CN107419329A - The preparation method of the full carbon structure of single-crystal diamond surface in situ n-type semiconductorization - Google Patents
The preparation method of the full carbon structure of single-crystal diamond surface in situ n-type semiconductorization Download PDFInfo
- Publication number
- CN107419329A CN107419329A CN201710363710.4A CN201710363710A CN107419329A CN 107419329 A CN107419329 A CN 107419329A CN 201710363710 A CN201710363710 A CN 201710363710A CN 107419329 A CN107419329 A CN 107419329A
- Authority
- CN
- China
- Prior art keywords
- diamond
- crystal diamond
- crystal
- situ
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
- 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
- C30B25/20—Epitaxial-layer growth characterised by the substrate the substrate being of the same materials as the epitaxial layer
- C30B25/205—Epitaxial-layer growth characterised by the substrate the substrate being of the same materials as the epitaxial layer the substrate being of insulating material
-
- 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
Abstract
A kind of preparation method of the full carbon structure of single-crystal diamond surface in situ n-type semiconductorization, belongs to semiconductor foundation circuit matrix material preparation field.Processing step is：A. single-crystal diamond is polished to surface roughness using mechanical polishing and is less than 1nm；B. pickling and H is used2Plasma etching in situ, makes seed crystal face form microcosmic forming core point；C. single crystal diamond substrate is placed in molybdenum support microflute, sample surfaces to groove height and sample and microflute gap ratio are maintained between 0.5 0.7；D. using single-crystal diamond as seed crystal, by controlling depositing operation to suppress space propagation and the diffusion into the surface of carbon-containing group, in single-crystal diamond surface sp3Suppress abstraction reaction under structure, rely on the step and defect area of single-crystal diamond, realize super Nano diamond forming core and growth；Nitrating realizes the n-type doping of super Nano diamond simultaneously, and the preparation of the conductive super Nano diamond thin layer of surface in situ n-type is finally realized in the case where not changing single crystal diamond seed crystal initial condition, forms a kind of diamond semiconductor of full carbon structure.
Description
Technical field：
The present invention relates to semiconductor foundation circuit matrix material preparation field；Particularly utilized on single-crystal diamond surface
Plasma etching and vapour deposition, form the super Nano diamond thin layer of n-type in diamond surface direct in-situ semiconductor transformation, obtain
A kind of diamond semiconductor of full carbon structure.
Technical background
Diamond have broader band gap (5.5eV), high carrier mobility (particularly hole mobility than single crystalline Si,
GaAs is much higher), low-k (5.7), high Johnson indexs and Keyse indexs (be above Si and GaAs ten again with
On) etc., it is described as high-frequency high-power and the ultimate wide bandgap semiconductor in high-temperature pressure-proof field, also referred to as forth generation is partly led
Body.And enable semiconductor devices normal work in extreme circumstances because of the splendid stability that it has.However, Buddha's warrior attendant
Carbon atom radius and lattice constant are smaller in stone, and energy gap is big, therefore solubility is very low in a diamond for many foreign atoms,
And the higher development for constraining diamond semiconductor of ionization energy of impurity.The p-type impurity energy level mixed in diamond film is deep, causes
Carrier concentration is low, and mobility is small, and resistivity is high, and ion doping still faces problems at present.Preparation on n-type diamond
Method is more using CVD and the method for ion implanting, and correlative study achieves certain progress, but effect is still undesirable, and destroys
Diamond crystal perfection itself.For this, scholars start to explore and have studied the mode of the super Nano diamond of N doping and realize
N-type conduction (Phys.Rev.B.74,235434 (2006) and its conductive mechanism (Phys.Rev.B.70,125412 (2004)).By
Then substantial amounts of crystal boundary in super Nano diamond be present, and nitrogen causes seepage flow approach in grain boundary area and improves n-type conduction,
Electrical conductivity absolute value is improved as the increase of nitrogen content improves carrier mobility and broadening energy band.Neda etc. is mixed with nitrogen
Miscellaneous super Nano diamond realizes n-type conduction and is prepared for piezoresistance sensor (DiamondRelat.Mater.70,145150
(2016)；Ultraviolet detector has been made using the super Nano diamond of N doping n-type in Abdelrahman etc.
