CN103787585A - Method for depositing diamond film on quartz substrate - Google Patents
Method for depositing diamond film on quartz substrate Download PDFInfo
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- CN103787585A CN103787585A CN201410047193.6A CN201410047193A CN103787585A CN 103787585 A CN103787585 A CN 103787585A CN 201410047193 A CN201410047193 A CN 201410047193A CN 103787585 A CN103787585 A CN 103787585A
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- quartz substrate
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Abstract
The invention discloses a method for depositing a diamond film on a quartz substrate. The method comprises the following steps: cleaning preparation of quartz substrate surface, preparation of silica sol, preparation of a single-layer silica film on the quartz substrate, preparation of a multi-layer silica film doped with nano diamond, acid etching, pretreatment of substrate surface, and deposition of the diamond film. Compared with the traditional diamond surface patterning, the method disclosed by the invention has the advantages that the film is good in adhesive force, high in deposition quality, long in service life, and simple and feasible in operation. The method can be applied to kinds of protective coatings such as optical apparatuses, optical windows and the like.
Description
Technical field
The present invention relates to diamond film and manufacture field, the particularly method of depositing diamond film on quartz substrate.
Background technology
The physical and chemical performance of diamond excellence becomes the multifunctional material of tool potentiality of 21st century.CVD diamond thin has high rigidity, high heat conductance and excellent corrosion resistance characteristic, and its performance can compare favourably with natural diamond.Therefore, the supercoat using diamond film as optical window can guarantee the optical property of window, also can strengthen the adaptability of window to severe environment, thus the work-ing life of improving quartzy optical window.
CVD legal system has hot-wire chemical gas-phase deposition (HFCVD) for the main method of diamond film, microwave plasma CVD (MPCVD), and DC arc plasma is sprayed (CVD) method etc.The advantages such as it is high that the standby diamond film of CVD legal system has quality, and growth velocity is fast, have broad application prospects as supercoat.Cause adamantine nucleation rate not high but the forming core point of heterogeneous substrate is less, this directly affects adamantine growth quality, and thermal expansivity differs and makes in temperature-fall period the contraction of film and substrate inconsistent compared with conference, produces internal stress, to affect adhesion of thin film, 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 of preparing diamond film on quartz substrate, comprise the steps:
A. the colloidal sol that preparation contains silica composition, by airtight gained colloidal sol, ageing under steady temperature;
B. by colloidal sol film forming on quartz substrate of preparation, form the quartz substrate containing silica membrane;
C. in the colloidal sol of described preparation, mix Nano diamond micro mist, form Nano diamond micro mist film on the described quartz substrate containing silica membrane surface, Nano diamond micro mist evenly mixes with carbon silica membrane, and be coated to the integrity that has guaranteed crystalline structure on homogeneity substrate, do not affect every character of substrate;
D. carry out etching processing on the quartz substrate surface having formed containing Nano diamond micro mist film, the Nano diamond particle of exposing surface, then coat paraffin in the edge of quartz substrate, at quartz substrate center etching silicon dioxide film, surface appears Nano diamond particle, planting brilliant process will improve Enhancing Nucleation Density greatly, reach 10
11/ cm
-1, make diamond film more evenly complete.
E. obtain at step D containing growing diamond film on the quartz substrate of Nano diamond micro mist film.
Add grain-size little Nano diamond micro mist thin film layer and well solved the problem that heterogeneous substrate depositing diamond film Enhancing Nucleation Density is low, thermal expansion coefficient difference is larger, can enhanced film and substrate between sticking power, and increase the service life.The prepared film surface of etching processing, makes it manifest diamond particle, has solved heterogeneous substrate depositing diamond film forming core difficult problem.
In some embodiments of the present invention, before steps A, also comprise step: A
0. quartz substrate is put into alcoholic solution and carry 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 some embodiments of the present invention, between step C and D, also comprise: C
0. on quartz substrate, prepare multilayer and have the silica membrane of mixing Nano diamond micro mist of concentration gradient.Utilize the method for adding the silica membrane of mixing Nano diamond micro mist with concentration gradient, the sticking power between enhanced film and substrate, and increase the service life.
