CN101244897B - Preparation method of glass marble cover with amorphous diamond film of photodetection system - Google Patents
Preparation method of glass marble cover with amorphous diamond film of photodetection system Download PDFInfo
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- CN101244897B CN101244897B CN2008100641715A CN200810064171A CN101244897B CN 101244897 B CN101244897 B CN 101244897B CN 2008100641715 A CN2008100641715 A CN 2008100641715A CN 200810064171 A CN200810064171 A CN 200810064171A CN 101244897 B CN101244897 B CN 101244897B
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- glass
- ball cover
- amorphous diamond
- cover substrate
- middle layer
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Abstract
The invention relates to a glass ball cover with an amorphous diamond film of a photodetection system and a preparation method, which belongs to a glass ball cover with a hard surface and the preparation method thereof. The glass ball cover with the amorphous diamond film of the invention is proposed for overcoming the defect that the glass ball cover outside the OEPS-27 photodetection system is low in hardness, bad in scratch resistance and corrosion resistance, easy in surface damage, and the existing coating method of the amorphous diamond film cannot coat the amorphous diamond film on the glass of the ball cover firmly. The glass ball cover consists of a glass basement of the ball cover, a silicon film interlayer and an amorphous diamond film; the silicon film interlayer is plated on the external surface of the glass basement of the ball cover, and the amorphous diamond film is plated on the external surface of the silicon film interlayer. The preparation steps are as follows: firstly, the glass basement of the ball cover is washed; secondly, ionizing and back washing are carried out; thirdly, the silicon film interlayer is deposited; fourthly, ion etching is carried out; fifthly, the amorphous diamond film is deposited on the silicon film interlayer. The glass ball cover with an amorphous diamond film and a preparation method of the invention has the advantages of leading the glass ball cover to be high in hardness, good in scratch resistance and corrosion resistance has good transmittance in optical working wave bands.
Description
Technical field
The present invention relates to a kind of glass ball cover and preparation method thereof, be specifically related to glass ball cover of a kind of outside surface coating non-crystal diamond film and preparation method thereof.
Background technology
The hardness of the glass ball cover of OEPS-27 Photodetection system outside own is lower, anti-zoned wiping and erosion resistance are relatively poor, the surface is easily caused damage even is broken, and causes transmitance to descend, thereby directly has influence on the works better and the work-ing life of OEPS-27 electro-optical system.In order to improve the hardness of glass ball cover own, usually at its surface applied hard non-crystal diamond film, but because the sticking power extreme difference of ball cover glass and non-crystal diamond film, the existing method that applies non-crystal diamond film is difficult on the surface of ball cover glass and applies non-crystal diamond film securely.
Summary of the invention
The present invention can not apply the shortcoming of non-crystal diamond film at the ball cover glass surface securely for the method for existing coating non-crystal diamond film, and proposes a kind of preparation method of glass ball cover of band non-crystal diamond film of Photodetection system.
The glass ball cover of the band amorphous diamond film of Photodetection system, it comprises ball cover substrate of glass 1 and amorphous diamond rete 3; It also comprises silicon fiml middle layer 2; Silicon fiml middle layer 2 is coated on the outside surface of ball cover substrate of glass 1, and amorphous diamond rete 3 is coated on the outside surface in silicon fiml middle layer 2.
The preparation method of the glass ball cover of the band amorphous diamond film of Photodetection system, concrete steps are as follows:
Step 1: with acetone ball cover substrate of glass 1 is cleaned 15min in Ultrasonic Cleaners, and then ball cover substrate of glass 1 is cleaned 15min in Ultrasonic Cleaners, rinse the back drying at room temperature well with deionized water at last with alcohol;
Step 2:, as target the ball cover substrate of glass 1 behind the cleaning-drying is placed on the sample warm table in the magnetron sputtering vacuum chamber with silicon single crystal, makes the vacuum tightness of vacuum chamber reach 1.5 * 10 by the indoor air of vacuum system extracting vacuum
-4Pa～2.0 * 10
-4Pa, be incubated 60min after then ball cover substrate of glass 1 being heated to 600 ℃, insulation finishes the back, and to feed purity be that 99.999% argon gas makes pressure rises in the vacuum chamber to 5.0Pa～6.0Pa, the volts DS that adds 400V～500V carries out the ionization backwash to the surface of ball cover substrate of glass 1, and the time of ionization backwash is 10min～20min;
Step 3: the ionization backwash cleans and finishes, the radio frequency power that applies 170W on the silicon single crystal target carries out starter, the flow of control argon gas is 25sccm, the silicon single crystal target spattered behind 3min～5min in advance the air pressure in the vacuum chamber reduced and remain on 1.2Pa, remove the deposition that baffle plate between silicon single crystal target and the ball cover substrate of glass 1 carries out silicon fiml middle layer 2, the scope of control sputtering time is 15s～40s, the scope of thicknesses of layers is 10nm～30nm, powered-down after deposition finishes, when treating that the interior temperature of vacuum chamber is reduced to room temperature, the ball cover substrate of glass 1 that is coated with silicon fiml middle layer 2 is taken out, finish and on ball cover substrate of glass 1, be coated with silicon fiml middle layer 2.
