CN109097754A - A kind of surface have high density nano diamond thin workpiece and a kind of preparation method of high density nano diamond thin - Google Patents
A kind of surface have high density nano diamond thin workpiece and a kind of preparation method of high density nano diamond thin Download PDFInfo
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- CN109097754A CN109097754A CN201710470374.3A CN201710470374A CN109097754A CN 109097754 A CN109097754 A CN 109097754A CN 201710470374 A CN201710470374 A CN 201710470374A CN 109097754 A CN109097754 A CN 109097754A
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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
- C23C16/22—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
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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
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Abstract
The present invention provides a kind of preparation methods of high density nano diamond thin, comprising: workpiece substrate is carried out surface preparation, keeps its surface positively charged or negative electricity；Lysine is added to the water, obtains lysine solution, then nano-diamond powder is added into lysine solution, obtains that Nano diamond particle surface is positively charged or the Nano diamond suspension of negative electricity after ultrasonic disperse；Workpiece substrate after surface preparation is immersed in the Nano diamond suspension with workpiece substrate oppositely charged, ultrasonic vibration makes Nano diamond granular absorption on workpiece substrate surface；After the completion of absorption, take out workpiece substrate, clean and after being dried with nitrogen, using chemical vapor depsotition equipment on workpiece substrate growing diamond membrane.This method may be implemented on complex part the preparation for carrying out the high-densit diamond thin of large-area nano grade thickness, and film quality is high, and binding force is strong, and simple process and low cost, has broad application prospects in Nano electro-mechanical system.
Description
Technical field
The present invention relates to Nano diamond technical fields, have high density nano thin diamond more particularly to a kind of surface
The workpiece of film and a kind of preparation method of high density nano diamond thin.
Background technique
Diamond thin is due to its high-melting-point, high heat conductance, high rigidity, good insulating, corrosion resistance are strong, dielectric constant
It is small, there are wide band gap semiconducter feature and the characteristics such as chemical stability is good, make it in wear-resistant coating, biomedicine, the micro- biography of film
Numerous high-technology fields such as sensor, Nano electro-mechanical system have broad application prospects.Currently in order to obtaining high quality Buddha's warrior attendant
Stone film carries out coating pretreatment to matrix usually using diamond nano powder to improve diamond thin in different matrix material
Enhancing Nucleation Density, however how to allow diamond nano powder to be uniformly coated on matrix surface, and do not limited by base shape size
It is a great problem.In addition, the thickness of film needs to control in nanoscale, this is just to needed for pretreatment in Nano electro-mechanical system
Nano-diamond powder in aqueous solution dispersibility more stringent requirements are proposed, how to control nano-diamond powder to deposition
Do not occur to reunite in substrate conditioning procedures is that current nano-diamond powder is applied to the another big of diamond thin forming core growth
Problem.
Currently in order to preparing high-densit diamond thin, usual way includes polishing, water slug method, bias increasing
Strong forming core method, aciding etc., although these methods can increase nucleation process early period of diamond thin to a certain extent,
It is that its humidification is limited, and still can not solve to carry out large-area nano grade high density nano on complicated micro-nano workpiece
The preparation of diamond thin.Therefore, it is necessary to a kind of preparation method of high density nano diamond thin be provided, to realize in shape
The diamond thin of high-densit nanometer grade thickness is prepared on the micro-nano workpiece of shape complexity, film quality is high, and and matrix
Between have stronger binding force.
Summary of the invention
In consideration of it, the present invention provides a kind of preparation methods of high density nano diamond thin, to solve the prior art
It is difficult to carry out the thin diamond film preparation of large-area nano grade thickness on the micro-nano matrix of complicated shape, the film prepared lacks
Fall into more, the poor problem of binding force.
In a first aspect, the present invention provides a kind of preparation methods of high density nano diamond thin, comprising the following steps:
Workpiece substrate is taken, the workpiece substrate is subjected to surface preparation, keeps the workpiece substrate surface positively charged or negative
Electricity；
Lysine is added to the water, obtains lysine solution, then Nano diamond is added into the lysine solution
Powder, obtains that Nano diamond particle surface is positively charged or the Nano diamond suspension of negative electricity after ultrasonic disperse；
Workpiece substrate after surface preparation is immersed in the Nano diamond with the workpiece substrate oppositely charged
In suspension, ultrasonic vibration makes the Nano diamond granular absorption in the Nano diamond suspension in the workpiece substrate
Surface；
After the completion of absorption, the workpiece substrate is taken out, clean and after being dried with nitrogen, using chemical vapor depsotition equipment,
The growing diamond membrane on the workpiece substrate.