(Appl.Phys.A.123,167(2017)).It can be seen that the super Nano diamond of N doping n-type becomes diamond n-type semiconductor
Effective ways, and its performance has reached the level of boron-doped diamond.But the current super Nano diamond of N doping n-type
Film preparation uses hetero-substrates, such as Si, often due to the low thermal conductivity of substrate and low resistance to pressure so that diamond is excellent
Good electric property is difficult to play, and limits the abundant application of super Nano diamond excellent properties.At the same time, in foreign substrate
Upper growth Nano diamond even super Nano diamond, is generally required using the side such as mechanical lapping or bias to improve nucleation rate
Method so that growth technique is complicated, and easily causes stress and the deformation of substrate.
The content of the invention
To solve the above problems, it is substrate forming core it is an object of the invention to propose one kind based on high heat conduction single-crystal diamond
The super nanometer n-type diamond of growth, so as to form a kind of full diamond carbon structural semiconductor for having good heat conductive and conductive characteristic concurrently.
After single-crystal diamond polishing is reached into extremely low roughness using mechanical polishing, it is placed in molybdenum support microflute, is ensured by pickling
Sample keeps certain geometry relation with groove, using H2Plasma etching in situ makes seed crystal face form microcosmic forming core point.With
Afterwards by controlling depositing operation, the step after single-crystal diamond etching is relied under not changing diamond seed initial condition is with lacking
Area is fallen into, nitrating realizes n-type doped growing while realizing super Nano diamond forming core, meets the conductive super nanometer of surface in situ n-type
The preparation of thin layer of diamond, form a kind of diamond semiconductor of full carbon structure.
The technical scheme is that：
A kind of preparation method of single-crystal diamond surface in situ n-type semiconductor.It is characterized in that pass through microwave plasma
Body etches directly generates the conductive super Nano diamond thin layer of n-type, processing step on single-crystal diamond surface with gas phase deposition technology
To be as follows：
(1) grinding and polishing of single crystal diamond seed crystal
To ensure that surface meets electronic device requirement after growing super Nano diamond, first to single crystal diamond film surface
Carry out precise polished.With the diadust that granularity is 40,20,10 and 2.5, pre-polish(ing) is carried out；After be placed in precision diamond
Finishing polish is carried out on polishing disk, realizes that surface roughness is less than 1nm after polishing.
(2) single crystal diamond seed crystal pickling processes
To ensure single-crystal diamond any surface finish, metal inclusion that may be present, hydrocarbon, graphite etc. are removed.Throw
Seed crystal sample is placed in HCl after light：H2SO4Mixed liquor in boil after use deionized water rinsing；Be sequentially placed into again acetone soln and
It is cleaned by ultrasonic drying in absolute ethyl alcohol.
(3) foundation of single-crystal diamond depositional environment
Single crystal diamond substrate is placed in the square microflute of molybdenum support, sample surfaces to rooved face height with sample survey edge and
Microflute spacing ratio is maintained between 0.5-0.7, molybdenum support thickness in 5-15mm, depth of mini longitudinal channels 500 microns -1500 microns it
Between.And molybdenum support is placed on copper heat conduction base station and ensures that heat scatters and disappears.This method can keep a suitable diamond substrate to sink
Long-pending part and Near-neighbor Environment.Because if diamond single crystal is in argon-arc plasma field, temperature and chamber pressure influence each other and are unable to reach
Suitable condition, and surface deposits super Nano diamond process easily the appearance of crystallite and seed crystal face side in the plasma
Edge temperature is too high and makes seed crystal face temperature distributing disproportionation and influences the flatness of sedimentary, so as to avoid fast-growth from occurring
Nanocluster so that diamond surface sedimentary reaches planarizing.Moreover, crystallite dimension depends on chemical reaction mean free path
Degree and boundary layer thickness, designed groove depth can improve the steady flow layer thickness of diamond surface, and crystallite dimension is thick with boundary layer
The increase of degree and reduce, be advantageous to the second nucleation of crystal grain；Simultaneously active group concentration can be ensured, ensured super nanocrystalline fast
Fast forming core growth.At the same time, molybdenum support thickness is controlled, its surface is in plasma ball edge, is reducing flow field to Buddha's warrior attendant
Ensure the concentration of group needed for growth, the forming core growth of stable super Nano diamond while stone surface erosion.