Step 4: the ball cover substrate of glass 1 that will be coated with silicon fiml middle layer 2 is fixed on the sample chuck of filtered cathodic vacuum arc vacuum chamber and goes to the etching position, with the filtered cathodic vacuum arc vacuum chamber be evacuated to vacuum tightness be 1.5 * 10
-4～2.0 * 10
-4Feeding purity is 99.999% argon gas behind the-Pa, and dominant discharge is 8sccm, makes the vacuum tightness in the vacuum chamber reach 1.5 * 10
-2～2.0 * 10
-2Pa utilizes the Kaufman ion gun that sample surfaces is carried out the etching cleaning, and etching argon ion energy is 800～1100eV, and etching time is 7min;
Step 5: after etching finishes, intermittently behind 10～20min sample disc is gone to deposition position, it is 60A that flame current is set, pulse-repetition is 1500Hz, the pulse pulsewidth is 25 μ s, stepless control be coated with silicon fiml middle layer 2 ball cover substrate of glass 1 pulsed bias scope for-3000V～-80V, deposited amorphous diamond rete 3, the scope of control depositing time is 100s～150s, the scope of thicknesses of layers is 40nm～60nm, after deposition finishes, in vacuum chamber, open the chamber door behind the feeding nitrogen and take out the ball cover substrate of glass 1 that on silicon fiml middle layer 2, is coated with amorphous diamond rete 3.
Beneficial effect of the present invention is to make the glass ball cover of OEPS-27 electro-optical system not only to have the advantage of hardness height, anti-zoned wiping and good corrosion resistance, and also have good transmitance, and effectively improved the repeat usage of the glass ball cover of OEPS-27 electro-optical system at the optics service band of OEPS-27 electro-optical system.Detect the superior in quality of the non-crystal diamond film that adopts preparation method's coating of the present invention based on optical film general specification (GJB2485-95), and extremely strong with the bonding force of ball cover substrate of glass 1; Detect surface hardness of the present invention based on nano indentation test and bring up to 20GPa by the 7.5GPa of the ball cover substrate of glass 1 of uncoated non-crystal diamond film; Young's modulus is brought up to 200GPa by the 114GPa of the ball cover substrate of glass 1 of uncoated non-crystal diamond film, sees Fig. 2 and Fig. 3; Two width of cloth also keep very high transmitance based on optical transmittance test detection the present invention at the optics service band, see Fig. 4.
Description of drawings
Fig. 1 is a structural representation of the present invention; Fig. 2 is the hardness and the Young's modulus synoptic diagram of the ball cover glass of surperficial uncoated non-crystal diamond film, and the blank post in the accompanying drawing is represented hardness parameter, and the shade post is represented the Young's modulus parameter; Fig. 3 is hardness of the present invention and Young's modulus synoptic diagram, and the blank post in the accompanying drawing is represented hardness parameter, and the shade post is represented the Young's modulus parameter; Fig. 4 is the ball cover glass of the present invention preparation and the fourier infrared transmitance comparison synoptic diagram of the ball cover glass of surperficial uncoated non-crystal diamond film, solid line is the fourier infrared transmittance curve of the ball cover glass of the present invention's preparation in the accompanying drawing, and dotted line is the fourier infrared transmittance curve of the ball cover glass of surperficial uncoated non-crystal diamond film.
Embodiment
Embodiment one: in conjunction with Fig. 1 present embodiment is described, present embodiment is by ball cover substrate of glass 1, and silicon fiml middle layer 2 and amorphous diamond rete 3 are formed; Silicon fiml middle layer 2 is coated on the outside surface of ball cover substrate of glass 1, and amorphous diamond rete 3 is coated on the outside surface in silicon fiml middle layer 2.Ball cover glass of the present invention is a kind of special opticglass, is aluminium oxide Al through its main component of composition detection
2O
3, calcium oxide CaO and little metal oxide compound and fluorochemical belong to a kind of calcium lead glass, have 80%～85% high permeability in laser and middle-infrared band.Increased silicon fiml middle layer 2 between ball cover substrate of glass 1 and the amorphous diamond rete group 3, it is under the prerequisite that does not influence whole optical transmittance, amorphous diamond rete group 3 is plated on the ball cover substrate of glass 1 securely, make the present invention not only have the advantage of hardness height, anti-zoned wiping and good corrosion resistance, and also have good transmitance at the optics service band of OEPS-27 electro-optical system.