Lysine is added as dispersing agent, under the action of lysine, nanometer in the present invention in Nano diamond suspension
Diamond particles can evenly dispersed in the solution, stable suspersion, hydration partial size is in smaller range, effective solution Nano diamond
The reunion of powder, settlement issues, and since there are two amino for tool in lysine molecule, so that bortz powder surface charge shape
State and quantity are easy to control, and the different electrical Nano diamonds of diamond particle surfaces band can be obtained by adjusting solution ph
The Nano diamond suspension is used for electrostatic attraction plantation crystal seed and prepares high density nano diamond thin in matrix by suspension
When, it can solve the problems, such as that diamond is low in heterogeneous matrix surface Enhancing Nucleation Density, effectively improve the Enhancing Nucleation Density of diamond thin, and
Impurity will not be introduced in above-mentioned process, so that available defect concentration is low, the strong high density nano diamond thin of binding force.
In an embodiment of the present invention, the lysine solution pH value is adjusted to 3-5, diamond particle surfaces can be obtained
Positively charged Nano diamond suspension.When pH value is 3-5, carboxyl in lysine molecule can preferentially with diamond particles table
Face mutually attracts, and amino obtains proton in water, makes diamond particles in electropositive, and due to there are two containing in lysine molecule
Amino, thus diamond particles electropositive can be made stronger, so as to preferably be combined with electronegative matrix.
In another embodiment of the present invention, the lysine solution pH value is adjusted to 6-10, diamond particles can be obtained
The electronegative Nano diamond suspension in surface.When pH value is 6-10, the positive charge quantity in lysine molecule is greater than Buddha's warrior attendant
The positive charge quantity of stone nano grain surface band, so that whole nano particle is negatively charged.Further, by the lysine
Solution ph is adjusted to 7-9.
In embodiment of the present invention, sodium hydroxide can be used, ammonium hydroxide or hydrochloric acid adjust lysine solution pH value.
In embodiment of the present invention, the concentration of lysine is 10 in the lysine solution-7~10-3Mol/L, further
Ground concentration is 10-5~10-4mol/L.The suitable concentration of lysine, it is ensured that the dispersibility and particle of diamond nano-particles
The quantity of electric charge on surface is embodied in the size distribution and Zeta potential of nano particle.
In embodiment of the present invention, the material of the workpiece substrate is silicon, silica, silicon carbide, copper oxide, silicon nitride
Or hard alloy.Specifically, workpiece substrate can be national defence, industry, aerospace, biomedicine, precision instrument, communication, vapour
The Workpiece structure in the fields such as vehicle, environmental protection, bioengineering and automation.E.g. cutter, switching device, integrated circuit, memory,
Component in sensor, printer etc..
In embodiment of the present invention, the concrete mode of the surface preparation is unlimited, as long as making workpiece substrate surface band
Upper required positive electricity or negative electricity can specifically include solvent cleaning treatment, oxygen plasma cleaning treatment, at chemical etching
At least one of reason, hydrogenation treatment.
For example, can be handled by surface hydriding when workpiece substrate is hard alloy material so that matrix surface is positively charged,
By oxygen plasma cleaning treatment or chemical etching processing so that matrix surface is negatively charged.The hydrogenation treatment specifically includes: will
Hard alloy workpiece matrix is placed in the vacuum chamber of filming equipment, is passed through high-purity hydrogen, and the control indoor air pressure of vacuum is 0.5~
20kPa, substrate temperature are 900~1100 DEG C.The chemical etching processing specifically: the hard is closed using Caro mixed acid
Golden workpiece substrate carries out 0.5~1min of oxide etch.The oxygen plasma cleaning treatment specifically: by hard alloy workpiece matrix
Oxygen plasma cleaning machine is placed in be cleaned.
When workpiece substrate is silicon or silica material, following surface preparation can be carried out to the workpiece substrate, made
Its surface takes negative electricity: it is NH that matrix, which is immersed in the proportion that temperature is 80-95 DEG C, first3H2O:H2O: H2O2=10:50:10 (body
Product ratio) solution in progress chemical etching processing in 5-10 minutes, then matrix is taken out, is cleaned by ultrasonic 2-3 in deionized water
Time, it is every all over ultrasound 5-10 minutes.