In some embodiments of the present invention, between step D and E, also comprise: D
0. quartz substrate after treatment step D is put into acetone soln and carry out ultrasonic cleaning, and then carry out supersound washing with deionized water, after taking-up, carry out surface drying processing.Acid solution in clean-up etch step, is beneficial to next step growing diamond film like this.
In some embodiments of the present invention, step B, step C and step C
0before carrying out, first colloidal sol is carried out to ultrasonication, the unsettled physical agglomeration of disperseing sol particle to form; To carry out under relative humidity is less than 50% environment with film forming on quartz substrate.
In some embodiments of the present invention, colloidal sol described in steps A is by drip deionized water and dehydrated alcohol in teos solution, regulate pH to 3-5, then add ethanamide to make, the decomposition that is more conducive to silicic acid under acidic conditions obtains more silicon-dioxide.
In some 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 evenly be mixed in solution, forms more nucleus.
In some embodiments of the present invention, described step C and step C
0middle preparation is mixed after the silica membrane of Nano diamond micro mist, quartz substrate is put into baking oven at temperature 400-600 ℃, thermal treatment 2 hours.
In some embodiments of the present invention, described step C
0the silica membrane of mixing Nano diamond micro mist of middle formation is 1-4 layer.
In some embodiments of the present invention, in described steps A, after described colloidal sol is airtight at the temperature of 50-100 ℃, ageing two days.
The advantage of the diamond surface graphics method that this method of preparing diamond film on quartz substrate surface is more traditional 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 obtains of the preparation method of an embodiment of the present invention.
Embodiment
Below in conjunction with specific embodiment, the present invention will be further described.
Embodiment 1:
1. the cleaning on quartz substrate surface preparation
By quartz substrate sample (the diameter 20mm of surfacing, thickness 2mm) put into purity 99.7% ethanol solution carry out ultrasonic (frequency 40kHz) clean 10 minutes, then carry out supersound washing 10 minutes with deionized water, after taking-up, at the temperature of 100 ℃, toast 30 minutes.
2. the preparation of silicon dioxide gel
Under 200 revs/min of speed of magnetic stirring apparatus, stir, with drop-burette, slowly to the deionized water that drips 14ml in the teos solution of 40ml purity 98.0%, the dehydrated alcohol of 120ml, adds a certain amount of hydrochloric acid to make pH value maintain 3 left and right.Homo(io)thermism, at 40 ℃, adds the ethanamide 0.5g of purity 99% and continues under 200 revs/min of speed and stir 2 hours.Afterwards by airtight the colloidal sol obtaining, ageing two days at the temperature of 50 ℃.Repeat above-mentioned steps, prepare three parts of identical colloidal sols.
3. on quartz substrate, prepare individual layer silica membrane
A copy of it colloidal sol prepared by step 2 is placed on the concussion processing of carrying out in ultrasonic wave (frequency 40kHz) 25 minutes, the unsettled physical agglomeration of disperseing sol particle to form.Be less than in relative humidity under 50% environment, continue 20s with the rotating speed of 2000r/min with photoresist spinner, make film forming on the quartz substrate of colloidal sol after step 1 is clean, under normal temperature, in saturated ammonia, place 24h.
4. preparation multilayer is mixed the silica membrane of Nano diamond
A copy of it colloidal sol prepared by step 2 mixes 1 carat, the Nano diamond micro mist of particle diameter 5nm, is placed on the concussion processing of carrying out 25min in ultrasonic wave (frequency 40kHz), the unsettled physical agglomeration of disperseing sol particle to form.Be less than in relative humidity under 50% environment, the quartz substrate containing silica membrane that step 3 is obtained is as substrate, and the rotating speed film forming 20s with photoresist spinner with 2000r/min places 24h under normal temperature in saturated ammonia.
