CN103787585B - The method of depositing diamond film on quartz substrate - Google Patents
The method of depositing diamond film on quartz substrate Download PDFInfo
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- CN103787585B CN103787585B CN201410047193.6A CN201410047193A CN103787585B CN 103787585 B CN103787585 B CN 103787585B CN 201410047193 A CN201410047193 A CN 201410047193A CN 103787585 B CN103787585 B CN 103787585B
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Abstract
This application discloses a kind of method preparing diamond film on quartz substrate, comprise on the cleaning preparation on quartz substrate surface, the preparation of silicon dioxide gel, quartz substrate and prepare individual layer silica membrane, silica membrane that preparation multilayer mixes Nano diamond, acid etch, the pre-treatment of substrate surface, depositing diamond film step.The advantage of the diamond surface graphics that method of the present invention is more traditional is that adhesive force is good, and deposition quality is high, long service life, and operation is simple and feasible, and the method can be applied to various optics, the supercoat such as optical window.
Description
Technical field
The present invention relates to diamond film and manufacture field, particularly the method for depositing diamond film on quartz substrate.
Background technology
The physical and chemical performance of diamond excellence becomes the multifunctional material of 21st century most potentiality.Cvd diamond film has high rigidity, the corrosion resistance characteristic of high heat conductance and excellence, and its performance can compare favourably with natural diamond.Therefore, diamond film can be ensured the optical property of window as the supercoat of optical window, also can strengthen the adaptability of window to severe environment, thus improve the work-ing life of quartz-optical window.
The main method that CVD prepares diamond film has hot-wire chemical gas-phase deposition (HFCVD), microwave plasma CVD (MPCVD), Dc arc plasma jet CVD (CVD) method etc.The advantages such as it is high that diamond film prepared by CVD has quality, and growth velocity is fast, have broad application prospects as supercoat.But the forming core of hetero-substrates point is less causes adamantine nucleation rate not high, this directly affects adamantine growth quality, and thermal expansivity difference makes the contraction of film and substrate in temperature-fall period inconsistent compared with conference, produces internal stress, to adhesion of thin film be affected, reduce the work-ing life of coating.
Summary of the invention
In view of problems of the prior art, the invention provides a kind of method preparing diamond film on quartz substrate, comprise the steps:
A. the colloidal sol of preparation containing silica composition, by airtight for gained colloidal sol, ageing under steady temperature;
B. by colloidal sol film forming on quartz substrate of preparation, the quartz substrate containing silica membrane is formed;
C. in the colloidal sol of described preparation, Nano diamond micro mist is mixed, Nano diamond micro mist film is formed on the described surface of the quartz substrate containing silica membrane, Nano diamond micro mist and carbon silica membrane Homogeneous phase mixing, and be coated to the integrity that homogeneity substrate ensure that crystalline structure, do not affect every character of substrate;
D. etching processing is carried out defining the quartz substrate surface containing Nano diamond micro mist film, the Nano diamond particle of exposing surface, then paraffin is coated in the edge of quartz substrate, at quartz substrate center etching silicon dioxide film, surface open Nano diamond particle, plant brilliant process and greatly will improve Enhancing Nucleation Density, reach 10
11/ cm
-1, make diamond film more evenly complete.
E. step D obtain containing Nano diamond micro mist film quartz substrate on growing diamond film.
Add the little Nano diamond micro mist thin film layer of grain-size and well solve the problem that hetero-substrates depositing diamond film Enhancing Nucleation Density is low, thermal expansion coefficient difference is larger, can sticking power between enhanced film and substrate, and increase the service life.Film surface prepared by etching processing, makes it manifest diamond particle, solves hetero-substrates depositing diamond film forming core difficult problem.
In certain embodiments of the present invention, before steps A, also step is comprised: A
0. quartz substrate is put into alcoholic solution and carries out ultrasonic cleaning, then carry out supersound washing with deionized water, take out post-drying.Be convenient to form the quartz substrate containing silica membrane, make its difficult drop-off.
In certain embodiments of the present invention, also comprise between step C and D: C
0. on quartz substrate, prepare the silica membrane mixing Nano diamond micro mist that multilayer has concentration gradient.Utilize the method for mixing the silica membrane of Nano diamond micro mist of adding and there is concentration gradient, the sticking power between enhanced film and substrate, and increase the service life.
In certain embodiments of the present invention, also comprise between step D and E: D
0. the quartz substrate after step D process is put into acetone soln and carries out ultrasonic cleaning, and then carry out supersound washing with deionized water, after taking-up, carry out surface drying process.Acid solution in such clean-up etch step, is beneficial to next step growing diamond film.