(4) the plasma surface etching of single crystal diamond seed crystal
Using H2 plasma etchings so that remove diamond surface it is that may be present distortion area or end of dislocation it is same
When generate the step and defect area of single-crystal diamond.The process starts and adjusted technological parameter in plasma and reaches stable shape
State process situ is completed, and is specifically：Hydrogen is 200-300sccm, methane flow 5-25sccm.Due to being passed through methane meeting
Elevate the temperature about 30-50 DEG C, therefore be passed through H2Afterwards, power 2000-3000W, the voltage-controlled temperature processed of adjusting cavity is at 700-740 DEG C
Left and right, etch 10-15 minutes.So that generated while diamond surface distortion area that may be present or end of dislocation is removed
The step and defect area of single-crystal diamond.In actual etching process, hydrogen plasma is to surface distortion and dislocation expansion area
Etch rate is much larger than intact region.Generated while diamond surface distortion area that may be present or end of dislocation is removed
The step and defect area of single-crystal diamond, the direct forming core of Nano diamond and growth are realized dependent on this.Meanwhile to single crystal diamond
The brilliant H2 plasma in situ etching of carpolite causes its surface to form a large amount of H and terminate, and the atom H on dangling bonds will be removed constantly simultaneously
Substituted by the constituent element containing C, keep the ideal interface needed for diamond film, contribute to super nanocrystalline forming core to grow.Suspension
Key is that the carbon source C that methane provides is substituted, and by controlling methane flow, adjusts power cavity pressure, ensures temperature and realize.
(5) deposition growing of the super nanometer layer in surface
Diamond state is not changed after etching, only by controlling power, temperature, chamber pressure and gas flow in quick forming core
The super Nano diamond of n-type doping is formed in growth course.By controlling carbon-containing group concentration in plasma, suppress containing carbon-based
The space propagation of group and diffusion into the surface, in single-crystal diamond surface sp3Suppress abstraction reaction under structure, rely on single-crystal diamond
Step and defect area, realize the direct forming core of Nano diamond and growth, methane flow 5-25sccm so that realize high CH4It is logical
Amount, in the case of preference temperature and relatively low pressure, forms CH in environment3And CH2Matrix, and dimer C2All it is a nanometer Buddha's warrior attendant
Material needed for the growth of stone forming core.The addition of nitrogen can also accelerate growth rate.By controlling nitrating ratio, in Nano diamond
Forming core simultaneously, realizes that the nitrogen-atoms of C-C lattices is incorporated to.Compared to CH4/H2Plasma, additional N2Provide many extra anti-
Answer path and include N new intermediate reaction thing and cause different N2Product can be caused to be formed nanocrystalline.
Further, the pre-polish(ing) time described in step (1) is 24-48 hours.
Further, step (1) the finishing polish step is：On precision diamond polishing disk, control rotating speed for 40 turns/
Minute, carried out respectively 20-30 hours in the case of 80 revs/min, 120 revs/min, 40-60 hours and 80-100 hours are thrown
Light processing.
Further step (2) described pickling processes are that seed crystal sample is placed in into HCl after polishing：H2SO4=1：5 mixing
Boiled in liquid 45 minutes to 1 hour, after use deionized water rinsing；It is clear that each ultrasound in acetone soln and absolute ethyl alcohol is sequentially placed into again
Wash 10-15 minutes, dry up.
Further, the concrete technology condition of step (5) the super Nano diamond for forming n-type doping is：Power
800w-3000w, 400-750 DEG C of temperature, chamber pressure are maintained in the case of 5~15.5kPa, in the hydrogen that flow is 100-500sccm
With the N that 1-60sccm flows are passed through in 5-25sccm methane2。
The key of implementation process of the present invention is：
(1) in single crystal diamond seed crystal surface treatment process, with the polishing of the bortz powder of different-grain diameter and appropriateness
Time is precise polished to the progress of seeded growth face, reaches extremely bright and clean, eliminates graphite-phase, avoids abnormal grain growth or formation from receiving
Rice cluster.
