CN105525344A - Seed crystal tray and base station assembly for diamond monocrystal homoepitaxy, and application thereof - Google Patents
Seed crystal tray and base station assembly for diamond monocrystal homoepitaxy, and application thereof Download PDFInfo
- Publication number
- CN105525344A CN105525344A CN201510974331.XA CN201510974331A CN105525344A CN 105525344 A CN105525344 A CN 105525344A CN 201510974331 A CN201510974331 A CN 201510974331A CN 105525344 A CN105525344 A CN 105525344A
- Authority
- CN
- China
- Prior art keywords
- seed crystal
- tray
- diamond
- diamond single
- epitaxy
- 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
- 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
-
- 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
- C30B25/12—Substrate holders or susceptors
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention is applicable to the technical field of diamond synthesis, and provides a seed crystal tray and base station assembly for diamond monocrystal homoepitaxy, and an application thereof. The seed crystal tray is placed on a water cooling stage of a microwave plasma chemical vapor deposition device, and a through hole for placing a seed crystal is formed in the center of the seed crystal tray. The base station assembly for diamond monocrystal homoepitaxy includes the water cooling stage and the seed crystal tray arranged on the water cooling stage, and the seed crystal tray is the seed crystal tray for diamond monocrystal homoepitaxy.
Description
Technical field
The invention belongs to Diamond Synthesizing Technology field, particularly relate to a kind of seed crystal tray for diamond single crystal iso-epitaxy, base station assembly and application thereof.
Background technology
Diamond integrates numerous excellent properties, there is high hardness, thermal conductivity, the advantages such as wide transmitted light bands of a spectrum, broad-band gap and high electron hole mobility, can be widely used in the fields such as cutter, coating, optical window and acoustic sensor, semi-conductor and electron device.At present, adamantine demand is large, and natural diamond reserves are little, and therefore, synthesis large size, high-quality diamond single crystal just seem particularly urgent.Microwave plasma CVD (MPCVD) method has that electrodeless pollution, equipment are stable, plasma density is concentrated and indiffusion, sample quality such as effectively can to repeat at the multiple advantage, being applicable to very much for growing high-quality, highly purified single-crystal diamond, is one of the most promising method of current diamond synthesis.In MPCVD method, the design of seed crystal tray determines that whether the distribution of growth temperature, plasma distribution and carbon source is even, plays key effect in diamond growth process.
The seed crystal tray that tradition uses is made up of metal molybdenum, and its stable in properties is pollution-free, and heat conduction is fast.The advantages such as seed crystal tray center has pit sulculus to place diamond seed, is placed on the water-cooled platform in resonant cavity, obtains growth temperature, have quick heating by input microwave power and pressure, workable.But there is the problem that growth temperature is difficult to be effectively controlled in the seed crystal tray that tradition uses.
Chinese patent CN204281889 discloses a kind of novel seed crystal tray for rapid growth of diamond single-crystal, and its tray center end is provided with pit, and pit exit end is be connected by chamfered transition with pallet end face place horizontal plane.This design can reduce the discontinuity of electromagnetic field in process of growth, suppresses marginal growth too fast, improves diamond quality.But, when using this seed crystal tray growing diamond, in process of growth, easy deposited graphite between seed crystal and groove, between substrate tray and water-cooled platform.The graphite of deposition can change the heat transfer path between diamond and water-cooled platform, thus directly affects heat-conducting effect, and the growth temperature of seed crystal is constantly raised, and is difficult to ensure the long stable growth condition of crystal, hinders the synthesis of large dimond monocrystalline.
A kind of method of control surface temperature when Chinese patent CN104775154A discloses isoepitaxial growth single-crystal diamond, the method welds goldleaf at seed crystal with in the middle of seed crystal tray, simultaneously, in order to prevent, heat conduction is too fast adds heat insulation silk under substrate tray, thus ensure that diamond and uniform plasma exposure, and then reach the homogeneity in temperature field, diamond film is obtained better.Although this invention effectively can suppress contacting of graphite and seed crystal and seed crystal tray, provide stable growth temperature.But the goldleaf welded between seed crystal with seed crystal tray groove there are certain requirements growth temperature, goldleaf can melt at about 1000 DEG C, and this limits deposition temperature range when using the method to a certain extent.
Summary of the invention
The object of the present invention is to provide a kind of seed crystal tray for diamond single crystal iso-epitaxy, be intended to solve seed temperature in existing MPCVD (microwave plasma CVD) system simultaneously and be difficult to the problem be effectively controlled.