Repeat afterwards above-mentioned steps, in the 3rd part of colloidal sol, mix 2 carats of the Nano diamond micro mists of particle diameter 5nm, prepare the second layer and mix the silica membrane of Nano diamond micro mist, put into the baking oven thermal treatment 2h of 400 ℃.
5. acid etch
Film surface prepared by step 4 drips 1ml, the hydrofluoric acid solution of purity 40%, and etching processing 2 minutes, makes it appear surperficial Nano diamond particle.Substrate edge place paraffinize, 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 substrate center.
6. the pre-treatment of substrate surface
The substrate that step 5 is 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, after taking-up, toasts 10 minutes at the temperature of 120 ℃.
7. depositing diamond film
The substrate that step 6 is cleaned is put into the vacuum cavity of MPCVD device, after vacuumizing, deposits, 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 ℃; Depositing time: 6 hours.After deposition finishes, by sample cool to room temperature, take out, growth thickness is 50 μ m.
Embodiment 2:
1. the cleaning on quartz substrate surface preparation
By quartz substrate sample (the diameter 20mm of surfacing, thickness 2mm) put into purity 99% aqueous isopropanol carry out ultrasonic (frequency 40kHz) clean 10 minutes, then carry out supersound washing 10 minutes with deionized water, after taking-up, at the temperature of 120 ℃, toast 25 minutes.
2. the preparation of silicon dioxide gel
Under 350 revs/min of speed of magnetic stirring apparatus, stir under rapid stirring, with drop-burette slowly to the deionized water that drips 14ml in the teos solution of 40ml purity 98.0%, the dehydrated alcohol of 120ml, adds a certain amount of hydrochloric acid to make pH value maintain 4 left and right.Homo(io)thermism, 60 ℃ of left and right, adds the ethanamide 0.5g of purity 99% and continues under 200 revs/min of speed and stir 2 hours.Afterwards by airtight colloidal sol, ageing two days at the temperature of 75 ℃.Repeat above-mentioned steps, prepare four parts of identical colloidal sols.
3. on quartz substrate, prepare individual layer silica membrane
A copy of it colloidal sol prepared by step 2 is placed on the concussion processing of carrying out in ultrasonic wave 25 minutes, the unsettled physical agglomeration of disperseing sol particle to form.Be less than in relative humidity under 50% environment, continue 20s with the rotating speed of 3000r/min with photoresist spinner, make film forming on the quartz substrate of colloidal sol after step 1 is clean, under normal temperature, in saturated ammonia, place 24h.
4. preparation multilayer is mixed the silica membrane of Nano diamond
A copy of it colloidal sol prepared by step 2 mixes the Nano diamond micro mist of 2 carats of particle diameter 30nm, is placed on the concussion processing of carrying out 25min in ultrasonic wave (frequency 40kHz), the unsettled physical agglomeration of disperseing sol particle to form.Be less than in relative humidity under 50% environment, the quartz substrate containing silica membrane that step 3 is obtained is as substrate, and the rotating speed film forming 20s with photoresist spinner with 3000r/min places 24h under normal temperature in saturated ammonia.
Repeat twice of above-mentioned steps, in two parts of colloidal sols preparing in step 2 respectively, mix 5 carats and 8 carats of the diadusts of particle diameter 30nm nanometer, prepare the second layer and the 3rd layer and mix the silica membrane of Nano diamond micro mist, put into the baking oven thermal treatment 2h of 500 ℃.
5. acid etch
Film surface prepared by step 4 drips the hydrofluoric acid solution of a small amount of purity 40.0%, and etching processing two minutes makes it appear surperficial Nano diamond particle.Substrate edge place paraffinize, 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 substrate center.
6. the pre-treatment of substrate surface
The substrate that step 5 is 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, after taking-up, toasts 10 minutes at the temperature of 130 ℃.