It, can be successively ultrasonic in acetone, alcohol and deionized water by workpiece substrate when workpiece substrate is silicon carbide material
Cleaning 10-30 minutes, makes workpiece substrate surface take negative electricity.It, can be by work when workpiece substrate is copper oxide or silicon nitride material
Part matrix is successively cleaned by ultrasonic 10-30 minutes in acetone, alcohol and deionized water, and workpiece substrate surface is made to become positively charged.
In embodiment of the present invention, in the Nano diamond suspension, the mass concentration of Nano diamond particle is
The partial size of 0.005-0.5%, Nano diamond particle are less than 50nm.In the application, the nano-diamond powder is commercial product,
(alternatively referred to as Nano diamond aggregation) is obtained with explosion method, does not carry out any processing, particle size is from several hundred nanometers to ten
Several microns, average grain diameter is other in the micron-scale.After ultrasonic disperse, nano-diamond powder becomes the smaller Nano diamond of partial size
Particle, optionally, in the Nano diamond suspension, the mass concentration of Nano diamond particle is 0.02-0.3%, nanometer
The partial size of diamond particles is 5-35nm, is further 10-30nm or 15-25nm.
Wherein, the time of the ultrasonic vibration is 10min-2h, power 200-500W.
Wherein, the mode of growing diamond membrane can be heated filament vapor deposition, microwave plasma enhanced chemical gaseous phase
Deposition, can also be obtained by the way of other chemical vapor depositions.Diamond crystals in diamond thin can be nanometer
Or micron level, it can be realized by the content of control reaction gas and gas pressure in vacuum, substrate temperature etc..
In an embodiment of the present invention, diamond thin, sedimentary condition are prepared by the way of heated filament vapor deposition are as follows:
Using hydrogen and methane as reaction gas, it is 0.6%-2%, gas pressure in vacuum range that methane, which accounts for total gas volume range,
For 2-10kPa；Filament wattage range is 5800-6800W, and the temperature range of matrix is 700-1000 DEG C；Sedimentation time is 0.5-
Diamond thin is prepared in 4h.
By controlling sedimentary condition, the diamond thin that diamond crystals are micron level or Nano grade can be obtained.
In embodiment of the present invention, the diamond thin with a thickness of 50-150nm, further, diamond thin
With a thickness of 50-80nm.
The preparation method for the high density nano diamond thin that first aspect present invention provides is, it can be achieved that on complex part
The preparation of the high-densit diamond thin of large-area nano grade thickness is carried out, film quality is high, and binding force is strong, and simple process,
At low cost, the fine dispersion of bortz powder can be realized by making dispersing agent using micro lysine, and need to only adjust pH
The positive negativity for adjusting Nano diamond Particle surface charge, is suitble to the workpiece surface of a variety of different substrate materials to prepare, and is suitable for extensive
Industrialized production has broad application prospects in Nano electro-mechanical system.
The present invention also provides the workpiece that a kind of surface has high density nano diamond thin, including workpiece substrate and tight
In the high density nano diamond thin on the workpiece substrate surface, the material of the workpiece substrate is silicon, titanium dioxide for close combination
Silicon, silicon carbide, copper oxide, silicon nitride or hard alloy, the diamond thin with a thickness of 50-150nm, the thin diamond
The area size of film is determined by specific workpiece.
The diamond thin with a thickness of 50-150nm, further, diamond thin with a thickness of 50-80nm.
The hardness of the diamond thin is 75-100GPa.
The binding force of the diamond thin and the workpiece substrate is 90-120N.
The workpiece substrate is the micro-nano workpiece with complex three-dimensional configuration.
The workpiece substrate is atomic force microscopy instrument probe.The surface of the probe has the high density nano
Diamond thin.The diamond thin can effectively improve the intensity of probe, and probe is avoided to be broken.
The probe is silicon material probe or silicon nitride material probe.
Surface provided by the invention has the workpiece of high density nano diamond thin, the optional type of workpiece substrate material
More, workpiece shapes construction is unlimited, and diamond thin has nanometer grade thickness, and film quality is high, and binding force is strong.
Advantages of the present invention will be illustrated partially in the following description, and a part is apparent according to specification
, or can implementation through the embodiment of the present invention and know.