In certain embodiments of the present invention, step B, step C and step C
0first colloidal sol is carried out ultrasonication before carrying out, the physical agglomeration of the granuloplastic instability of dispersion sol; Carry out under relative humidity is less than the environment of 50% with film forming on quartz substrate.
In certain embodiments of the present invention, colloidal sol described in steps A is by dripping deionized water and dehydrated alcohol in teos solution, regulate pH to 3-5, then add ethanamide and obtain, the decomposition being more conducive to silicic acid in acid condition obtains more silicon-dioxide.
In certain embodiments of the present invention, described step B, step C and step C
0the rotating speed of middle photoresist spinner is 2000-4000r/min, and the time length is 20s; Described step C and step C
0in the Nano diamond grain size of micropowder that mixes be 5-50nm, Nano diamond micro crystal size is little, can Homogeneous phase mixing in solution, form more nucleus.
In certain embodiments of the present invention, described step C and step C
0after the silica membrane of Nano diamond micro mist is mixed in middle preparation, quartz substrate is put into baking oven at temperature 400-600 DEG C, thermal treatment 2 hours.
In certain embodiments of the present invention, described step C
0the silica membrane mixing Nano diamond micro mist of middle formation is 1-4 layer.
In certain embodiments of the present invention, in described steps A, after described colloidal sol is airtight at the temperature of 50-100 DEG C, ageing two days.
This advantage preparing the more traditional diamond surface graphics method of the method for diamond film on quartz substrate surface is: adhesive force is good; long service life; operation is simple and feasible, and the method can be applied to various optics, the supercoat of optical window etc.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the diamond film structure that the preparation method of an embodiment of the present invention obtains.
Embodiment
Below in conjunction with specific embodiment, the present invention will be further described.
Embodiment 1:
1. the cleaning preparation on quartz substrate surface
By quartz substrate sample (the diameter 20mm of surfacing, thickness 2mm) put into purity 99.7% ethanol solution and carry out ultrasonic (frequency 40kHz) and clean 10 minutes, then carry out supersound washing 10 minutes with deionized water, toast 30 minutes at the temperature of 100 DEG C after taking-up.
2. the preparation of silicon dioxide gel
Stir under magnetic stirring apparatus 200 revs/min of speed, in the teos solution of 40ml purity 98.0%, drip the deionized water of 14ml slowly with drop-burette, the dehydrated alcohol of 120ml, add a certain amount of hydrochloric acid and make pH value maintain about 3.Homo(io)thermism, at 40 DEG C, adds the ethanamide 0.5g of purity 99% and under 200 revs/min of speed, continues stirring 2 hours.Afterwards by airtight for the colloidal sol obtained, ageing two days at the temperature of 50 DEG C.Repeat above-mentioned steps, prepare three parts of identical colloidal sols.
3. individual layer silica membrane prepared by quartz substrate
A copy of it colloidal sol step 2 prepared is placed in ultrasonic wave (frequency 40kHz) the concussion process carried out 25 minutes, the physical agglomeration of the granuloplastic instability of dispersion sol.Be less than the environment of 50% in relative humidity under, continue 20s with photoresist spinner with the rotating speed of 2000r/min, make film forming on the quartz substrate of colloidal sol after step 1 is clean, under normal temperature, in saturated ammonia, place 24h.
4. prepare the silica membrane that multilayer mixes Nano diamond
A copy of it colloidal sol step 2 prepared mixes 1 carat, the Nano diamond micro mist of particle diameter 5nm, is placed on the concussion process carrying out 25min in ultrasonic wave (frequency 40kHz), the physical agglomeration of the granuloplastic instability of dispersion sol.Be less than the environment of 50% in relative humidity under, the quartz substrate containing silica membrane step 3 obtained, as substrate, with photoresist spinner with the rotating speed film forming 20s of 2000r/min, places 24h under normal temperature in saturated ammonia.
Repeat above-mentioned steps afterwards, in the 3rd part of colloidal sol, mix the Nano diamond micro mist 2 carats of particle diameter 5nm, prepare the silica membrane that the second layer mixes Nano diamond micro mist, put into the baking oven thermal treatment 2h of 400 DEG C.