(2) in surface polishing process is realized, except using mechanical polishing method, also use chemical mechanical polishing, etc.
The means such as gas ions auxiliary or composite polishing, carry out accurate planarizing process, to reach rough surface to diamond substrate surface
Degree is less than 1nm.
(3) foundation of single-crystal diamond depositional environment is the geometry of the size design deposition table based on diamond single crystal seed crystal
Structure, between sample surfaces to rooved face height and sample survey edge and microflute spacing ratio are maintained at 0.5-0.7, control molybdenum support
Thickness makes its surface be in plasma ball edge.Foundation and the control environment of the forming core growth of stable super Nano diamond.
(4) the pure H of single crystal diamond seed crystal2Plasma surface etches.It is so that may be present removing diamond surface
The step and defect area of single-crystal diamond are produced while distortion area or end of dislocation.Substantial amounts of hydrogen termination is formed simultaneously.Keep
Ideal interface needed for diamond film, super nanocrystalline forming core is contributed to grow.
(5) in pure H2By controlling carbon-containing group concentration in plasma, methane flow 8-15sccm in environment so that real
Existing high CH4Flux, in the case of preference temperature and relatively low pressure, CH is formed in environment3And C2H matrixes, and dimer C2All
It is the material needed for super Nano diamond forming core growth.
(6) power 800-3000W, 400-750 DEG C of temperature are being set, chamber pressure is maintained at 5~15.5kPa.What is added is highly concentrated
Spend nitrogen source 1-60sccm N2The growth of diamond is can speed up, to ensure that the quick forming core of super Nano diamond grows.Simultaneously
To guarantee to realize N doping while single-crystal diamond surface forms super Nano diamond, the conductive super nanometer of n-type is formed
Diamond layer.
(7) in addition to N doping, different sources of the gas is may be incorporated into and realize that S, P adulterate to form n-type conduction, or the doping such as B
Form p-type electric-conducting.
(8) diamond substrate seed crystal can use HTHP seed crystal or homoepitaxy single-crystal diamond.Equally can also
Using polycrystalline diamond and the composite construction of silicon, GaN, SiC etc. and diamond.
The compared to the prior art possessed beneficial effect of the present invention is：
(1) single-crystal diamond has nature highest thermal conductivity, and forming n-type by high heat conduction single-crystal diamond surface leads
Susceptance rice/super Nano diamond, good n-type conduction is being formed meanwhile, it is capable to realize the high efficiency and heat radiation of device.
(2) deposit super Nano diamond on single-crystal diamond surface, and its bright and clean surface without grinding, add nanometer
The forming core preprocessing means such as bortz powder, biasing, can quick shape using the step of single-crystal diamond after etching in itself and defect
Into Nano diamond crystal grain and crystal boundary, forming core is realized, greatly reduces the complexity of preparation flow.
(3) present invention realizes that single-crystal diamond surface deposits super Nano diamond, avoids interface mismatch between dissimilar substances
And the problem of influenceing performance.The mutually destruction of the diamond caused by ion implanting and CVD growth are adulterated is it also avoid simultaneously
The foreign atom of sum is difficult to ionization and is easy to graphited problem in high temperature environments.The full diamond lattic structure has more excellent
Heat endurance.
(4) diamond single crystal surface forms nano-diamond composite, turns into full diamond lattic structure, or full carbon knot
Structure, in addition to good thermal conductivity and electric conductivity, due to the chemical inertness of diamond carbon material, the full carbon structure will also have
Can be that the exploitation of adverse circumstances electronic device carries with a series of excellent specific properties such as good acid-alkali-corrosive-resisting, radiation hardness
For substrate, the application field of the diamond electronic device has further been widened.
Brief description of the drawings
Fig. 1 is the sample positive and negative Raman of deposition high nitrogenous super Nano diamond thin layer in single-crystal diamond surface of the present invention
(Raman) spectrogram.