Detailed description of the invention
Fig. 1 is the cross-section structure for the silicon wafer that the surface that the embodiment of the present invention 1 provides has high density nano diamond thin
Schematic diagram；
Fig. 2 is the SEM figure that the surface of the embodiment of the present invention 1 has the silicon wafer of high density nano diamond thin.
Specific embodiment
As described below is the preferred embodiment of the embodiment of the present invention, it is noted that for the common skill of the art
For art personnel, without departing from the principles of the embodiments of the present invention, several improvements and modifications can also be made, these improvement
Also it is considered as the protection scope of the embodiment of the present invention with retouching.
Embodiment 1
A kind of preparation method of high density nano diamond thin, comprising the following steps:
Step 1 takes silicon wafer matrix to carry out surface preparation, keeps silicon chip surface negatively charged；Matrix, which is immersed in temperature, first is
92 DEG C, proportion be NH3H2O:H2O:H2O210 minutes in the solution of=10:50:10 (volume ratio), then matrix is taken out, is being gone
It is cleaned by ultrasonic 3 times in ionized water, it is every all over ultrasound 5 minutes；
Step 2, prepares the positively charged Nano diamond suspension of diamond particle surfaces: adding lysine in water and matches
It is 5 × 10 at lysine concentration-6The lysine solution that mol/L, pH are 7, the nano-diamond powder purchased in the market is added to
In above-mentioned lysine solution, through ultrasonic disperse, the Nano diamond that the mass concentration of Nano diamond particle is 0.005% is obtained
Suspension；
Matrix in step 1 through surface preparation is put into the nanodiamond suspension of step 2 preparation by step 3
In, sonic oscillation 20 minutes, power 280W made Nano diamond granular absorption on silicon substrate surface；
Step 4 embathes matrix taking-up, in deionized water then using being dried with nitrogen；
Sample after being dried with nitrogen is placed in hot-filament chemical vapor deposition equipment by step 5, raw using following parameter
Long diamond thin: deposition pressure 2000Pa, sedimentation time 15 minutes, reaction gas hydrogen 800sccm, methane 16sccm.Lamp
Silk power 7000W, finally obtains the high density nano diamond thin for being formed in silicon substrate surface by 1000 DEG C of substrate temperature, thin
Film thickness is 50nm.
Fig. 1 is the section for the silicon wafer 100 that the surface that the embodiment of the present invention 1 provides has high density nano diamond thin
Structural schematic diagram；10 be silicon wafer matrix in figure, and 11 be nano-diamond film.
Fig. 2 is the SEM figure that the surface of the embodiment of the present invention 1 has the silicon wafer of high density nano diamond thin, and Fig. 2 is aobvious
Show, nano-diamond film 21 is combined closely on the silicon wafer matrix 20, with a thickness of 50nm.
Embodiment 2
A kind of preparation method of high density nano diamond thin, comprising the following steps:
Step 1 takes silica substrate to carry out surface preparation, keeps matrix surface negatively charged: matrix being immersed in temperature first
Degree is 82 DEG C, proportion is NH3H2O:H2O:H2O210 minutes in the solution of=10:50:10 (volume ratio), then matrix is taken out,
It is cleaned by ultrasonic 3 times in deionized water, it is every all over ultrasound 5 minutes；
Step 2, prepares the positively charged Nano diamond suspension of diamond particle surfaces: adding lysine in water and matches
It is 5 × 10 at lysine concentration-6The lysine solution that mol/L, pH are 4, the nano-diamond powder purchased in the market is added to
In above-mentioned lysine solution, through ultrasonic disperse, the Nano diamond that the mass concentration of Nano diamond particle is 0.005% is obtained
Suspension；
Matrix in step 1 through surface preparation is put into the nanodiamond suspension of step 2 preparation by step 3
In, sonic oscillation 30 minutes, power 280W made Nano diamond granular absorption on silica substrate surface；
Step 4 embathes matrix taking-up, in deionized water then using being dried with nitrogen；
Sample after being dried with nitrogen is placed in hot-filament chemical vapor deposition equipment by step 5, raw using following parameter
Long diamond thin: deposition pressure 4000Pa, sedimentation time 0.5 hour, reaction gas hydrogen 800sccm, methane 16sccm.
Filament wattage 6300W, finally obtains the high density nano diamond for being formed in silica substrate surface by 950 DEG C of substrate temperature
Film, film thickness 80nm.