Another object of the present invention is to provide a kind of base station assembly for diamond single crystal iso-epitaxy, comprise above-mentioned seed crystal tray.
Another object of the present invention is that providing a kind of uses above-mentioned base station assembly to prepare the method for diamond single crystal.
The present invention is achieved in that a kind of seed crystal tray for diamond single crystal iso-epitaxy, and described seed crystal tray is placed on the water-cooled platform of microwave plasma CVD device, and described seed crystal tray center offers the perforation for placing seed crystal.
Accordingly, a kind of base station assembly for diamond single crystal iso-epitaxy, comprise water-cooled platform and be arranged on the seed crystal tray on described water-cooled platform, described seed crystal tray is the above-mentioned seed crystal tray for diamond single crystal iso-epitaxy.
And, a kind ofly use above-mentioned base station assembly to prepare the method for diamond single crystal, comprise the following steps:
After described seed crystal and seed crystal tray are carried out surface cleaning process respectively, described seed crystal tray is placed on described water-cooled platform, described seed crystal is placed in the perforation of described seed crystal tray;
Off-response chamber door, the air pressure being pumped to described reaction chamber is 10
-3-10
-4pa, passes into hydrogen, and input pressure and microwave power, etch described seed crystal with hydrogen plasma;
Pass into methane gas after etching terminates, regulation and control pressure and power input regulate diamond film temperature, prepare diamond single crystal.
Seed crystal tray for diamond single crystal iso-epitaxy provided by the invention, described seed crystal tray center offers the perforation for placing seed crystal, seed crystal can be realized contact with water-cooled platform, and described seed crystal does not directly contact with described seed crystal tray, thus avoid the temperature drift that deposited graphite causes, for seed crystal provides stable effective growing environment, make diamond single crystal remain on continued propagation under high power density, obtain excellent diamonds monocrystalline.Meanwhile, the concave surface of described seed crystal tray can suppress the too fast growth of seed crystal edges, effectively suppresses twin etc. to affect the factor of diamond quality, improves the quality of diamond single crystal further.In addition, the seed crystal tray for diamond single crystal iso-epitaxy provided by the invention, do not need welding goldleaf to suppress graphite on the impact of temperature, therefore, growth temperature by the restriction of goldleaf fusing point, does not extend its deposition temperature range.
Base station assembly for diamond single crystal iso-epitaxy provided by the invention, containing above-mentioned seed crystal tray, therefore, can temperature drift that effectively graphite causes in Developing restraint process, the too fast growth in further suppression edge, for seed crystal provides stable effective growing environment, make diamond single crystal remain on continued propagation under high power density, obtain excellent diamonds monocrystalline.
The method of diamond single crystal prepared by use base station assembly provided by the invention, only described seed crystal need be placed in the perforation of described seed crystal tray, arranges the preparation that the parameters such as working gas, pressure, power can realize standby excellent diamonds monocrystalline.The method is simple to operate, and controllability is strong, is easy to the industrialization realizing single-crystal diamond.
Accompanying drawing explanation
Fig. 1 is the seed crystal tray structural representation for diamond single crystal iso-epitaxy that the embodiment of the present invention provides;
Fig. 2 is the base station unit construction schematic diagram for diamond single crystal iso-epitaxy that the embodiment of the present invention provides;
Fig. 3 is the single-crystal diamond shape appearance figure that the embodiment of the present invention 1 provides;
Fig. 4 is the Raman spectrogram of the single-crystal diamond that the embodiment of the present invention 1 provides.
Embodiment
In order to make the technical problem to be solved in the present invention, technical scheme and beneficial effect clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Composition graphs 1, embodiments provide a kind of seed crystal tray 1 for diamond single crystal iso-epitaxy, described seed crystal tray 1 is placed on the water-cooled platform 2 of microwave plasma CVD device, and described seed crystal tray 1 center offers the perforation 11 for placing seed crystal.
Concrete, the MPCVD seed crystal tray material that the material of described seed crystal tray 1 can select this area conventional, the embodiment of the present invention preferably adopts refractory metal material molybdenum to prepare described seed crystal tray 1.The shape of described seed crystal tray 1 adopts symmetrical structure, preferably adopts to utilize to obtain the cylindric of uniform growth temperature, plasma distribution and carbon source substep.The embodiment of the present invention can select the seed crystal tray 1 of different thickness according to seed crystal thickness and growth technique.As further preferred embodiment, the diameter R of described seed crystal tray 1 is 25-50mm, and pallet thickness D is 3-20mm.Concrete, the thickness of described seed crystal represents with d, and the thickness of described seed crystal tray 1 is preferably 1/2d-3/2d, thus both can ensure that growth remained at high power density, seed crystal edges can be suppressed again to grow, finally grow higher caliper, high-quality diamond.