Fig. 2 is scanning (SEM) photo of deposition high nitrogenous super Nano diamond thin layer in single-crystal diamond surface of the present invention
Embodiment
Embodiment one
(1) HTHP single crystal diamond seed crystal surface is away from the ratio between cell wall spacing L with seed crystal away from molybdenum bracket height H
0.57, its molybdenum support thickness 5mm, 700 μm of depth of mini longitudinal channels；(2) N is pressed2：(H2+CH4)=1：312 flow-rate ratio：N2For 1sccm, H2For
12sccm、CH4It is 10.6~10.65kPa in chamber pressure for 300sccm, slow power per liter is simultaneously maintained at 1600-1650W；(3) seed crystal
Surface temperature is at 640 DEG C~645 DEG C, sedimentation time 1 hour, after be slowly cooled to room temperature.It is attached that gained sedimentary draws spectrogram to see
Figure, main Raman shift peak is located at：1140,1332,1340,1470 and 1580cm-1Place.Wherein, 1332cm-1What place occurred
It is the characteristic peak of diamond, the halfwidth at the peak is very big, is that typical super Nano diamond carrys out Raman collection of illustrative plates.Surface topography map is such as
Shown in figure two.
Embodiment two
(1) HTHP single crystal diamond seed crystal surface is away from the ratio between cell wall spacing L with seed crystal away from molybdenum bracket height H
0.62, its molybdenum support thickness 8mm, 800 μm of depth of mini longitudinal channels；(2) N is pressed2：(H2+CH4)=30：312 flow-rate ratio：N2For 30sccm, H2
For 12sccm, CH4It is 12.7~12.75kPa in chamber pressure for 300sccm, slow power per liter is simultaneously maintained at 1800-1850W；(3) seed
Brilliant surface temperature is at 680 DEG C~685 DEG C, sedimentation time 1 hour, after be slowly cooled to room temperature.Gained sedimentary draw spectrogram with
Embodiment one is identical.
Embodiment three
(1) HTHP single crystal diamond seed crystal surface is away from the ratio between cell wall spacing L with seed crystal away from molybdenum bracket height H
0.63, its molybdenum support thickness 10mm, 900 μm of depth of mini longitudinal channels；(2) N is pressed2：(H2+CH4)=30：312 flow-rate ratio：N2For 30sccm,
H2For 12sccm, CH4It is 14.1~14.5kPa in chamber pressure for 300sccm, slow power per liter is simultaneously maintained at 2350-2400W or so；
(3) seed crystal face temperature is at 745 DEG C~755 DEG C, sedimentation time 1 hour, after be slowly cooled to room temperature.Gained sedimentary draws spectrum
Figure is identical with embodiment one.
Embodiment four
(1) HTHP single crystal diamond seed crystal surface is away from the ratio between cell wall spacing L with seed crystal away from molybdenum bracket height H
0.60, its molybdenum support thickness 15mm, 1500 μm of depth of mini longitudinal channels；(2) N is pressed2：(H2+CH4)=60：312 flow-rate ratio：N2For
60sccm、H2For 12sccm, CH4It is 14.5~15kPa in chamber pressure for 300sccm, slow power per liter is simultaneously maintained at 2350-2400W
Left and right；(3) seed crystal face temperature is at 745 DEG C~755 DEG C, sedimentation time 1 hour, after be slowly cooled to room temperature.Gained sedimentary
Draw spectrogram identical with embodiment one.
