CN101244897A - Glass ball cover with amorphous diamond film for photoelectric detection system and preparation method thereof - Google Patents

Abstract

A glass spherical cover with an amorphous diamond film for a photoelectric detection system and a preparation method thereof, which belong to a glass spherical cover with a hard surface and a preparation method thereof. It is to overcome the low hardness of the glass dome cover outside the OEPS-27 photoelectric detection system, poor scratch resistance and corrosion resistance, easy damage to the surface, and the existing method of coating amorphous diamond film cannot be firmly fixed on the dome cover glass. Drawbacks of coating amorphous diamond films are presented. It consists of a dome cover glass substrate, a silicon film middle layer and an amorphous diamond film layer; the silicon film middle layer is plated on the outer surface of the dome glass base, and the amorphous diamond film is plated on the outer surface of the silicon film middle layer. The preparation steps are as follows: (1) cleaning the dome cover glass substrate, (2) ionizing backsputtering, (3) depositing the middle layer of the silicon film, (4) ion etching, and (5) depositing the amorphous diamond film layer on the middle layer of the silicon film. The beneficial effect of the invention is that the glass spherical cover has high hardness, good scratch resistance and corrosion resistance, and good transmittance in the optical working band.

Description

Glass ball cover with amorphous diamond film for photoelectric detection system and preparation method thereof

technical field

The invention relates to a glass ball cover and a preparation method thereof, in particular to a glass ball cover whose outer surface is coated with an amorphous diamond film and a preparation method thereof.

Background technique

The glass dome outside the OEPS-27 photoelectric detection system has low hardness, poor scratch resistance and corrosion resistance, and the surface is easily damaged or even cracked, resulting in a decrease in transmittance, which directly affects the OEPS-27 photoelectric system. normal operation and service life. In order to improve the hardness of the glass dome itself, a hard amorphous diamond film is usually coated on its surface, but due to the extremely poor adhesion between the dome glass and the amorphous diamond film, the existing method of coating an amorphous diamond film is difficult. An amorphous diamond film is firmly coated on the surface of the dome glass.

Contents of the invention

The present invention solves the low hardness, poor scratch resistance and corrosion resistance of the OEPS-27 photoelectric system external glass dome cover, the surface is easily damaged, and the existing method of coating an amorphous diamond film cannot be applied to the dome cover. In view of the disadvantage of firmly coating the amorphous diamond film on the glass surface, a glass ball cover with an amorphous diamond film for a photodetection system and its preparation method are proposed.

A glass dome cover with an amorphous diamond film for a photoelectric detection system, which includes a dome glass substrate 1, a silicon film intermediate layer 2 and an amorphous diamond film layer 3; the silicon film interlayer 2 is plated on the outside of the dome glass substrate 1 On the surface, the amorphous diamond film layer 3 is plated on the outer surface of the silicon film middle layer 2 .

The preparation method of the glass ball cover with the amorphous diamond film of the photoelectric detection system, the specific steps are as follows:

Step 1: Wash the ball cover glass substrate 1 in an ultrasonic cleaner with acetone for 15 minutes, then wash the ball cover glass substrate 1 with alcohol in an ultrasonic cleaner for 15 minutes, and finally rinse it with deionized water and dry it at room temperature;

Step 2: Using single crystal silicon as the target material, place the cleaned and dried dome glass substrate 1 on the sample heating table in the magnetron sputtering vacuum chamber, and extract the air in the vacuum chamber through the vacuum system to make the vacuum degree of the vacuum chamber reach 1.5×10 ^-4 Pa to 2.0×10 ^-4 Pa, then heat the dome glass substrate 1 to 600°C and keep it warm for 60 minutes. Pa ~ 6.0Pa, add 400V ~ 500V DC voltage to ionize the surface of the dome glass substrate 1, and the ionization backsplash time is 10min ~ 20min

Step 3: After ionization and backsputter cleaning, apply 170W RF power to the monocrystalline silicon target for ignition, control the flow rate of argon gas to 25 sccm, pre-sputter the monocrystalline silicon target for 3 minutes to 5 minutes, and reduce the air pressure in the vacuum chamber Lower and keep it at 1.2Pa, remove the baffle between the single crystal silicon target and the dome glass substrate 1 to deposit the silicon film interlayer 2, control the sputtering time range from 15s to 40s, and the range of film thickness After the deposition is completed, turn off the power, and when the temperature in the vacuum chamber drops to room temperature, take out the dome glass substrate 1 coated with the silicon film intermediate layer 2, and finish coating the dome glass substrate 1 with the silicon film middle layer. Layer 2.