In the embodiment of the present invention, the center of described seed crystal tray 1 offers perforation 11, and described perforation 11 can realize seed crystal and contact with described the direct of water-cooled platform 2, and security deposit's hard rock temperature is unlikely to too high, improve power density, to reach the requirement of single-crystal diamond high power density growth.In addition, the perforation at described seed crystal tray 1 center can also suppress the extension of seed crystal edges, improves growth quality, make in the whole process of single-crystal diamond, growth temperature is stablized, and adamantine growth remains in steady state, finally realizes the synthesis of high quality, high thickness diamond single crystal.Shape due to described seed crystal is tended to square more, therefore, deposits for the ease of the stable of described seed crystal, and as preferred embodiment, described perforation 11 is square perforation.Further, the length of side of described square perforation should with the size of described seed crystal for foundation sets, unsuitable excessive or too small, to ensure to leave certain space (namely described seed crystal does not directly contact with described seed crystal tray) between described seed crystal and described seed crystal tray, to prevent the surface growth polycrystalline diamond at described seed crystal tray, affect the quality of single-crystal diamond.As preferred embodiment, the length of side L of described square perforation is 3-10mm.
In the embodiment of the present invention, seed crystal is placed in described perforation 11 when directly contacting with described water-cooled platform 2, because diamond heat-conducting is very fast, causes seed crystal face temperature described in process of growth to be difficult to improve, thus affect growth efficiency and the quality of single-crystal diamond.In order to effectively regulate described seed crystal face temperature, as preferred embodiment, between described seed crystal and described water-cooled platform 2, be provided with heat insulation silk.Described heat insulation silk can under the prerequisite avoiding deposited graphite to affect temperature, and the temperature of seed crystal face described in flexible, regulates and controls different growth temperature.The material of described heat insulation silk, specification following for the base station assembly of diamond single crystal iso-epitaxy in be described in detail.
The seed crystal tray for diamond single crystal iso-epitaxy that the embodiment of the present invention provides, first, described seed crystal tray center offers the perforation for placing seed crystal, seed crystal can be realized contact with water-cooled platform, and described seed crystal does not directly contact with described seed crystal tray, thus avoid the temperature drift that deposited graphite causes, ensure that in process of growth, power density is continual and steady, for seed crystal provides stable effective growing environment, enable diamond single crystal stablize continued propagation, obtain excellent diamonds monocrystalline.Meanwhile, the concave surface of described seed crystal tray can suppress the too fast growth of seed crystal edges, effectively suppresses twin etc. to affect the factor of diamond quality, improves the quality of diamond single crystal further.The embodiment of the present invention highly can also select the seed crystal tray of different thickness according to described seeded growth, ensure under high power density, realize thicker adamantine synthesis.
Secondly, the embodiment of the present invention can place heat insulation silk under diamond seed, can prevent described seed crystal from directly contacting with described water-cooled platform, thus avoids making the too low problem affecting growth efficiency and diamond single crystal quality of diamond temperature because heat conduction is too fast.
Again, the embodiment of the present invention can according to select different heat insulation silk material, diameter regulates diamond single crystal iso-epitaxy time surface growth temperature (surface growth temperature-controllable during diamond single crystal iso-epitaxy), and controllable scope is larger.Can ensure like this to have larger growth temperature range of choice, the temperature drift because graphite deposits produces can be avoided again, simplify experimental implementation, under making seed crystal realize high power density, stablize continued propagation.
In addition, the seed crystal tray for diamond single crystal iso-epitaxy that the embodiment of the present invention provides, do not need welding goldleaf to suppress graphite on the impact of temperature, therefore, growth temperature by the restriction of goldleaf fusing point, does not extend its deposition temperature range.
Accordingly, composition graphs 2, the embodiment of the present invention additionally provides a kind of base station assembly for diamond single crystal iso-epitaxy, and the seed crystal tray 1 comprising water-cooled platform 2 and be arranged on described water-cooled platform 2, described seed crystal tray 1 is the above-mentioned seed crystal tray 1 for diamond single crystal iso-epitaxy.