Claims (6)
1. a kind of preparation method of single-crystal diamond surface in situ n-type semiconductor, it is characterised in that pass through microwave plasma
Etching directly generates the conductive super Nano diamond thin layer of n-type on single-crystal diamond surface with gas phase deposition technology, and processing step is
It is as follows：
(1) grinding and polishing of single crystal diamond seed crystal
With the diadust that granularity is 40,20,10 and 2.5, pre-polish(ing) is carried out；After to be placed in precision diamond polishing disk enterprising
Row finishing polish, realize that surface roughness is less than 1nm after polishing；
(2) single crystal diamond seed crystal pickling processes
(3) foundation of single-crystal diamond depositional environment
Single crystal diamond substrate is placed in the square microflute of molybdenum support, sample surfaces to rooved face height survey edge and microflute with sample
Spacing ratio is maintained between 0.5-0.7, and molybdenum support thickness is in 5-15mm, and depth of mini longitudinal channels is between 500 microns -1500 microns；And
Molybdenum support is placed on copper heat conduction base station and ensures that heat scatters and disappears；
(4) the plasma surface etching of single crystal diamond seed crystal
Using H2Plasma etching so that produced while diamond surface distortion area that may be present or end of dislocation is removed
The step and defect area of single-crystal diamond are given birth to；
(5) deposition growing of the super nanometer layer in surface
Diamond state is not changed after etching, only by controlling power, temperature, chamber pressure and gas flow to be grown in quick forming core
During formed n-type doping super Nano diamond.
A kind of 2. preparation method of single-crystal diamond surface in situ n-type semiconductor as claimed in claim 1, it is characterised in that step
Suddenly the pre-polish(ing) time described in (1) is 24-48 hours.
A kind of 3. preparation method of single-crystal diamond surface in situ n-type semiconductor as claimed in claim 1, it is characterised in that step
Suddenly (1) described finishing polish step is：On precision diamond polishing disk, rotating speed is controlled as 40 revs/min, 80 revs/min, 120
Carried out respectively in the case of rev/min 20-30 hours, 40-60 hours and 80-100 hours are processed by shot blasting.
A kind of 4. preparation method of single-crystal diamond surface in situ n-type semiconductor as claimed in claim 1, it is characterised in that step
Suddenly (2) described pickling processes are that seed crystal sample is placed in into HCl after polishing：H2SO4=1：Boiled in 5 mixed liquor 45 minutes small to 1
When, after use deionized water rinsing；Each ultrasonic cleaning 10-15 minute, drying are sequentially placed into acetone soln and absolute ethyl alcohol again.
A kind of 5. preparation method of single-crystal diamond surface in situ n-type semiconductor as claimed in claim 1, it is characterised in that step
Suddenly (4) are described uses H2Plasma etch process is：Hydrogen is 200-300sccm, is being passed through H2Afterwards, power is set
2000-3000W, the voltage-controlled temperature processed of adjusting cavity etch 10-15 minutes at 700-740 DEG C or so.
A kind of 6. preparation method of single-crystal diamond surface in situ n-type semiconductor as claimed in claim 1, it is characterised in that step
Suddenly the concrete technology condition of (5) described super Nano diamond for forming n-type doping is：Power 800w-3000w, temperature 400-750
DEG C, chamber pressure is maintained in the case of 5~15.5kPa, is passed through in the hydrogen and 5-25sccm methane that flow is 100-500sccm
The N of 1-60sccm flows2。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710363710.4A CN107419329B (en) | 2017-05-22 | 2017-05-22 | The preparation method of the full carbon structure of single-crystal diamond surface in situ n-type semiconductorization |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710363710.4A CN107419329B (en) | 2017-05-22 | 2017-05-22 | The preparation method of the full carbon structure of single-crystal diamond surface in situ n-type semiconductorization |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107419329A true CN107419329A (en) | 2017-12-01 |