Embodiment two: present embodiment is described in conjunction with Fig. 1, present embodiment and embodiment one difference are that the upper surface at amorphous diamond rete 3 has also increased by the second amorphous diamond rete, 4, the second amorphous diamond retes 4 and has been coated on the outside surface of amorphous diamond rete 3.Other composition is identical with embodiment one with mode of connection.The benefit that increases by the second amorphous diamond rete 4 is further to improve surface hardness and anti-zoned wiping performance.
Embodiment three: present embodiment and embodiment one difference are to comprise at least two layers of amorphous diamond rete.Other composition is identical with embodiment one with mode of connection.
Embodiment four: the preparation method of the glass ball cover of the band non-crystal diamond film of present embodiment Photodetection system is characterized in that preparation method's step is as follows:
Step 1: with acetone ball cover substrate of glass 1 is cleaned 15min in Ultrasonic Cleaners, and then ball cover substrate of glass 1 is cleaned 15min in Ultrasonic Cleaners, rinse the back drying at room temperature well with deionized water at last with alcohol;
Step 2:, as target the ball cover substrate of glass 1 behind the cleaning-drying is placed on the sample warm table in the magnetron sputtering vacuum chamber with silicon single crystal, makes the vacuum tightness of vacuum chamber reach 1.5 * 10 by the indoor air of vacuum system extracting vacuum
-4Pa～2.0 * 10
-4Pa, be incubated 60min after then ball cover substrate of glass 1 being heated to 600 ℃, insulation finishes the back, and to feed purity be that 99.999% argon gas makes pressure rises in the vacuum chamber to 5.0Pa～6.0Pa, the volts DS that adds 400V～500V carries out the ionization backwash to the surface of ball cover substrate of glass 1, and the time of ionization backwash is 10min～20min;
Step 3: the ionization backwash cleans and finishes, the radio frequency power that applies 170W on the silicon single crystal target carries out starter, the flow of control argon gas is 25sccm, the silicon single crystal target spattered behind 3min～5min in advance the air pressure in the vacuum chamber reduced and remain on 1.2Pa, remove the deposition that baffle plate between silicon single crystal target and the ball cover substrate of glass 1 carries out silicon fiml middle layer 2, the scope of control sputtering time is 15s～40s, and the scope of thicknesses of layers is 10nm～30nm; Powered-down after deposition finishes when treating that the interior temperature of vacuum chamber is reduced to room temperature, takes out the ball cover substrate of glass 1 that is coated with silicon fiml middle layer 2, finishes and be coated with silicon fiml middle layer 2 on ball cover substrate of glass 1.
Step 4: the ball cover substrate of glass 1 that will be coated with silicon fiml middle layer 2 is fixed on the sample chuck of filtered cathodic vacuum arc vacuum chamber and goes to the etching position, with the filtered cathodic vacuum arc vacuum chamber be evacuated to vacuum tightness be 1.5 * 10
-4～2.0 * 10
-4Feeding purity is 99.999% argon gas behind the Pa, and dominant discharge is 8sccm, makes the vacuum tightness in the vacuum chamber reach 1.5 * 10
-2～2.0 * 10
-2Pa utilizes the Kaufman ion gun that sample surfaces is carried out the etching cleaning, and etching argon ion energy is 800～1100eV, and etching time is 7min
Step 5: after etching finishes, intermittently behind 10～20min sample disc is gone to deposition position, it is 60A that flame current is set, pulse-repetition is 1500Hz, the pulse pulsewidth is 25 μ s, stepless control be coated with silicon fiml middle layer 2 ball cover substrate of glass 1 pulsed bias scope for-3000V～-80V, deposited amorphous diamond rete 3, the scope of control depositing time is 100～150s, the scope of thicknesses of layers is 40nm～60nm, after deposition finishes, in vacuum chamber, open the chamber door behind the feeding nitrogen and take out the ball cover substrate of glass 1 that on silicon fiml middle layer 2, is coated with amorphous diamond rete 3.This preparation method silicon fiml middle layer 2 all has good binding with ball cover substrate of glass 1 and amorphous diamond rete 3, overcome the shortcoming that ordinary method can't be plated in the amorphous diamond rete this type of ball cover glass basis 1 securely, and prepared the multilayer non-crystal diamond film by the bias voltage that stepless control is coated with the ball cover substrate of glass 1 in silicon fiml middle layer 2, reach the reduction internal stress, strengthened the purpose of amorphous diamond rete tack.