7. depositing diamond film
The substrate that step 6 is cleaned is put into the vacuum cavity of HFCVD device, after vacuumizing, deposits, and working conditions is as follows, working gas: hydrogen and methane blended gas; Gas flow: hydrogen 200sccm, methane: 8sccm; Hot-wire temperature: 2000 ℃; Operating pressure: 3.5kPa; Depositing temperature: 650 ℃; Depositing time: 6 hours.After deposition finishes, by sample cool to room temperature, take out, growth thickness is about 10 μ m.
Embodiment 3:
1. the cleaning on quartz substrate surface preparation
By quartz substrate sample (the diameter 20mm of surfacing, thickness 2mm) put into purity 99% aqueous isopropanol carry out ultrasonic (frequency 40kHz) clean 10 minutes, then carry out supersound washing 10 minutes with deionized water, after taking-up, at the temperature of 120 ℃, toast 25 minutes.
2. the preparation of silicon dioxide gel
Under 500 revs/min of speed of magnetic stirring apparatus, stir under rapid stirring, with drop-burette slowly to the deionized water that drips 14ml in the teos solution of 40ml purity 98.0%, the dehydrated alcohol of 120ml, adds a certain amount of hydrochloric acid to make pH value maintain 5 left and right.Homo(io)thermism, 80 ℃ of left and right, adds the ethanamide 0.5g of purity 99% and continues under 200 revs/min of speed and stir 2 hours.Afterwards by airtight colloidal sol, ageing two days at the temperature of 100 ℃.Repeat above-mentioned steps, prepare six parts of identical colloidal sols.
3. on quartz substrate, prepare individual layer silica membrane
A copy of it colloidal sol prepared by step 2 is placed on the concussion processing of carrying out in ultrasonic wave 25 minutes, the unsettled physical agglomeration of disperseing sol particle to form.Be less than in relative humidity under 50% environment, continue 20s with the rotating speed of 4000r/min with photoresist spinner, make film forming on the quartz substrate of colloidal sol after step 1 is clean, under normal temperature, in saturated ammonia, place 24h.
4. preparation multilayer is mixed the silica membrane of Nano diamond
A copy of it colloidal sol prepared by step 2 mixes 3 carats of particle diameter 50nm Nano diamond micro mists, is placed on the concussion processing of carrying out 25min in ultrasonic wave (frequency 40kHz), the unsettled physical agglomeration of disperseing sol particle to form.Be less than in relative humidity under 50% environment, the quartz substrate containing silica membrane that step 3 is obtained is as substrate, and the rotating speed film forming 20s with photoresist spinner with 4000r/min places 24h under normal temperature in saturated ammonia.
Repeat afterwards above-mentioned steps four times, in other four points of colloidal sols, mix 5 carats of the Nano diamond micro mists of particle diameter 50nm more at every turn, prepare the second layer to layer 5 and mix the silica membrane of Nano diamond micro mist, put into the baking oven thermal treatment 2h of 600 ℃.
5. acid etch
Film surface prepared by step 4 drips the hydrofluoric acid solution of a small amount of purity 40.0%, and etching processing two minutes makes it appear surperficial Nano diamond particle.Substrate edge place paraffinize, 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 substrate center.
6. the pre-treatment of substrate surface
The substrate that step 5 is 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, after taking-up, leaves standstill to surface drying.
7. depositing diamond film
The substrate that step 6 is cleaned is put into the vacuum cavity of DCCVD device, after vacuumizing, deposits, 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 ℃; Depositing time: 6 hours.After deposition finishes, by sample cool to room temperature, take out, growth thickness is about 10 μ m.
As shown in Figure 1, be followed successively by from top to bottom quartz plate, silica membrane, the silica membrane of mixing Nano diamond, diamond film.
Above some embodiments of the present invention describe in detail, but the invention is not restricted to above-mentioned embodiment, in the ken possessing, can also under the prerequisite that does not depart from aim of the present invention, make a variety of changes those of ordinary skills.