Concrete, the setting of the structure of described seed crystal tray 1, shape and described perforation as mentioned before, in order to save length, repeats no more herein.
In the embodiment of the present invention, as previously mentioned, seed crystal is placed in described perforation 11 when directly contacting with described water-cooled platform 2, because diamond heat-conducting is very fast, cause seed crystal face temperature described in process of growth to be difficult to improve, thus affect growth efficiency and the quality of single-crystal diamond.In order to effectively regulate described seed crystal face temperature, as preferred embodiment, be provided with the heat insulation silk 3 for regulating seed crystal face temperature in described perforation, described heat insulation silk 3 is arranged on described water-cooled platform 2 surface of described punch position.The deposition that described heat insulation silk avoids graphite causes temperature drift, and further, can under the prerequisite avoiding deposited graphite to affect temperature, the temperature of seed crystal face described in flexible, regulates and controls different growth temperature.
The length of described heat insulation silk 3 should match with the size of described perforation, and the diameter of described heat insulation silk 3 is regulated by the needs of described seed crystal face temperature; The embodiment of the present invention can also select the heat insulation silk 3 of different size to regulate the distance between described seed crystal and described water-cooled platform 2, thus realizes different growth techniques.Common, when described seed crystal needs to arrange higher surface temperature, select the described heat insulation silk 3 of diameter comparatively large (heat conduction is relatively poor); When described seed crystal needs to arrange lower surface temperature, select the described heat insulation silk 3 of diameter less (heat conduction is relatively better).As preferred embodiment, the length of described heat insulation silk 3 is 1-10mm, and diameter is 0.1-0.8mm.Concrete, the length of described heat insulation silk 3 can be the concrete numerical value such as 1mm, 2mm, 3mm, 4mm, 5mm, 6mm, 7mm, 8mm, 9mm, 10mm, and diameter can be the concrete numerical value such as 0.1mm, 0.2mm, 0.3mm, 0.4mm, 0.5mm, 0.6mm, 0.7mm, 0.8mm.
In the embodiment of the present invention, for the ease of the stable placement of described seed crystal, described heat insulation silk 3 is preferably set to V-type or ellipse.The described heat insulation silk 3 made will ensure that heat insulation silk is smooth, to ensure that described seed crystal can keep level above being placed on, with uniform plasma exposure.Preferably, the material of described heat insulation silk 3 is molybdenum filament, tantalum wire or tungsten filament, more preferably good heat conduction effect, high temperature resistant molybdenum filament.Preferred described heat insulation silk 3 has the characteristic of uniform in material, makes described seed crystal and uniform plasma exposure, ensures the even of described seed crystal face temperature and carbon source density, the quality of further bonding diamond.
The base station assembly for diamond single crystal iso-epitaxy that the embodiment of the present invention provides, containing above-mentioned seed crystal tray, therefore, can temperature drift that effectively graphite causes in Developing restraint process, the too fast growth in further suppression edge, for seed crystal provides stable effective growing environment, make diamond single crystal remain on continued propagation under high power density, obtain excellent diamonds monocrystalline.
Secondly, the embodiment of the present invention can place heat insulation silk under diamond seed, can prevent described seed crystal from directly contacting with described water-cooled platform, thus avoids making the too low problem affecting growth efficiency and diamond single crystal quality of diamond temperature because heat conduction is too fast.
Again, the embodiment of the present invention can according to material, the diameter selecting different heat insulation silk, regulate the surface growth temperature (surface growth temperature-controllable during diamond single crystal iso-epitaxy) during diamond single crystal iso-epitaxy, meet the growth technique requirement of differing temps, have larger thermal creep stress scope.Can ensure like this to have larger growth temperature range of choice, the temperature drift because graphite deposits produces can be avoided again, simplify experimental implementation, under making seed crystal realize high power density, stablize continued propagation.
And, embodiments provide and a kind ofly use above-mentioned base station assembly to prepare the method for diamond single crystal, comprise the following steps:
S01., after described seed crystal and seed crystal tray being carried out surface cleaning process respectively, described seed crystal tray is placed on described water-cooled platform, described seed crystal is placed in the perforation of described seed crystal tray;
S02. off-response chamber door, the air pressure being pumped to described reaction chamber is 10
-3-10
-4pa, passes into hydrogen, and input pressure and microwave power, etch described seed crystal with hydrogen plasma;
S03. etching passes into methane gas after terminating, and regulation and control pressure and power input regulate diamond film temperature, prepare diamond single crystal.
Concrete, in above-mentioned steps S01, described seed crystal and seed crystal tray, respectively through showing clean, ensure described seed crystal and seed crystal tray cleaning, pollution-free.Concrete, the method for described seed crystal face clean is preferably: described seed crystal is placed in successively mixing acid, deionized water, acetone ultrasonic cleaning; The method of described seed crystal tray surface cleaning process is preferably: described seed crystal tray is placed in acetone ultrasonic cleaning.
Described seed crystal tray is placed on described water-cooled platform, described seed crystal is placed in the perforation of described seed crystal tray, the high power density of single crystal diamond film can be ensured.As preferred embodiment, between described seed crystal and water-cooled platform, place heat insulation silk.Concrete, described seed crystal tray is placed on described water-cooled platform, the described seed crystal tray of different thickness and the heat insulation silk of different size is selected according to described seed crystal thickness and growth technique, described heat insulation silk is placed in the central hole of described seed crystal tray, again the described seed crystal cleaned up is placed on described heat insulation silk, the described seed crystal of steady placement, ensures and uniform plasma exposure, homogeneous temperature.Preferably, heat insulation silk is made V-type or ellipse to meet different growth techniques.
In above-mentioned steps S02, described in process of bleeding mechanical pump and molecular pump can be used respectively to bleed, the air pressure being pumped to described reaction chamber is 10
-3-10
-4pa, and ensure that in reaction cavity, foreign gas is discharged.
In above-mentioned steps S03, pass into methane gas after etching terminates, the throughput ratio of setting methane and hydrogen sets methane concentration, preferably, the volumetric concentration of described methane is between 1%-10%, specifically can be 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%.Regulation and control pressure and power input regulate diamond film temperature, between the preferred 800-1300 of described growth temperature DEG C, specifically can be 800 DEG C, 900 DEG C, 1000 DEG C, 1100 DEG C, 1200 DEG C, 1300 DEG C.
After growth terminates, the means such as opticmicroscope, Raman spectrum can be adopted to characterize diamond quality.
The method of diamond single crystal prepared by the use base station assembly that the embodiment of the present invention provides, and only described seed crystal need be placed in the perforation of described seed crystal tray, arranges the preparation that the parameters such as working gas, pressure, power can realize standby excellent diamonds monocrystalline.The method is simple to operate, and controllability is strong, is easy to the industrialization realizing single-crystal diamond.
Be described below in conjunction with specific embodiment.
Embodiment 1
Use above-mentioned base station assembly to prepare a method for diamond single crystal, comprise the following steps:
S11. after described seed crystal and seed crystal tray being carried out surface cleaning process respectively, described seed crystal tray is placed on described water-cooled platform, heat insulation silk is placed in the perforation of described seed crystal tray, described seed crystal is placed on heat insulation silk; Concrete,
Select seed crystal, thickness is 1.07mm, at mixing acid (HNO
3: H
2sO
4=1:1) middle ultrasonic cleaning 30min, removing seed crystal face metal impurities; Then be placed on ultrasonic cleaning 30min in deionization water-bath and remove remaining acid solution; Subsequently by seed crystal in acetone ultrasonic 30min wash away the impurity such as organism.Meanwhile, by seed crystal tray described in the embodiment of the present invention also ultrasonic cleaning 30min in acetone, obtain clean seed crystal and seed crystal tray;
Select molybdenum filament as heat insulation silk, molybdenum filament diameter is 0.18mm, and molybdenum filament is rolled over shape in 90 °;
Be placed on water-cooled platform by the seed crystal tray cleaned up, the smooth perforation being placed in seed crystal tray center of the molybdenum filament made, then puts into ready seed crystal.
S12. off-response cavity, is evacuated to 10
-4pa, passes into hydrogen 300sccm, uses hydrogen plasma etched seed.Apply suitable pressure and power, seed temperature remains on 850 DEG C, etches one hour.Pass into methane after etching terminates, methane concentration is 8%, regulating power and pressure, ensures that seed crystal is 950 DEG C of growths.Now because there is heat insulation silk between seed crystal and water-cooled platform, the graphite of deposition can not impact seed temperature, and whole process of growth keeps stable;
S13. after growing 92h, seed crystal is placed in thicker seed crystal tray and grows, keep high power density, after 25h, seed crystal CVD layer thickness is 3.08mm.
After growth terminates, adopt the means such as opticmicroscope, Raman spectrum to characterize diamond quality, as shown in Figure 3, Raman spectrogram as shown in Figure 4 for the pattern of the single-crystal diamond that the embodiment of the present invention obtains, as seen from the figure, the pattern of described single-crystal diamond is good, purity is high.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. for a seed crystal tray for diamond single crystal iso-epitaxy, described seed crystal tray is placed on the water-cooled platform of microwave plasma CVD device, it is characterized in that, described seed crystal tray center offers the perforation for placing seed crystal.
2., as claimed in claim 1 for the seed crystal tray of diamond single crystal iso-epitaxy, it is characterized in that, described perforation is square perforation, and the length of side of described square perforation is 3-10mm.
3., as claimed in claim 1 or 2 for the seed crystal tray of diamond single crystal iso-epitaxy, it is characterized in that, the thickness of described seed crystal represents with d, and the thickness of described seed crystal tray is 1/2d-3/2d.
4. the base station assembly for diamond single crystal iso-epitaxy, comprise water-cooled platform and be arranged on the seed crystal tray on described water-cooled platform, it is characterized in that, described seed crystal tray is the arbitrary described seed crystal tray for diamond single crystal iso-epitaxy of claim 1-3.
5. as claimed in claim 4 for the base station assembly of diamond single crystal iso-epitaxy, it is characterized in that, being provided with the heat insulation silk for regulating seed crystal face temperature in described perforation, described heat insulation silk is arranged on the described water-cooled platform surface of described punch position.
6., as claimed in claim 5 for the base station assembly of diamond single crystal iso-epitaxy, it is characterized in that, the length of described heat insulation silk is 1-10mm, and diameter is 0.1-0.8mm.
7., as claimed in claim 6 for the base station assembly of diamond single crystal iso-epitaxy, it is characterized in that, described heat insulation silk is set to V-type or ellipse.
8. the base station assembly for diamond single crystal iso-epitaxy as described in as arbitrary in claim 5-7, it is characterized in that, described heat insulation silk material is molybdenum filament, tantalum wire or tungsten filament.
9. use the arbitrary described base station assembly of claim 4-8 to prepare a method for diamond single crystal, comprise the following steps:
After described seed crystal and seed crystal tray are carried out surface cleaning process respectively, described seed crystal tray is placed on described water-cooled platform, described seed crystal is placed in the perforation of described seed crystal tray;
Off-response chamber door, the air pressure being pumped to described reaction chamber is 10
-3-10
-4pa, passes into hydrogen, and input pressure and microwave power, etch described seed crystal with hydrogen plasma;
Pass into methane gas after etching terminates, regulation and control pressure and power input regulate diamond film temperature, prepare diamond single crystal.
10. the method using base station assembly to prepare diamond single crystal as claimed in claim 9, is characterized in that, between described seed crystal and water-cooled platform, place heat insulation silk.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510974331.XA CN105525344B (en) | 2015-12-23 | 2015-12-23 | Seed crystal tray, base station component and its application for diamond single crystal homoepitaxy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510974331.XA CN105525344B (en) | 2015-12-23 | 2015-12-23 | Seed crystal tray, base station component and its application for diamond single crystal homoepitaxy |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105525344A true CN105525344A (en) | 2016-04-27 |
| CN105525344B CN105525344B (en) | 2018-05-01 |
Family
ID=55767858
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510974331.XA Active CN105525344B (en) | 2015-12-23 | 2015-12-23 | Seed crystal tray, base station component and its application for diamond single crystal homoepitaxy |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105525344B (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106012003A (en) * | 2016-06-07 | 2016-10-12 | 武汉工程大学 | Two-dimensional expansion method for CVD monocrystal diamond |