| CN107419329B CN107419329B (en) | 2019-08-27 |
Family
ID=60427965
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710363710.4A Active CN107419329B (en) | 2017-05-22 | 2017-05-22 | The preparation method of the full carbon structure of single-crystal diamond surface in situ n-type semiconductorization |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107419329B (en) |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108411276A (en) * | 2018-04-08 | 2018-08-17 | 河南佰特科技有限公司 | A kind of crystal seed implantation methods of cvd diamond thick film |
| CN108588822A (en) * | 2018-04-08 | 2018-09-28 | 北京科技大学 | The method of uninterrupted dynamic in-situ synthetic single crystal and super nano-diamond composite |
| CN109537052A (en) * | 2018-11-27 | 2019-03-29 | 西安碳星半导体科技有限公司 | A kind of pretreated method of CVD single crystal diamond film |
| CN110281142A (en) * | 2019-06-20 | 2019-09-27 | 山东大学 | Diamond seed preparation method, diamond seed and monocrystalline |
| CN110571310A (en) * | 2019-09-20 | 2019-12-13 | 西安交通大学 | (100) Ohmic contact forming method for oriented n-type monocrystal diamond electrode |
| CN110600366A (en) * | 2019-09-20 | 2019-12-20 | 西安交通大学 | (100) Crystal orientation diamond n-channel junction field effect transistor and preparation method thereof |
| CN111088523A (en) * | 2020-01-07 | 2020-05-01 | 北京科技大学 | Method for heteroepitaxial growth of large-size single crystal diamond |
| CN111172508A (en) * | 2020-02-24 | 2020-05-19 | 北京科技大学 | Method for improving pressure limit of diamond opposite-top anvil |
| CN111206280A (en) * | 2020-01-07 | 2020-05-29 | 北京科技大学 | Method for epitaxial growth of high-quality large-size single crystal diamond |
| CN113278947A (en) * | 2021-05-27 | 2021-08-20 | 杭州超然金刚石有限公司 | Crystal diamond nitrogen-doped semiconductor composite material and preparation method thereof |
| CN113337887A (en) * | 2021-06-01 | 2021-09-03 | 南京大学 | Application of laser-assisted MPCVD method in enhancing SiV color center of single crystal diamond and single crystal diamond with SiV color center |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104878447A (en) * | 2015-06-04 | 2015-09-02 | 哈尔滨工业大学 | Seed crystal-substrate in-situ connection method for homoepitaxial-growth monocrystalline diamond |
| CN105331948A (en) * | 2015-09-25 | 2016-02-17 | 北京科技大学 | Manufacturing method for surface type-P conductive diamond heat sink material |
| CN106012003A (en) * | 2016-06-07 | 2016-10-12 | 武汉工程大学 | Two-dimensional expansion method for CVD monocrystal diamond |
| CN106048719A (en) * | 2016-07-08 | 2016-10-26 | 武汉大学 | Substrate holder and method for growing monocrystalline diamond |
-
2017
- 2017-05-22 CN CN201710363710.4A patent/CN107419329B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104878447A (en) * | 2015-06-04 | 2015-09-02 | 哈尔滨工业大学 | Seed crystal-substrate in-situ connection method for homoepitaxial-growth monocrystalline diamond |
| CN105331948A (en) * | 2015-09-25 | 2016-02-17 | 北京科技大学 | Manufacturing method for surface type-P conductive diamond heat sink material |
| CN106012003A (en) * | 2016-06-07 | 2016-10-12 | 武汉工程大学 | Two-dimensional expansion method for CVD monocrystal diamond |
| CN106048719A (en) * | 2016-07-08 | 2016-10-26 | 武汉大学 | Substrate holder and method for growing monocrystalline diamond |
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108588822B (en) * | 2018-04-08 | 2019-12-17 | 北京科技大学 | Method for uninterrupted dynamic in-situ synthesis of single crystal and ultra-nano diamond composite structure |
| CN108588822A (en) * | 2018-04-08 | 2018-09-28 | 北京科技大学 | The method of uninterrupted dynamic in-situ synthetic single crystal and super nano-diamond composite |
| CN108411276A (en) * | 2018-04-08 | 2018-08-17 | 河南佰特科技有限公司 | A kind of crystal seed implantation methods of cvd diamond thick film |
| CN109537052A (en) * | 2018-11-27 | 2019-03-29 | 西安碳星半导体科技有限公司 | A kind of pretreated method of CVD single crystal diamond film |
| CN110281142A (en) * | 2019-06-20 | 2019-09-27 | 山东大学 | Diamond seed preparation method, diamond seed and monocrystalline |
| CN110600366A (en) * | 2019-09-20 | 2019-12-20 | 西安交通大学 | (100) Crystal orientation diamond n-channel junction field effect transistor and preparation method thereof |