Embodiment 3
A kind of preparation method of high density nano diamond thin, comprising the following steps:
Step 1 takes silicon carbide substrate to carry out surface preparation, keeps matrix surface negatively charged: by matrix respectively successively third
It is cleaned by ultrasonic 15 minutes in ketone, alcohol and water deionized water.
Step 2, prepares the positively charged Nano diamond suspension of diamond particle surfaces: adding lysine in water and matches
It is 5 × 10 at lysine concentration-6The lysine solution that mol/L, pH are 3, the nano-diamond powder purchased in the market is added to
In above-mentioned lysine solution, through ultrasonic disperse, the Nano diamond that the mass concentration of Nano diamond particle is 0.05% is obtained
Suspension；
Matrix in step 1 through surface preparation is put into the nanodiamond suspension of step 2 preparation by step 3
In, sonic oscillation 30 minutes, power 280W made Nano diamond granular absorption on silicon carbide substrate surface；
Step 4 embathes matrix taking-up, in deionized water then using being dried with nitrogen；
Sample after being dried with nitrogen is placed in hot-filament chemical vapor deposition equipment by step 5, raw using following parameter
Long diamond thin: deposition pressure 4000Pa, sedimentation time 0.5 hour, reaction gas hydrogen 800sccm, methane 16sccm.
Filament wattage 6300W, finally obtains the high density nano thin diamond for being formed in silicon carbide substrate surface by 950 DEG C of substrate temperature
Film, film thickness 60nm.
Embodiment 4
A kind of preparation method of high density nano diamond thin, comprising the following steps:
Step 1, take oxidation Copper substrate carry out surface preparation, keep matrix surface positively charged: will oxidation Copper substrate respectively according to
It is secondary to be cleaned by ultrasonic 15 minutes in acetone, alcohol and water deionized water；
Step 2 prepares the electronegative Nano diamond suspension of diamond particle surfaces: adding lysine in water and matches
It is 10 at lysine concentration-7~10-3The nano-diamond powder purchased in the market is added the lysine solution that mol/L, pH are 6
Into above-mentioned lysine solution, through ultrasonic disperse, the nanometer Buddha's warrior attendant that the mass concentration of Nano diamond particle is 0.005% is obtained
Stone suspension；
Matrix in step 1 through surface preparation is put into the nanodiamond suspension of step 2 preparation by step 3
In, ultrasonic vibration 30 minutes, ultrasonic power 280W made Nano diamond granular absorption in copper oxide matrix surface, wherein inhaling
The partial size for being attached to the Nano diamond particle of copper oxide matrix surface is 20-25nm；
Step 4 takes out matrix, is put into deionized water and embathes, then dry with nitrogen；
Sample of the nitrogen after dry is placed on the vacuum of microwave plasma enhanced chemical vapor depsotition equipment by step 5
In room, following parameter growing diamond membrane is used: using hydrogen and methane as reaction gas, controlling the flow point of hydrogen and methane
Not Wei 800sccm and 16sccm, deposition pressure 4.2kPa, 950 DEG C of substrate temperature, filament wattage 6300W, sedimentation time 0.5 is small
When, finally obtain the high density nano diamond thin for being formed in copper oxide matrix surface, film thickness 50nm.
Embodiment 5
A kind of preparation method of high density nano diamond thin, comprising the following steps:
Step 1 takes hard alloy substrate to carry out surface hydriding processing, keeps matrix surface positively charged: first successively by matrix
It is cleaned by ultrasonic 3-5 minutes in deionized water and alcohol, then matrix is put into microwave plasma enhanced chemical vapor deposition and is set
In standby vacuum chamber, to vacuum chamber in be only passed through high-purity hydrogen, control deposition pressure range is 4.2kPa, substrate temperature 1000
DEG C, microwave power 1000W；
Step 2 prepares the electronegative Nano diamond suspension of diamond particle surfaces, adds lysine in water and matches
It is 10 at lysine concentration-7~10-3The nano-diamond powder purchased in the market is added the lysine solution that mol/L, pH are 7
Into above-mentioned lysine solution, through ultrasonic disperse, the Nano diamond that the mass concentration of Nano diamond particle is 0.5% is obtained
Suspension；
Matrix in step 1 through surface preparation is put into the nanodiamond suspension of step 2 preparation by step 3
In, ultrasonic vibration 30 minutes, ultrasonic power 280W made Nano diamond granular absorption in cemented carbide substrate surfaces, wherein
The partial size for being adsorbed on the Nano diamond of cemented carbide substrate surfaces is 20-25nm；
Step 4 takes out matrix, is put into deionized water and embathes, then dry with nitrogen；
Sample of the nitrogen after dry is placed on the vacuum of microwave plasma enhanced chemical vapor depsotition equipment by step 5
In room, following parameter growing diamond membrane is used: using hydrogen and methane as reaction gas, controlling the flow point of hydrogen and methane
Not Wei 800sccm and 16sccm, deposition pressure 4.2kPa, 950 DEG C of substrate temperature, filament wattage 6300W, sedimentation time 0.5 is small
When, finally obtain the high density nano diamond thin for being formed in cemented carbide substrate surfaces, film thickness 100nm.