Embodiment five: present embodiment and embodiment four differences be in the step 5 ball cover substrate of glass 1 pulsed bias that control is coated with silicon fiml middle layer 2 for-1000V～-500V.Other parameter is identical with embodiment four with step.
Embodiment six: present embodiment and embodiment four differences are that the depositing time of amorphous diamond rete 3 in the step 5 is 200s～250s.Other parameter is identical with embodiment four with step.The depositing time that prolongs amorphous diamond rete 3 is increased for the thickness that makes amorphous diamond rete 3, thereby satisfies various application demands.
Embodiment seven: present embodiment and embodiment four differences are in the preparation method of the deposition second amorphous diamond rete 4 on the amorphous diamond rete 3 as follows: after amorphous diamond rete 3 depositions finish, intermittently behind 10min～20min, ball cover substrate of glass 1 pulsed bias that adjusting is coated with silicon fiml middle layer 2 for-200V～-80V, deposit the second amorphous diamond rete 4, the scope of depositing time is 50s～120S, and the scope of thicknesses of layers is 20nm～50nm.Other parameter is identical with embodiment four with step.The benefit that increases by the second amorphous diamond rete 4 is further to improve surface hardness and anti-zoned wiping performance.
Claims (3)
1. the preparation method of the glass ball cover of the band amorphous diamond film of Photodetection system, the glass ball cover of the band amorphous diamond film of described Photodetection system comprises ball cover substrate of glass (1) and amorphous diamond rete (3); It also comprises silicon fiml middle layer (2); Silicon fiml middle layer (2) is coated on the outside surface of ball cover substrate of glass (1), and amorphous diamond rete (3) is coated on the outside surface of silicon fiml middle layer (2); Upper surface at amorphous diamond rete (3) also comprises the second amorphous diamond rete (4), and the second amorphous diamond rete (4) is coated on the outside surface of amorphous diamond rete (3); The step that it is characterized in that the preparation method is as follows:
Step 1: with acetone ball cover substrate of glass (1) is cleaned 15min in Ultrasonic Cleaners, and then ball cover substrate of glass (1) is cleaned 15min in Ultrasonic Cleaners, rinse the back drying at room temperature well with deionized water at last with alcohol;
Step 2:, as target the ball cover substrate of glass (1) behind the cleaning-drying is placed on the interior sample warm table of magnetron sputtering vacuum chamber with silicon single crystal, makes the vacuum tightness of vacuum chamber reach 1.5 * 10 by the indoor air of vacuum system extracting vacuum
-4Pa～2.0 * 10
-4Pa, be incubated 60min after then ball cover substrate of glass (1) being heated to 600 ℃, insulation finishes the back, and to feed purity be that 99.999% argon gas makes pressure rises in the vacuum chamber to 5.0Pa～6.0Pa, the volts DS that adds 400V～500V carries out the ionization backwash to the surface of ball cover substrate of glass (1), and the time of ionization backwash is 10min～20min;
Step 3: the ionization backwash cleans and finishes, the radio frequency power that applies 170W on the silicon single crystal target carries out starter, the flow of control argon gas is 25sccm, the silicon single crystal target spattered behind 3min～5min in advance the air pressure in the vacuum chamber reduced and remain on 1.2Pa, remove the deposition that baffle plate between silicon single crystal target and the ball cover substrate of glass (1) carries out silicon fiml middle layer (2), the scope of control sputtering time is 15s～40s, the scope of thicknesses of layers is 10nm～30nm, powered-down after deposition finishes, when treating that the interior temperature of vacuum chamber is reduced to room temperature, the ball cover substrate of glass (1) that will be coated with silicon fiml middle layer (2) is taken out, and finishes and be coated with silicon fiml middle layer (2) on ball cover substrate of glass (1);
Step 4: the ball cover substrate of glass (1) that will be coated with silicon fiml middle layer (2) is fixed on the sample chuck of filtered cathodic vacuum arc vacuum chamber and goes to the etching position, with the filtered cathodic vacuum arc vacuum chamber be evacuated to vacuum tightness be 1.5 * 10
-4～2.0 * 10
-4Feeding purity is 99.999% argon gas behind the Pa, and dominant discharge is 8sccm, makes the vacuum tightness in the vacuum chamber reach 1.5 * 10
-2～2.0 * 10
-2Pa utilizes the Kaufman ion gun that sample surfaces is carried out the etching cleaning, and etching argon ion energy is 800～1100eV, and etching time is 7min;
Step 5: after etching finishes, intermittently behind 10～20min sample disc is gone to deposition position, it is 60A that flame current is set, pulse-repetition is 1500Hz, the pulse pulsewidth is 25 μ s, stepless control be coated with silicon fiml middle layer (2) ball cover substrate of glass (1) pulsed bias scope for-3000V～-80V, deposited amorphous diamond rete (3), the scope of control depositing time is 100s～150s, the scope of thicknesses of layers is 40nm～60nm, after deposition finishes, in vacuum chamber, open the chamber door behind the feeding nitrogen and take out the ball cover substrate of glass (1) that on silicon fiml middle layer (2), is coated with amorphous diamond rete (3).