5. acid etch
Film surface step 4 prepared drips 1ml, the hydrofluoric acid solution of purity 40%, etching processing 2 minutes, makes it appear the Nano diamond particle on surface.Substrate edge place paraffinize, the heart drips purity 40%HF acid 3ml and purity 28% nitric acid 9ml mixing solutions (its volume proportion is 3:1) etching surface silicon-dioxide 30min in the substrate.
6. the pre-treatment of substrate surface
Substrate step 5 processed is put into purity 28% acetone soln and is carried out ultrasonic cleaning 15 minutes, then carries out supersound washing 15 minutes with deionized water, toasts 10 minutes after taking-up at the temperature of 120 DEG C.
7. depositing diamond film
The vacuum cavity of MPCVD device put into by substrate step 6 cleaned, and deposits after vacuumizing, and working conditions is as follows, working gas: hydrogen and methane blended gas; Gas flow: hydrogen 200sccm, methane 5sccm; Microwave power: 1200W; Operating pressure: 5.0kPa; Depositing temperature: 600 DEG C; Depositing time: 6 hours.By sample cool to room temperature after deposition terminates, take out, growth thickness is 50 μm.
Embodiment 2:
1. the cleaning preparation on quartz substrate surface
By quartz substrate sample (the diameter 20mm of surfacing, thickness 2mm) put into purity 99% aqueous isopropanol and carry out ultrasonic (frequency 40kHz) and clean 10 minutes, then carry out supersound washing 10 minutes with deionized water, toast 25 minutes at the temperature of 120 DEG C after taking-up.
2. the preparation of silicon dioxide gel
Stir rapid stirring under 350 revs/min of speed of magnetic stirring apparatus under, in the teos solution of 40ml purity 98.0%, the deionized water of 14ml is dripped slowly with drop-burette, the dehydrated alcohol of 120ml, adds a certain amount of hydrochloric acid and makes pH value maintain about 4.Homo(io)thermism, at about 60 DEG C, adds the ethanamide 0.5g of purity 99% and under 200 revs/min of speed, continues stirring 2 hours.Afterwards by airtight for colloidal sol, ageing two days at the temperature of 75 DEG C.Repeat above-mentioned steps, prepare four parts of identical colloidal sols.
3. individual layer silica membrane prepared by quartz substrate
A copy of it colloidal sol step 2 prepared is placed in ultrasonic wave the concussion process carried out 25 minutes, the physical agglomeration of the granuloplastic instability of dispersion sol.Be less than the environment of 50% in relative humidity under, continue 20s with photoresist spinner with the rotating speed of 3000r/min, make film forming on the quartz substrate of colloidal sol after step 1 is clean, under normal temperature, in saturated ammonia, place 24h.
4. prepare the silica membrane that multilayer mixes Nano diamond
A copy of it colloidal sol step 2 prepared mixes the Nano diamond micro mist of 2 carats of particle diameter 30nm, is placed on the concussion process carrying out 25min in ultrasonic wave (frequency 40kHz), the physical agglomeration of the granuloplastic instability of dispersion sol.Be less than the environment of 50% in relative humidity under, the quartz substrate containing silica membrane step 3 obtained, as substrate, with photoresist spinner with the rotating speed film forming 20s of 3000r/min, places 24h under normal temperature in saturated ammonia.
Repeat above-mentioned steps twice, the diadust 5 carats of particle diameter 30nm nanometer and 8 carats are mixed in the two parts of colloidal sols prepared in step 2 respectively, prepare the silica membrane that the second layer and third layer mix Nano diamond micro mist, put into the baking oven thermal treatment 2h of 500 DEG C.
5. acid etch
Film surface step 4 prepared drips the hydrofluoric acid solution of a small amount of purity 40.0%, etching processing two minutes, makes it appear the Nano diamond particle on surface.Substrate edge place paraffinize, the heart drips purity 40%HF acid 3ml and purity 28% nitric acid 9ml mixing solutions (its volume proportion is 3:1) etching surface silicon-dioxide 30min in the substrate.
6. the pre-treatment of substrate surface
Substrate step 5 processed is put into purity 28% acetone soln and is carried out ultrasonic cleaning 15 minutes, then carries out supersound washing 15 minutes with deionized water, toasts 10 minutes after taking-up at the temperature of 130 DEG C.
7. depositing diamond film
The vacuum cavity of HFCVD device put into by substrate step 6 cleaned, and deposits after vacuumizing, and working conditions is as follows, working gas: hydrogen and methane blended gas; Gas flow: hydrogen 200sccm, methane: 8sccm; Hot-wire temperature: 2000 DEG C; Operating pressure: 3.5kPa; Depositing temperature: 650 DEG C; Depositing time: 6 hours.By sample cool to room temperature after deposition terminates, take out, growth thickness is about 10 μm.
