
The exit region of body pipeline external;The temperature of three region settings is different, i.e., the intermediate region entrance area temperature > temperature > goes out
Mouth regional temperature.
2. a kind of N doping method for preparing low COP defect silicon single crystal according to claim 1, which is characterized in that by institute
The ammonia thermal dissociation device stated is mounted on the middle part of monocrystal stove inner cavity chamber, and setting calorifier inlets region, goes out intermediate region
Mouth regional temperature is successively are as follows: 1200 ~ 1300 DEG C, 1100 ~ 1200 DEG C, 1000 ~ 1100 DEG C.
3. a kind of N doping method for preparing low COP defect silicon single crystal according to claim 1, which is characterized in that by institute
The ammonia thermal dissociation device stated is mounted on the lower part of monocrystal stove inner cavity chamber, i.e., close to graphite heater position, setting heating
Device entrance area, intermediate region, exit region temperature are successively are as follows: 800 ~ 900 DEG C, 700 ~ 800 DEG C, 600 ~ 700 DEG C.
4. a kind of N doping method for preparing low COP defect silicon single crystal according to claim 1, which is characterized in that described
Netted dissociation area similar spongiform airflow channel is made of high temperature resistant, chemically inert porous ceramic film material.
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Application publication date: 20190215 Assignee: CLP Jinghua (Tianjin) semiconductor materials Co.,Ltd. Assignor: CHINA ELECTRONICS TECHNOLOGY GROUP CORPORATION NO.46 Research Institute Contract record no.: X2024980003546 Denomination of invention: A nitrogen doping method for preparing low COP defect silicon single crystals Granted publication date: 20210112 License type: Common License Record date: 20240327 |