2. the preparation method of the glass ball cover of the band amorphous diamond film of Photodetection system according to claim 1, it is characterized in that ball cover substrate of glass (1) pulsed bias that control in the step 5 is coated with silicon fiml middle layer (2) for-1000V～-500V.
3. the preparation method of the glass ball cover of the band amorphous diamond film of Photodetection system according to claim 1, it is as follows to it is characterized in that going up the preparation method who deposits the second amorphous diamond rete (4) at amorphous diamond rete (3): after amorphous diamond rete (3) deposition finishes, intermittently behind 10min～20min, regulate ball cover substrate of glass (1) pulsed bias and be-200V～-80V, deposit the second amorphous diamond rete (4), the scope of thicknesses of layers is 20nm～50nm, and the scope of depositing time is 50s～120s.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2008100641715A CN101244897B (en) | 2008-03-25 | 2008-03-25 | Preparation method of glass marble cover with amorphous diamond film of photodetection system |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2008100641715A CN101244897B (en) | 2008-03-25 | 2008-03-25 | Preparation method of glass marble cover with amorphous diamond film of photodetection system |
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| CN101244897A CN101244897A (en) | 2008-08-20 |
| CN101244897B true CN101244897B (en) | 2011-08-31 |
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| CN106119796A (en) * | 2016-08-03 | 2016-11-16 | 广东工业大学 | A kind of preparation method of amorphous diamond coatings |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1033653A (en) * | 1987-12-22 | 1989-07-05 | 昆明物理研究所 | Method for coating diamond-like carbon film on infrared lens of germanium and silicon |
| CN1227162A (en) * | 1998-12-04 | 1999-09-01 | 中国科学院上海冶金研究所 | Non-crystal multilayer diamond film material with metal titanium as interface layer and its preparing method and use |
| US6753042B1 (en) * | 2000-05-02 | 2004-06-22 | Itac Limited | Diamond-like carbon thin film coating process |
| CN1752278A (en) * | 2005-10-14 | 2006-03-29 | 南京航空航天大学 | Method for mfg. diamond coating on spherical substrate and device thereof |
| CN1928151A (en) * | 2006-07-21 | 2007-03-14 | 上海大学 | Method for preparing thickness controllable trilayer type diamond membrane |
-
2008
- 2008-03-25 CN CN2008100641715A patent/CN101244897B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1033653A (en) * | 1987-12-22 | 1989-07-05 | 昆明物理研究所 | Method for coating diamond-like carbon film on infrared lens of germanium and silicon |
| CN1227162A (en) * | 1998-12-04 | 1999-09-01 | 中国科学院上海冶金研究所 | Non-crystal multilayer diamond film material with metal titanium as interface layer and its preparing method and use |
| US6753042B1 (en) * | 2000-05-02 | 2004-06-22 | Itac Limited | Diamond-like carbon thin film coating process |
| CN1752278A (en) * | 2005-10-14 | 2006-03-29 | 南京航空航天大学 | Method for mfg. diamond coating on spherical substrate and device thereof |
| CN1928151A (en) * | 2006-07-21 | 2007-03-14 | 上海大学 | Method for preparing thickness controllable trilayer type diamond membrane |
Non-Patent Citations (2)
| Title |
|---|
| JP实公开6-33239Y2 1994.08.31 |
| JP特开平5-174369A 1993.07.13 |
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Assignee: Jiangsu spark Solar Lighting Co., Ltd. Assignor: Harbin Institute of Technology Contract record no.: 2012320000297 Denomination of invention: Preparation method of glass marble cover with amorphous diamond film of photodetection system Granted publication date: 20110831 License type: Exclusive License Open date: 20080820 Record date: 20120326 |
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