Embodiment 3:
1. the cleaning preparation on quartz substrate surface
By quartz substrate sample (the diameter 20mm of surfacing, thickness 2mm) put into purity 99% aqueous isopropanol and carry out ultrasonic (frequency 40kHz) and clean 10 minutes, then carry out supersound washing 10 minutes with deionized water, toast 25 minutes at the temperature of 120 DEG C after taking-up.
2. the preparation of silicon dioxide gel
Stir rapid stirring under 500 revs/min of speed of magnetic stirring apparatus under, in the teos solution of 40ml purity 98.0%, the deionized water of 14ml is dripped slowly with drop-burette, the dehydrated alcohol of 120ml, adds a certain amount of hydrochloric acid and makes pH value maintain about 5.Homo(io)thermism, at about 80 DEG C, adds the ethanamide 0.5g of purity 99% and under 200 revs/min of speed, continues stirring 2 hours.Afterwards by airtight for colloidal sol, ageing two days at the temperature of 100 DEG C.Repeat above-mentioned steps, prepare six parts of identical colloidal sols.
3. individual layer silica membrane prepared by quartz substrate
A copy of it colloidal sol step 2 prepared is placed in ultrasonic wave the concussion process carried out 25 minutes, the physical agglomeration of the granuloplastic instability of dispersion sol.Be less than the environment of 50% in relative humidity under, continue 20s with photoresist spinner with the rotating speed of 4000r/min, make film forming on the quartz substrate of colloidal sol after step 1 is clean, under normal temperature, in saturated ammonia, place 24h.
4. prepare the silica membrane that multilayer mixes Nano diamond
A copy of it colloidal sol step 2 prepared mixes 3 carats of particle diameter 50nm Nano diamond micro mists, is placed on the concussion process carrying out 25min in ultrasonic wave (frequency 40kHz), the physical agglomeration of the granuloplastic instability of dispersion sol.Be less than the environment of 50% in relative humidity under, the quartz substrate containing silica membrane step 3 obtained, as substrate, with photoresist spinner with the rotating speed film forming 20s of 4000r/min, places 24h under normal temperature in saturated ammonia.
Repeat four above-mentioned steps afterwards, in other four points of colloidal sols, mix the Nano diamond micro mist 5 carats of particle diameter 50nm more at every turn, prepare the silica membrane that the second layer to layer 5 mixes Nano diamond micro mist, put into the baking oven thermal treatment 2h of 600 DEG C.
5. acid etch
Film surface step 4 prepared drips the hydrofluoric acid solution of a small amount of purity 40.0%, etching processing two minutes, makes it appear the Nano diamond particle on surface.Substrate edge place paraffinize, the heart drips purity 40%HF acid 3ml and purity 28% nitric acid 9ml mixing solutions (its volume proportion is 3:1) etching surface silicon-dioxide 30min in the substrate.
6. the pre-treatment of substrate surface
Substrate step 5 processed is put into purity 28% acetone soln and is carried out ultrasonic cleaning 15 minutes, then carries out supersound washing 15 minutes with deionized water, leaves standstill to surface drying after taking-up.
7. depositing diamond film
The vacuum cavity of DCCVD device put into by substrate step 6 cleaned, and deposits after vacuumizing, and working conditions is as follows, working gas: hydrogen and methane blended gas; Gas flow: hydrogen 200sccm, methane: 8sccm; Operating pressure: 3.5kPa; Depositing temperature: 650 DEG C; Depositing time: 6 hours.By sample cool to room temperature after deposition terminates, take out, growth thickness is about 10 μm.
As shown in Figure 1, quartz plate, silica membrane, the silica membrane mixing Nano diamond, diamond film is followed successively by from top to bottom.
Above some embodiments of the present invention elaborate, but the invention is not restricted to above-mentioned embodiment, in the ken that those of ordinary skill in the art possess, can also make a variety of changes under the prerequisite not departing from present inventive concept.