Claims (10)
1. the method for preparing diamond film on quartz substrate, comprises the steps:
A. the colloidal sol that preparation contains silica composition, by airtight gained colloidal sol, ageing under steady temperature;
B. by colloidal sol film forming on quartz substrate of preparation, form the quartz substrate containing silica membrane;
C. in the colloidal sol of described preparation, mix Nano diamond micro mist, form Nano diamond micro mist film on the described quartz substrate containing silica membrane surface;
D. carry out etching processing on the quartz substrate surface having formed 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. obtain at step D containing growing diamond film on the quartz substrate of Nano diamond micro mist film.
2. the method for preparing diamond film on quartz substrate according to claim 1, is characterized in that, also comprises step before steps A:
A
0. quartz substrate is put into alcoholic solution and carry out ultrasonic cleaning, then carry out supersound washing with deionized water, take out post-drying.
3. the method for preparing diamond film on quartz substrate according to claim 2, is characterized in that, between step C and D, also comprises:
C
0. on quartz substrate, prepare multilayer and have the silica membrane of mixing Nano diamond micro mist of concentration gradient.
4. the method for preparing diamond film on quartz substrate according to claim 3, is characterized in that, between step D and E, also comprises:
D
0. quartz substrate after treatment step D is put into acetone soln and carry out ultrasonic cleaning, and then carry out supersound washing with deionized water, after taking-up, carry out surface drying processing.
5. according to the method for preparing diamond film on quartz substrate described in claim 3 or 4, it is characterized in that step B, step C and step C
0before carrying out, first colloidal sol is carried out to ultrasonication, the unsettled physical agglomeration of disperseing sol particle to form; With
On quartz substrate, film forming is to carry out under relative humidity is less than 50% environment.
6. the method for preparing diamond film on quartz substrate according to claim 5, is characterized in that, colloidal sol described in steps A is by drip deionized water and dehydrated alcohol in teos solution, regulates pH to 3-5, then adds ethanamide to make.
7. according to the method for preparing diamond film on quartz substrate described in claim 3 or 6, it 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 for preparing diamond film on quartz substrate according to claim 7, is characterized in that, described step C and step C
0middle preparation is mixed after the silica membrane of Nano diamond micro mist, quartz substrate is put into baking oven at temperature 400-600 ℃, thermal treatment 2 hours.
9. according to the method for preparing diamond film on quartz substrate described in claim 3 or 8, it is characterized in that described step C
0the silica membrane of mixing Nano diamond micro mist of middle formation is 1-4 layer.
10. the method for 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 ℃, ageing two days.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018059367A1 (en) * | 2016-09-30 | 2018-04-05 | 浙江工业大学 | Method for compositing si-v luminescent diamond particle with quartz optical fiber |
| CN110318030A (en) * | 2018-03-29 | 2019-10-11 | 中国科学院宁波材料技术与工程研究所 | A kind of self-supporting superfine nano-crystalline 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 |
| CN111748790A (en) * | 2020-06-18 | 2020-10-09 | 太原理工大学 | Silica-diamond composite material coated by silica film and preparation method |
| CN112361972A (en) * | 2020-11-18 | 2021-02-12 | 华侨大学 | Multilayer film thickness and optical characteristic detection method |
| CN112684537A (en) * | 2020-12-16 | 2021-04-20 | 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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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018059367A1 (en) * | 2016-09-30 | 2018-04-05 | 浙江工业大学 | Method for compositing si-v luminescent diamond particle with quartz optical fiber |
| CN110318030A (en) * | 2018-03-29 | 2019-10-11 | 中国科学院宁波材料技术与工程研究所 | A kind of self-supporting superfine nano-crystalline diamond thick-film |
| 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 |
| CN111748790A (en) * | 2020-06-18 | 2020-10-09 | 太原理工大学 | Silica-diamond composite material coated by silica film and preparation method |
| CN112361972A (en) * | 2020-11-18 | 2021-02-12 | 华侨大学 | Multilayer film thickness and optical characteristic detection method |
| CN112684537A (en) * | 2020-12-16 | 2021-04-20 | 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 |
| 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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