| CN110571310A (en) * | 2019-09-20 | 2019-12-13 | 西安交通大学 | (100) Ohmic contact forming method for oriented n-type monocrystal diamond electrode |
| CN110571310B (en) * | 2019-09-20 | 2020-11-17 | 西安交通大学 | Ohmic contact forming method for (100) oriented n-type monocrystal diamond electrode |
| CN110600366B (en) * | 2019-09-20 | 2021-06-18 | 西安交通大学 | (100) Crystal orientation diamond n-channel junction field effect transistor and preparation method thereof |
| CN111088523A (en) * | 2020-01-07 | 2020-05-01 | 北京科技大学 | Method for heteroepitaxial growth of large-size single crystal diamond |
| CN111206280A (en) * | 2020-01-07 | 2020-05-29 | 北京科技大学 | Method for epitaxial growth of high-quality large-size single crystal diamond |
| CN111088523B (en) * | 2020-01-07 | 2021-04-20 | 北京科技大学 | Method for heteroepitaxial growth of large-size single crystal diamond |
| CN111172508A (en) * | 2020-02-24 | 2020-05-19 | 北京科技大学 | Method for improving pressure limit of diamond opposite-top anvil |
| CN113278947A (en) * | 2021-05-27 | 2021-08-20 | 杭州超然金刚石有限公司 | Crystal diamond nitrogen-doped semiconductor composite material and preparation method thereof |
| CN113337887A (en) * | 2021-06-01 | 2021-09-03 | 南京大学 | Application of laser-assisted MPCVD method in enhancing SiV color center of single crystal diamond and single crystal diamond with SiV color center |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107419329B (en) | 2019-08-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107419329B (en) | The preparation method of the full carbon structure of single-crystal diamond surface in situ n-type semiconductorization | |
| CN108588822B (en) | Method for uninterrupted dynamic in-situ synthesis of single crystal and ultra-nano diamond composite structure | |
| CN102102220B (en) | Preparation method of graphene on diamond (111) surface | |
| JP4786223B2 (en) | Epitaxial silicon carbide single crystal substrate and manufacturing method thereof | |
| TW201723212A (en) | SiC composite substrate and method for manufacturing same | |
| TW200303580A (en) | Production method of sic monitor wafer | |
| CN102534808B (en) | Method for obtaining high-quality silicon carbide surfaces | |
| JPWO2010087518A1 (en) | Epitaxial silicon carbide single crystal substrate and manufacturing method thereof | |
| CN110863243B (en) | Secondary epitaxial method for preparing high-quality diamond single crystal by adopting nano structure | |
| JP6742477B2 (en) | Epitaxial silicon carbide single crystal wafer manufacturing method and epitaxial silicon carbide single crystal wafer | |
| US20230260841A1 (en) | Method for producing a composite structure comprising a thin layer of monocrystalline sic on a carrier substrate of polycrystalline sic | |
| JP2011009746A (en) | Method of manufacturing epitaxially coated semiconductor wafer | |
| CN104851781B (en) | Preparation method of N-type low-deflection-angle silicon carbide epitaxial wafer | |
| KR20140117277A (en) | SINGLE-CRYSTAL 4H-SiC SUBSTRATE AND METHOD FOR MANUFACTURING THE SAME | |
| CN111118471A (en) | Preparation method of high-quality polycrystalline diamond film | |
| CN106783540A (en) | The method for reducing epitaxial wafer surface scratch | |
| CN113089093B (en) | Method for forming diamond semiconductor structure | |
| JP5786759B2 (en) | Method for manufacturing epitaxial silicon carbide wafer | |
| Geis | Growth of textured diamond films on foreign substrates from attached seed crystals | |
| CN111733454A (en) | Separation method of CVD homoepitaxy diamond large single crystal based on boron-doped transition layer | |
| CN113964016A (en) | Method for manufacturing silicon carbide epitaxial wafer | |
| Vikharev et al. | Combined single-crystalline and polycrystalline CVD diamond substrates for diamond electronics | |
| CN114032616B (en) | SiC step flow low-speed growth method for chemical potential regulation growth monomer under non-equilibrium condition | |
| CN113174582A (en) | Method for preparing diamond film by microwave plasma chemical vapor deposition method | |
| CN115161767B (en) | Preparation method of (100)/(111) orientation composite high-performance diamond semiconductor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |