CN106893997B - Nano-diamond film preparation substrate pre-treatment method - Google Patents
Nano-diamond film preparation substrate pre-treatment method Download PDFInfo
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- CN106893997B CN106893997B CN201710080946.7A CN201710080946A CN106893997B CN 106893997 B CN106893997 B CN 106893997B CN 201710080946 A CN201710080946 A CN 201710080946A CN 106893997 B CN106893997 B CN 106893997B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0272—Deposition of sub-layers, e.g. to promote the adhesion of the main coating
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
- C23C16/27—Diamond only
- C23C16/274—Diamond only using microwave discharges
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
- C23C16/511—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges using microwave discharges
Abstract
The invention discloses a kind of nano-diamond film preparation substrate pre-treatment methods, utilize the open loop multiple-limb polymerization of glycidol, functional group is formed on Nano diamond powder surface, obtain the Nano diamond powder (ND-PG) of dispersed fabulous polyglycerol grafting in the solution, it is dissolved in methanol solution, the seed crystal solution being nucleated for film is obtained, thus to provide effective method using microwave plasma chemical vapor deposition high quality nano-diamond film in foreign substrate.The present invention greatly increases the dispersibility of powder in water in Nano diamond powder surface graft functional group, reduces and reunites, the peripheral further functionalization of spin-off effects, the nucleation density for being conducive to increase substrate, improves nucleation quality, makes great sense to preparation high quality nano-diamond film.
Description
Technical field
The present invention relates to a kind of inorganic non-metallic material manufacturing process, prepare more particularly to a kind of nano-diamond film
Technique further relates to a kind of substrate pre-treatment method, is applied to diamond thin preparation technical field.
Background technique
Diamond is normal as a kind of material with many special performances, such as big forbidden bandwidth (reaching 5.5eV), low dielectric
Number, high-breakdown-voltage, high electron hole mobility, high heat conductance and superior radiation resistance, and chemical stability is good, institute
Have that these physics, chemically and electrically characteristic is likely to become diamond following to work under the mal-conditions such as high temperature intense radiation
Electronic equipment material.
People had focused on more attentions and have prepared diamond thin using CVD method in recent years, and achieved very big
Progress, but it is very harsh to the requirement of substrate in the preparation process of diamond thin, be difficult to grow Buddha's warrior attendant on many substrates
Stone film, and the speed of growth is slower, and the diamond thin crystal boundary and defect of growth are more, are difficult to meet diamond thin each
The application of a aspect.Therefore the step of depositing diamond film needs some reinforcements nucleation in foreign substrate, directly untreated
The nucleation density for the grown above silicon crossed is about 104-105cm-2.The method of pretreatment non-diamond substrate has mechanical grinding at present
Mill method, ultrasonic cleaning, biased nucleation method, diadust nucleation process etc., by pre-processed substrate, nucleation density can be more than
1011cm-2.This is more meaningful for the nano-diamond film that average grain size is nanometer scale.
But diadust density is big, and nano-scale particle is easy to reunite, and the seed crystal solution dispersion directly prepared is poor, shadow
Ring nucleation.In order to improve the dispersibility of Nano diamond powder in organic solvent, changed using the modified method of surface functional group
Variation minor structure is mostly used linear polyethers class compound come improved research, and for super-branched polyhydroxy as polyglycerol
The research of compound is fewer, and polyglycerol, which is applied to improvement Nano diamond powder modification, yet there are no related report.
Summary of the invention
In order to solve prior art problem, it is an object of the present invention to overcome the deficiencies of the prior art, and to provide one kind
Nano-diamond film preparation substrate pre-treatment method, using the open loop multiple-limb polymerization of glycidol, in nanogold
Hard rock powder surface forms functional group, obtains the Nano diamond powder of dispersed fabulous polyglycerol grafting in the solution
(ND-PG), be dissolved in methanol solution, obtain the seed crystal solution being nucleated for film, thus in foreign substrate using microwave etc. from
Sub- chemical vapor deposition high quality nano-diamond film provides effective method.
Purpose is created to reach foregoing invention, the present invention adopts the following technical solutions:
A kind of nano-diamond film preparation substrate pre-treatment method, includes the following steps:
A. the pretreatment of Nano diamond powder:
The concentrated sulfuric acid and mass percent concentration with mass percent concentration not less than 98% are not less than 60% concentrated nitric acid
Mixed solution prepares strong acid mixed liquor according to the ratio that the volume ratio of the concentrated sulfuric acid and concentrated nitric acid is 1:1~5:1, then by granularity
It is added in strong acid mixed liquor and is sufficiently mixed for the Nano diamond powder of 1~30nm, and to diamond at 100~300 DEG C
The mixed liquor of powder and strong acid heats 1-5h, obtains powder, then after powder is evaporated, adds deionized water, then
It is filtered, after the powder made is until be in neutrality, re-dry case dries powder, obtains ND pretreatment powder；
B. the preparation of the Nano diamond powder of polyglycerol grafting:
The ND pretreatment powder for taking 20~90mg to prepare in the step a dissolves in 3~10mL epoxy prapanol solvent, will
Obtained suspension is obtained not less than 1~3h of ultrasonic treatment at room temperature, then progress 1~10h of magnetic stirring at 100~200 DEG C
To modified ND-PG gel, then modified ND-PG gel is cooled to not higher than after room temperature, then with 30~100mL methanol ultrasound 2
~8h diluting modification ND-PG gel, and the extra precipitating of removal is filtered, obtain modified Nano diamond seed dispersion liquid；
C. substrate pre-treatment:
Substrate acetone, ethyl alcohol are cleaned, sol evenning machine is then utilized, the modification prepared in the step b is received
Rice diamond seed dispersion liquid is with spin coating 3~10 times on substrate of the speed of 3000~8000r/min, then makes to be coated on substrate
Modified Nano diamond seed dispersion liquid liquid film drying solidification after to get to have modified Nano diamond seed superficial layer
Compound substrate, on modified Nano diamond seed superficial layer continued growth prepare nano-diamond film.It is preferred that serving as a contrast
Bottom is the foreign substrate of diamond；The material of further preferred substrate is silicon, glass or quartz.
The present invention compared with prior art, has following obvious prominent substantive distinguishing features and remarkable advantage:
1. the present invention is using new nano-diamond film preparation substrate pre-treatment method, using super-branched polyhydroxylated
The ring-opening polymerisation effect for closing object changes molecular structure, the good hydrophilic property of hydroxyl, while super-branched structure and linear chain structure phase
Than can more densely packed be covered on the surface of nano particle, can preferably improve the dispersion of Nano diamond powder in the solution
Property, the present invention is easy to form functional group, the modified Nano diamond of preparation on nano-diamond particles surface using glycidol
Seed crystal good hydrophilic property, biocompatibility are good；
2. the present invention greatly increases the dispersibility of powder in water, subtracts in Nano diamond powder surface graft functional group
Few to reunite, the peripheral further functionalization of spin-off effects is conducive to the nucleation density for increasing substrate, nucleation quality is improved, to preparation
High quality nano-diamond film makes great sense；
It is modified 3. the present invention carries out surface to Nano diamond powder using super-branched polyol, is successive modified
Provide a large amount of amendable hydroxyl groups.
Specific embodiment
Details are as follows for the preferred embodiment of the present invention:
Embodiment one:
In the present embodiment, a kind of nano-diamond film preparation substrate pre-treatment method, includes the following steps:
A. the pretreatment of Nano diamond powder:
The concentrated nitric acid mixing that the concentrated sulfuric acid and mass percent concentration for being 98.3% with mass percent concentration are 60% is molten
Liquid prepares strong acid mixed liquor, the nanometer for being then 10nm by granularity according to the ratio that the volume ratio of the concentrated sulfuric acid and concentrated nitric acid is 3:1
Diamond (ND) powder, which is added in strong acid mixed liquor, to be sufficiently mixed, and the mixing at 180 DEG C to diamond dust and strong acid
Liquid heats 3h, obtains powder, then after powder is evaporated, adds deionized water, be then filtered, the powder made
After end is until be in neutrality, re-dry case dries powder, obtains ND pretreatment powder；
B. the preparation of the Nano diamond powder (ND-PG) of polyglycerol grafting:
The ND pretreatment powder for taking 60mg to prepare in the step a dissolves in 7mL epoxy prapanol solvent, outstanding by what is obtained
Turbid is ultrasonically treated 2h at 25 DEG C of room temperature, then magnetic stirring 1h is carried out at 140 DEG C, obtains modified ND-PG gel, then will
After modified ND-PG gel is cooled to room temperature, then use 60mL methanol ultrasound 5h diluting modification ND-PG gel, and filter remove it is extra
Precipitating, obtains modified Nano diamond seed dispersion liquid；The present embodiment is made using the ring-opening polymerisation of super-branched polyol
With molecular structure is changed, seed crystal solution is prepared using the Nano diamond powder that super-branched polyol surface was modified,
The good hydrophilic property of hydroxyl, while super-branched structure can more densely packed be covered on nano particle compared with linear chain structure
Surface can preferably improve the dispersibility of Nano diamond powder in the solution；
C. substrate pre-treatment:
Silicon chip substrate acetone, ethyl alcohol are cleaned, sol evenning machine is then utilized, changes what is prepared in the step b
Property Nano diamond seed crystal dispersion liquid with the speed of 6000r/min spin coating 7 times in silicon chip substrate, then make be coated on substrate on
The liquid film drying of modified Nano diamond seed dispersion liquid solidify after to get to modified Nano diamond seed superficial layer
Compound substrate, on modified Nano diamond seed superficial layer continued growth prepare nano-diamond film.
The present embodiment utilizes the open loop multiple-limb polymerization of glycidol, forms function on Nano diamond powder surface
Group obtains the Nano diamond powder (ND-PG) of dispersed fabulous polyglycerol grafting in the solution, is dissolved in methanol solution,
The seed crystal solution being nucleated for film is obtained, to provide for deposition preparation high quality nano-diamond film in foreign substrate
Effective method.
Experimental test and analysis:
The processed silicon wafer of embodiment one will be passed through, i.e., there is modified Nano diamond seed table by prepared by embodiment one
The compound substrate of surface layer is put into the cavity of MPCVD instrument, is vacuumized, H2And CH4As reaction gas, deposition pressure is
50Torr, microwave power 3kW, time 1h are vapor-deposited high-quality on Heterogeneous Composite substrate using microwave plasma chemical
Measure nano-diamond film.
The nano-diamond film prepared is characterized using atomic force microscope, the common seed with the prior art
The film of brilliant solution preparation compares discovery, under similarity condition before roughness of film be 50nm, and utilize embodiment one
The compound substrate growth with modified Nano diamond seed superficial layer of preparation prepares the rough surface of nano-diamond film
Degree is 20nm, and partial size also reaches Nano grade.The nanogold that embodiment one was modified using super-branched polyol surface
Hard rock powder prepares seed crystal solution, prepares pretreatment foreign substrate using embodiment one to deposit nano-diamond film, in height
Temperature is lower to be greatly increased by the open loop multiple-limb polymerization of glycidol in Nano diamond powder surface graft functional group
The dispersibility of powder in water reduces and reunites, and is conducive to the nucleation density for increasing substrate, improves nucleation quality, high-quality to preparing
Amount nano-diamond film makes great sense.
Embodiment two:
The present embodiment is basically the same as the first embodiment, and is particular in that:
In the present embodiment, a kind of nano-diamond film preparation substrate pre-treatment method, includes the following steps:
A. the pretreatment of Nano diamond powder:
The concentrated nitric acid mixing that the concentrated sulfuric acid and mass percent concentration for being 98.3% with mass percent concentration are 60% is molten
Liquid prepares strong acid mixed liquor, the nanometer for being then 1nm by granularity according to the ratio that the volume ratio of the concentrated sulfuric acid and concentrated nitric acid is 1:1
Diamond (ND) powder, which is added in strong acid mixed liquor, to be sufficiently mixed, and the mixing at 100 DEG C to diamond dust and strong acid
Liquid heats 5h, obtains powder, then after powder is evaporated, adds deionized water, be then filtered, the powder made
After end is until be in neutrality, re-dry case dries powder, obtains ND pretreatment powder；
B. the preparation of the Nano diamond powder (ND-PG) of polyglycerol grafting:
The ND pretreatment powder for taking 90mg to prepare in the step a dissolves in 3mL epoxy prapanol solvent, outstanding by what is obtained
Turbid is ultrasonically treated 3h at 25 DEG C of room temperature, then magnetic stirring 1h is carried out at 200 DEG C, obtains modified ND-PG gel, then will
After modified ND-PG gel is cooled to room temperature, then use 100mL methanol ultrasound 8h diluting modification ND-PG gel, and filter remove it is extra
Precipitating, obtains modified Nano diamond seed dispersion liquid；The present embodiment is made using the ring-opening polymerisation of super-branched polyol
With molecular structure is changed, seed crystal solution is prepared using the Nano diamond powder that super-branched polyol surface was modified,
The good hydrophilic property of hydroxyl, while super-branched structure can more densely packed be covered on nano particle compared with linear chain structure
Surface can preferably improve the dispersibility of Nano diamond powder in the solution；
C. substrate pre-treatment:
Glass substrate acetone, ethyl alcohol are cleaned, sol evenning machine is then utilized, changes what is prepared in the step b
Property Nano diamond seed crystal dispersion liquid with the speed of 8000r/min spin coating 10 times on a glass substrate, then make be coated on substrate on
Modified Nano diamond seed dispersion liquid liquid film drying solidification after to get to have modified Nano diamond seed superficial layer
Compound substrate, on modified Nano diamond seed superficial layer continued growth prepare nano-diamond film.
The present embodiment utilizes the open loop multiple-limb polymerization of glycidol, forms function on Nano diamond powder surface
Group obtains the Nano diamond powder (ND-PG) of dispersed fabulous polyglycerol grafting in the solution, is dissolved in methanol solution,
The seed crystal solution being nucleated for film is obtained, to provide for deposition preparation high quality nano-diamond film in foreign substrate
Effective method.
Experimental test and analysis:
Compound substrate with modified Nano diamond seed superficial layer prepared by embodiment two is put into MPCVD instrument
It in cavity, vacuumizes, H2And CH4As reaction gas, deposition pressure 50Torr, microwave power 3kW, time 1h, different
In matter compound substrate, microwave plasma chemical vapor deposition high quality nano-diamond film is utilized.
The nano-diamond film prepared is characterized using atomic force microscope, the common seed with the prior art
The film of brilliant solution preparation compares discovery, under similarity condition before roughness of film be 50nm, and utilize embodiment two
The compound substrate growth with modified Nano diamond seed superficial layer of preparation prepares the rough surface of nano-diamond film
Degree is 32nm, and partial size also reaches Nano grade.
Embodiment three:
The present embodiment is substantially the same as in the previous example, and is particular in that:
In the present embodiment, a kind of nano-diamond film preparation substrate pre-treatment method, includes the following steps:
A. the pretreatment of Nano diamond powder:
The concentrated nitric acid mixing that the concentrated sulfuric acid and mass percent concentration for being 98.3% with mass percent concentration are 60% is molten
Liquid prepares strong acid mixed liquor, the nanometer for being then 1nm by granularity according to the ratio that the volume ratio of the concentrated sulfuric acid and concentrated nitric acid is 5:1
Diamond (ND) powder, which is added in strong acid mixed liquor, to be sufficiently mixed, and the mixing at 300 DEG C to diamond dust and strong acid
Liquid heats 1h, obtains powder, then after powder is evaporated, adds deionized water, be then filtered, the powder made
After end is until be in neutrality, re-dry case dries powder, obtains ND pretreatment powder；
B. the preparation of the Nano diamond powder (ND-PG) of polyglycerol grafting:
The ND pretreatment powder for taking 20mg to prepare in the step a dissolves in 10mL epoxy prapanol solvent, by what is obtained
Suspension is ultrasonically treated 1h at 25 DEG C of room temperature, then magnetic stirring 10h is carried out at 100 DEG C, obtains modified ND-PG gel, so
Afterwards will be after modified ND-PG gel be cooled to room temperature, then with 30mL methanol ultrasound 2h diluting modification ND-PG gel, and filter removal
Extra precipitating obtains modified Nano diamond seed dispersion liquid；The present embodiment is poly- using the open loop of super-branched polyol
With molecular structure is changed, the Nano diamond powder preparation seed crystal being modified using super-branched polyol surface is molten for cooperation
Liquid, the good hydrophilic property of hydroxyl, while super-branched structure can more densely packed be covered on nano particle compared with linear chain structure
Surface, can preferably improve the dispersibility of Nano diamond powder in the solution；
C. substrate pre-treatment:
Glass substrate acetone, ethyl alcohol are cleaned, sol evenning machine is then utilized, changes what is prepared in the step b
Property Nano diamond seed crystal dispersion liquid with the speed of 3000r/min spin coating 3 times on a glass substrate, then make be coated on substrate on
The liquid film drying of modified Nano diamond seed dispersion liquid solidify after to get to modified Nano diamond seed superficial layer
Compound substrate, on modified Nano diamond seed superficial layer continued growth prepare nano-diamond film.
The present embodiment utilizes the open loop multiple-limb polymerization of glycidol, forms function on Nano diamond powder surface
Group obtains the Nano diamond powder (ND-PG) of dispersed fabulous polyglycerol grafting in the solution, is dissolved in methanol solution,
The seed crystal solution being nucleated for film is obtained, to provide for deposition preparation high quality nano-diamond film in foreign substrate
Effective ways.
Experimental test and analysis:
Compound substrate with modified Nano diamond seed superficial layer prepared by embodiment three is put into MPCVD instrument
It in cavity, vacuumizes, H2And CH4As reaction gas, deposition pressure 50Torr, microwave power 3kW, time 1h, different
In matter compound substrate, microwave plasma chemical vapor deposition high quality nano-diamond film is utilized.
The nano-diamond film prepared is characterized using atomic force microscope, the common seed with the prior art
The film of brilliant solution preparation compares discovery, under similarity condition before roughness of film be 50nm, and utilize embodiment three
The compound substrate growth with modified Nano diamond seed superficial layer of preparation prepares the rough surface of nano-diamond film
Degree is 40nm, and partial size also reaches Nano grade.
The embodiment of the present invention is illustrated above, but the present invention is not limited to the above embodiments, it can also be according to this hair
The purpose of bright innovation and creation makes a variety of variations, and that does under the Spirit Essence and principle of all technical solutions according to the present invention changes
Become, modification, substitution, combination or simplified, should be equivalent substitute mode, as long as meeting goal of the invention of the invention, as long as not
Away from the technical principle and inventive concept of nano-diamond film preparation substrate pre-treatment method of the present invention, the present invention is belonged to
Protection scope.
Claims (3)
1. a kind of nano-diamond film preparation substrate pre-treatment method, which comprises the steps of:
A. the pretreatment of Nano diamond powder:
The concentrated nitric acid of the concentrated sulfuric acid and mass percent concentration not less than 60% with mass percent concentration not less than 98% carries out
Mixing, according to the volume ratio of the concentrated sulfuric acid and concentrated nitric acid be 1:1~5:1 ratio prepare strong acid mixed liquor, then by granularity be 1~
The Nano diamond powder of 30nm, which is added in strong acid mixed liquor, to be sufficiently mixed, and at 100~300 DEG C to diamond dust and
The mixed liquor of strong acid heats 1-5h, obtains powder, then after powder is evaporated, adds deionized water, then carried out
Filter, after the powder made is until be in neutrality, re-dry case dries powder, obtains ND pretreatment powder；
B. the preparation of the Nano diamond powder of polyglycerol grafting:
The ND pretreatment powder for taking 20~90mg to prepare in the step a dissolves in 3~10mL epoxy prapanol solvent, will obtain
Suspension not less than at room temperature be ultrasonically treated 1~3h, then at 100~200 DEG C carry out 1~10h of magnetic stirring, changed
Property ND-PG gel, then modified ND-PG gel is cooled to not higher than after room temperature, then with 30~100mL methanol ultrasound, 2~8h
Diluting modification ND-PG gel, and the extra precipitating of removal is filtered, obtain modified Nano diamond seed dispersion liquid；
C. substrate pre-treatment:
Substrate acetone, ethyl alcohol are cleaned, sol evenning machine is then utilized, by the modified Nano prepared in the step b gold
Hard rock seed crystal dispersion liquid is with spin coating 3~10 times on substrate of the speed of 3000~8000r/min, then makes to be coated on changing on substrate
Property Nano diamond seed crystal dispersion liquid liquid film drying solidify after being answered to get to modified Nano diamond seed superficial layer
Close substrate, on modified Nano diamond seed superficial layer continued growth prepare nano-diamond film.
2. nano-diamond film preparation substrate pre-treatment method according to claim 1, it is characterised in that: in the step
In rapid c, the substrate is the foreign substrate of diamond.
3. nano-diamond film preparation substrate pre-treatment method according to claim 1, it is characterised in that: in the step
In rapid c, the material of the substrate is silicon, glass or quartz.
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| WO2021046748A1 (en) * | 2019-09-11 | 2021-03-18 | 深圳先进技术研究院 | Ultrathin diamond film, and preparation method therefor and application thereof |
| CN112553590B (en) * | 2020-12-02 | 2021-07-06 | 上海征世科技股份有限公司 | Diamond film based on plasma vapor deposition and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101613511A (en) * | 2009-07-15 | 2009-12-30 | 天津工业大学 | A kind of ptfe composite and preparation method thereof |
| CN104724664A (en) * | 2015-03-14 | 2015-06-24 | 王宏兴 | Preparation method and application of monocrystal diamond nano-pillar array structure |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6021892A (en) * | 1983-07-14 | 1985-02-04 | Matsushita Electric Ind Co Ltd | Substrate treated to form single crystal on surface and preparation thereof |
| US20090016950A1 (en) * | 2006-06-05 | 2009-01-15 | Reginald Bernard Little | Terrestrial lightning-powered magnetic organized single crystal diamond blocks: The forces of nature to form the beautiful gem |
-
2017
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101613511A (en) * | 2009-07-15 | 2009-12-30 | 天津工业大学 | A kind of ptfe composite and preparation method thereof |
| CN104724664A (en) * | 2015-03-14 | 2015-06-24 | 王宏兴 | Preparation method and application of monocrystal diamond nano-pillar array structure |
Non-Patent Citations (1)
| Title |
|---|
| "纳米金刚石薄膜的光学性能研究";蒋丽雯等;《红外与毫米波学报》;20060630;第25卷(第3期);第195-198页 |
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