| CN107955967A (en) * | 2017-11-30 | 2018-04-24 | 河北普莱斯曼金刚石科技有限公司 | Growth of Single Crystal Diamond device and method |
| CN108360064A (en) * | 2018-02-26 | 2018-08-03 | 湖北碳六科技有限公司 | A method of it improving MPCVD and prepares single-crystal diamond stability |
| CN109355702A (en) * | 2018-12-19 | 2019-02-19 | 长沙新材料产业研究院有限公司 | A method of for reducing CVD diamond synthesis impurity content |
| CN110042464A (en) * | 2019-04-02 | 2019-07-23 | 西安电子科技大学 | A kind of method of multi-disc single-crystal diamond expanding growth simultaneously |
| CN110820044A (en) * | 2019-12-02 | 2020-02-21 | 长沙新材料产业研究院有限公司 | High-quality diamond growth method and system |
| CN111663179A (en) * | 2019-03-05 | 2020-09-15 | 中国科学院物理研究所 | Seed crystal support for growth of single crystal diamond |
| CN113957516A (en) * | 2021-10-29 | 2022-01-21 | 中国电子科技集团公司第二十六研究所 | Tray device for growing crystals by horizontal directional crystallization method and use method |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002198318A (en) * | 2001-12-21 | 2002-07-12 | Sumitomo Metal Ind Ltd | Epitaxial growth method |
| CN101037793A (en) * | 2007-02-07 | 2007-09-19 | 吉林大学 | Device and method for high-speed rapid growth of diamond single-crystal |
| KR100773232B1 (en) * | 2006-12-29 | 2007-11-05 | 주식회사 실트론 | Wafer tray for preventing wafer contamination |
| CN202039158U (en) * | 2011-04-01 | 2011-11-16 | 东莞市天域半导体科技有限公司 | CVD graphite tray structure used for growing of semiconductor epitaxial wafer |
| CN203728962U (en) * | 2014-01-23 | 2014-07-23 | 新磊半导体科技（苏州）有限公司 | Substrate supporting plate in molecular beam epitaxial large-scale production device |
| CN203768486U (en) * | 2014-01-23 | 2014-08-13 | 新磊半导体科技（苏州）有限公司 | Substrate growth pallet with cut edge of molecular beam epitaxy (MBE) large-scale production equipment |
| CN204281889U (en) * | 2014-12-01 | 2015-04-22 | 常州宝颐金刚石科技有限公司 | A kind of novel seed crystal tray for rapid growth of diamond single-crystal |
| CN104775154A (en) * | 2015-04-25 | 2015-07-15 | 哈尔滨工业大学 | Method for controlling surface temperature in homoepitaxial growth of monocrystal diamond |
| 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 |
| CN104903490A (en) * | 2012-08-30 | 2015-09-09 | 二A科技有限公司 | Apparatus and method of producing diamond |
| CN104988578A (en) * | 2015-07-24 | 2015-10-21 | 哈尔滨工业大学 | Method for optimizing monocrystal diamond homoepitaxial growth by utilizing plasma baffle |
-
2015
- 2015-12-23 CN CN201510974331.XA patent/CN105525344B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002198318A (en) * | 2001-12-21 | 2002-07-12 | Sumitomo Metal Ind Ltd | Epitaxial growth method |
| KR100773232B1 (en) * | 2006-12-29 | 2007-11-05 | 주식회사 실트론 | Wafer tray for preventing wafer contamination |
| CN101037793A (en) * | 2007-02-07 | 2007-09-19 | 吉林大学 | Device and method for high-speed rapid growth of diamond single-crystal |
| CN202039158U (en) * | 2011-04-01 | 2011-11-16 | 东莞市天域半导体科技有限公司 | CVD graphite tray structure used for growing of semiconductor epitaxial wafer |
| CN104903490A (en) * | 2012-08-30 | 2015-09-09 | 二A科技有限公司 | Apparatus and method of producing diamond |
| CN203728962U (en) * | 2014-01-23 | 2014-07-23 | 新磊半导体科技（苏州）有限公司 | Substrate supporting plate in molecular beam epitaxial large-scale production device |
| CN203768486U (en) * | 2014-01-23 | 2014-08-13 | 新磊半导体科技（苏州）有限公司 | Substrate growth pallet with cut edge of molecular beam epitaxy (MBE) large-scale production equipment |
| CN204281889U (en) * | 2014-12-01 | 2015-04-22 | 常州宝颐金刚石科技有限公司 | A kind of novel seed crystal tray for rapid growth of diamond single-crystal |
| CN104775154A (en) * | 2015-04-25 | 2015-07-15 | 哈尔滨工业大学 | Method for controlling surface temperature in homoepitaxial growth of monocrystal diamond |
| 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 |
| CN104988578A (en) * | 2015-07-24 | 2015-10-21 | 哈尔滨工业大学 | Method for optimizing monocrystal diamond homoepitaxial growth by utilizing plasma baffle |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106012003A (en) * | 2016-06-07 | 2016-10-12 | 武汉工程大学 | Two-dimensional expansion method for CVD monocrystal diamond |
| CN107955967A (en) * | 2017-11-30 | 2018-04-24 | 河北普莱斯曼金刚石科技有限公司 | Growth of Single Crystal Diamond device and method |