Claims (10)
1. a kind of preparation method of high density nano diamond thin, which comprises the following steps:
Workpiece substrate is taken, the workpiece substrate is subjected to surface preparation, keeps the workpiece substrate surface positively charged or negative electricity；
Lysine is added to the water, obtains lysine solution, then nano-diamond powder is added into the lysine solution, is surpassed
Obtain that Nano diamond particle surface is positively charged or the Nano diamond suspension of negative electricity after sound dispersion；
Workpiece substrate after surface preparation is immersed in suspended with the Nano diamond of the workpiece substrate oppositely charged
In liquid, ultrasonic vibration makes the Nano diamond granular absorption in the Nano diamond suspension on the workpiece substrate surface；
After the completion of absorption, the workpiece substrate is taken out, cleaned and after being dried with nitrogen, using chemical vapor depsotition equipment, in institute
State growing diamond membrane on workpiece substrate.
2. preparation method as described in claim 1, which is characterized in that the lysine solution pH value is adjusted to 3-5, is obtained
The positively charged Nano diamond suspension of Nano diamond particle surface.
3. preparation method as described in claim 1, which is characterized in that the lysine solution pH value is adjusted to 6-10, is obtained
To the electronegative Nano diamond suspension of Nano diamond particle surface.
4. preparation method as described in claim 1, which is characterized in that the concentration of lysine is 10 in the lysine solution-7
~10-3mol/L。
5. preparation method as described in claim 1, which is characterized in that the material of the workpiece substrate is silicon, silica, carbon
SiClx, copper oxide, silicon nitride or hard alloy.
6. preparation method as described in claim 1, which is characterized in that the surface preparation includes solvent cleaning treatment, oxygen
At least one of plasma cleaning processing, chemical etching processing, hydrogenation treatment.
7. preparation method as described in claim 1, which is characterized in that in the Nano diamond suspension, Nano diamond
The mass concentration of particle is 0.005-0.5%, and the partial size of Nano diamond particle is less than 50nm.
8. the workpiece that a kind of surface has high density nano diamond thin, which is characterized in that including workpiece substrate and close knot
The high density nano diamond thin on the workpiece substrate surface is closed, the material of the workpiece substrate is silicon, silica, carbon
SiClx, copper oxide, silicon nitride or hard alloy, the diamond thin with a thickness of 50-150nm.
9. workpiece as claimed in claim 8, which is characterized in that the workpiece substrate is the probe of atomic force microscopy instrument.
10. workpiece as claimed in claim 8, which is characterized in that the workpiece substrate is the micro-nano with complex three-dimensional configuration
Rice workpiece.
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| CN110885968A (en) * | 2018-09-07 | 2020-03-17 | 深圳先进技术研究院 | Preparation method of diamond coating, diamond coating prepared by preparation method and cutting tool |
| CN111004033A (en) * | 2019-11-28 | 2020-04-14 | 江苏禾吉新材料科技有限公司 | Preparation method of polycrystalline diamond cutter for cutting straws |
| CN112553590A (en) * | 2020-12-02 | 2021-03-26 | 上海征世科技有限公司 | Diamond film based on plasma vapor deposition and preparation method thereof |
| CN113897675A (en) * | 2021-09-15 | 2022-01-07 | 湖南新锋先进材料科技有限公司 | Diamond-doped particles and preparation method and application thereof |
| CN114559712A (en) * | 2022-02-15 | 2022-05-31 | 江苏诺德新材料股份有限公司 | High-temperature-resistant low-loss copper-clad plate and preparation process thereof |
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