Claims (10)
1. on quartz substrate, prepare the method for diamond film, comprise the steps:
A. the colloidal sol of preparation containing silica composition, by airtight for gained colloidal sol, ageing under steady temperature;
B. by colloidal sol film forming on quartz substrate of preparation, the quartz substrate containing silica membrane is formed;
C. in the colloidal sol of described preparation, mix Nano diamond micro mist, form Nano diamond micro mist film on the described surface of the quartz substrate containing silica membrane;
D. carry out etching processing defining the quartz substrate surface containing Nano diamond micro mist film, the Nano diamond particle of exposing surface, then coats paraffin in the edge of quartz substrate, at quartz substrate center etching silicon dioxide film;
E. step D obtain containing Nano diamond micro mist film quartz substrate on growing diamond film.
2. the method preparing diamond film on quartz substrate according to claim 1, is characterized in that, before steps A, also comprise step:
A
0. quartz substrate is put into alcoholic solution and carries out ultrasonic cleaning, then carry out supersound washing with deionized water, take out post-drying.
3. the method preparing diamond film on quartz substrate according to claim 2, is characterized in that, also comprise between step C and D:
C
0. on quartz substrate, prepare the Nano diamond micro mist film that multilayer has concentration gradient.
4. the method preparing diamond film on quartz substrate according to claim 3, is characterized in that, also comprise between step D and E:
D
0. the quartz substrate after step D process is put into acetone soln and carries out ultrasonic cleaning, and then carry out supersound washing with deionized water, after taking-up, carry out surface drying process.
5. the method preparing diamond film on quartz substrate according to claim 3 or 4, is characterized in that, step B, step C and step C
0first colloidal sol is carried out ultrasonication before carrying out, the physical agglomeration of the granuloplastic instability of dispersion sol; With
On quartz substrate, film forming is carried out under relative humidity is less than the environment of 50%.
6. the method preparing diamond film on quartz substrate according to claim 5, is characterized in that, colloidal sol described in steps A is by dripping deionized water and dehydrated alcohol in teos solution, regulate pH to 3-5, then add ethanamide obtain.
7. the method preparing diamond film on quartz substrate according to claim 3 or 6, is characterized in that, described step B, step C and step C
0the rotating speed of middle photoresist spinner is 2000-4000r/min, and the time length is 20s; Described step C and step C
0in the Nano diamond grain size of micropowder that mixes be 5-50nm.
8. the method preparing diamond film on quartz substrate according to claim 7, is characterized in that, described step C and step C
0in prepare Nano diamond micro mist film after, quartz substrate is put into baking oven at temperature 400-600 DEG C, thermal treatment 2 hours.
9. the method preparing diamond film on quartz substrate according to claim 3 or 8, is characterized in that, described step C
0the silica membrane mixing Nano diamond micro mist of middle formation is 1-4 layer.
10. the method preparing diamond film on quartz substrate according to claim 9, is characterized in that, after colloidal sol described in steps A is airtight at the temperature of 50-100 DEG C, and ageing two days.
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| CN106637129B (en) * | 2016-09-30 | 2019-04-09 | 浙江工业大学 | A kind of complex method for the diamond particles and silica fibre that Si-V is luminous |
| CN110318030B (en) * | 2018-03-29 | 2021-10-22 | 中国科学院宁波材料技术与工程研究所 | Self-supporting superfine nanocrystalline diamond thick film |
| CN110449332A (en) * | 2019-08-13 | 2019-11-15 | 上海金铎禹辰水环境工程有限公司 | A kind of composite construction diamond thin and preparation method thereof |
| CN111748790B (en) * | 2020-06-18 | 2022-03-08 | 太原理工大学 | Silica-diamond composite material coated by silica film and preparation method |
| CN112361972B (en) * | 2020-11-18 | 2022-11-01 | 华侨大学 | Multilayer film thickness and optical characteristic detection method |
| CN112684537B (en) * | 2020-12-16 | 2022-06-10 | 新沂市中大石英科技有限公司 | Quartz optical fiber with excellent optical transmission performance and preparation method thereof |
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| EP0417190A1 (en) * | 1988-06-03 | 1991-03-20 | Massachusetts Institute Of Technology | Silicon dioxide films on diamond |
| CN1041119C (en) * | 1994-04-01 | 1998-12-09 | 吉林大学 | SOI integrate circuit chip material containing diamond film and its making technology |
| CN1037386C (en) * | 1995-12-12 | 1998-02-11 | 吉林大学 | Thin silicon chip material on diamond film and its prepn. |
| CN1082099C (en) * | 1999-05-08 | 2002-04-03 | 吉林大学 | Process for selective growth of diamond film by nano crystal introduction |
| KR101268272B1 (en) * | 2004-05-27 | 2013-05-31 | 도쿠리츠교세이호징 붓시쯔 자이료 겐큐키코 | Nano-crystal diamond film manufacturing method thereof and device using nano-crystal diamond film |
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