| CN108360064A (en) * | 2018-02-26 | 2018-08-03 | 湖北碳六科技有限公司 | A method of it improving MPCVD and prepares single-crystal diamond stability |
| CN109355702A (en) * | 2018-12-19 | 2019-02-19 | 长沙新材料产业研究院有限公司 | A method of for reducing CVD diamond synthesis impurity content |
| CN111663179A (en) * | 2019-03-05 | 2020-09-15 | 中国科学院物理研究所 | Seed crystal support for growth of single crystal diamond |
| CN110042464A (en) * | 2019-04-02 | 2019-07-23 | 西安电子科技大学 | A kind of method of multi-disc single-crystal diamond expanding growth simultaneously |
| CN110820044A (en) * | 2019-12-02 | 2020-02-21 | 长沙新材料产业研究院有限公司 | High-quality diamond growth method and system |
| CN113957516A (en) * | 2021-10-29 | 2022-01-21 | 中国电子科技集团公司第二十六研究所 | Tray device for growing crystals by horizontal directional crystallization method and use method |
| CN113957516B (en) * | 2021-10-29 | 2024-01-30 | 中国电子科技集团公司第二十六研究所 | Tray device for growing crystals by horizontal directional crystallization method and use method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105525344B (en) | 2018-05-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105525344A (en) | Seed crystal tray and base station assembly for diamond monocrystal homoepitaxy, and application thereof | |
| JP6631517B2 (en) | Diamond substrate and diamond composite substrate | |
| CN106012003B (en) | The two-dimentional expansion method of CVD single-crystal diamonds | |
| WO2016169108A1 (en) | Local-area carbon supply device and method for preparing wafer-level graphene monocrystalline based on local-area carbon supply | |
| CN102057084A (en) | Seed crystal for growth of silicon carbide single crystal, process for producing the same, and silicone carbide single crystal and process for producing the same | |
| CN109355702B (en) | Method for reducing impurity content of CVD synthetic diamond | |
| CN108385086A (en) | Chip bench system and the method for improving diamond film growth uniformity using the system | |
| CN109722641A (en) | Diamond/graphene composite heat conduction film and preparation method thereof and cooling system | |
| CN106929828A (en) | A kind of chip bench that diamond film is prepared for MPCVD method | |
| CN103193224A (en) | Method for preparing graphene film on nonmetallic substrate at low temperature | |
| CN104152986A (en) | Method for quickly preparing 3C-SiC epitaxial film | |
| JP2011018772A (en) | Susceptor for silicon carbide single crystal film forming device | |
| CN103606514A (en) | Chemical corrosion transfer method based on GaN substrate CVD epitaxial growth graphene | |
| CN107164740A (en) | A kind of method that use MPCVD method prepares diamond film | |
| JP2002265296A (en) | Diamond thin film and manufacturing method therefor | |
| JP2004204299A (en) | Diamond film-deposition silicon and electrode | |
| CN101613881B (en) | Method for preparing SiC nanowire array | |
| CN113088937A (en) | Device for preparing single crystal diamond by improving stability through microwave plasma CVD and method for preparing single crystal diamond | |
| EP0959148B1 (en) | Method for producing diamond films using a vapour-phase synthesis system | |
| CN206751920U (en) | A kind of chip bench that diamond film is prepared for MPCVD method | |
| CN112609240B (en) | Method for improving heterogeneous epitaxial large-size nucleation uniformity of diamond based on composite structure sample platform | |
| CN111996581B (en) | Loss-free rapid separation method for single crystal diamond and substrate | |
| CN112695382B (en) | Method for improving heterogeneous epitaxial nucleation uniformity of diamond based on grid structure electrode | |
| CN212293841U (en) | Heat dissipation device for growing diamond | |
| CN102787305A (en) | Device and method for reducing impurity deposit in chemical vapor deposition process |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20210526 Address after: 221000 1-295, management committee of Quanzhan Economic Development Zone, No. 6, Tengfei Road, Quanzhan Economic Development Zone, Quanzhan District, Xuzhou City, Jiangsu Province Patentee after: Xuzhou Jinglan New Material Technology Co.,Ltd. Address before: 518000 No. 1068, Xue Yuan Avenue, Xili University Town, Nanshan District, Shenzhen, Guangdong Patentee before: SHENZHEN INSTITUTES OF ADVANCED TECHNOLOGY CHINESE ACADEMY OF SCIENCES |