Step 4: Fix the dome glass substrate 1 coated with the silicon film intermediate layer 2 on the sample chuck of the filtered cathode vacuum arc vacuum chamber and turn it to the etching position, and evacuate the filtered cathode vacuum arc vacuum chamber to a vacuum degree After the pressure is 1.5×10 ^-4 ~ 2.0×10 ^-4 -Pa, argon gas with a purity of 99.999% is introduced, and the flow rate is controlled at 8 sccm, so that the vacuum degree in the vacuum chamber reaches 1.5×10 ^-2 ~ 2.0×10 ^-2 Pa, The surface of the sample was etched and cleaned with a Kaufman ion gun, the etching energy of argon ions was 800-1100eV, and the etching time was 7 minutes;

Step 5: After the etching is completed, turn the sample plate to the deposition position after an interval of 10 to 20 minutes, set the arc current to 60A, the pulse frequency to 1500Hz, and the pulse width to 25μs, and continuously control the dome cover coated with the silicon film intermediate layer 2 The glass substrate 1 pulse bias ranges from -3000V to -80V, deposits the amorphous diamond film layer 3, controls the deposition time in the range of 100s to 150s, and the thickness of the film in the range of 40nm to 60nm. After the nitrogen gas is fed, the door of the chamber is opened to take out the dome glass substrate 1 coated with the amorphous diamond film layer 3 on the silicon film intermediate layer 2 .

The beneficial effect of the present invention is that the glass dome cover of the OEPS-27 photoelectric system not only has the advantages of high hardness, good scratch resistance and corrosion resistance, but also has good transmittance in the optical working band of the OEPS-27 photoelectric system , and effectively improved the reuse rate of the glass dome cover of the OEPS-27 photoelectric system. The quality of the amorphous diamond film coated by the preparation method of the present invention is excellent and has a strong binding force with the dome glass substrate 1 based on the general specification for optical film layers (GJB2485-95); The surface hardness of the invention is raised to 20GPa from 7.5GPa of the spherical cover glass substrate 1 not coated with the amorphous diamond film; Fig. 2 and Fig. 3; two pictures based on the optical transmittance test to detect that the present invention still maintains a high transmittance in the optical working band, as shown in Fig. 4 .

Description of drawings

Fig. 1 is the structural representation of the present invention; Fig. 2 is the hardness and Young's modulus schematic diagram of the dome glass that surface is not coated with amorphous diamond film, and the blank column in the accompanying drawing represents hardness parameter, and shadow column represents Young's modulus Parameter; Fig. 3 is the hardness of the present invention and Young's modulus schematic diagram, and the blank column in the accompanying drawing represents hardness parameter, and the shaded column represents Young's modulus parameter; Fig. 4 is the ball cover glass prepared by the present invention and the surface is not coated The comparison schematic diagram of the Fourier infrared transmittance of the dome glass of the amorphous diamond film, the solid line in the accompanying drawing is the Fourier infrared transmittance curve of the dome glass prepared by the present invention, and the dotted line is the ball whose surface is not coated with the amorphous diamond film FTIR transmittance curve of cover glass.

Detailed ways

Specific embodiment one: this embodiment is described in conjunction with Fig. 1, and this embodiment is made up of dome cover glass substrate 1, silicon film interlayer 2 and amorphous diamond film layer 3; Silicon film interlayer 2 is plated on dome cover glass substrate 1 On the outer surface of the silicon film middle layer 2, an amorphous diamond film layer 3 is plated. The dome glass of the present invention is a special optical glass whose main components are aluminum oxide Al ₂ O ₃ , calcium oxide CaO and a small amount of metal oxides and fluorides. It belongs to a kind of calcium aluminum glass. Laser and mid-infrared bands have a high transmittance of 80% to 85%. A silicon film intermediate layer 2 is added between the dome cover glass substrate 1 and the amorphous diamond film group 3, which firmly coats the amorphous diamond film group 3 on the dome cover without affecting the overall optical transmittance. On the glass substrate 1, the present invention not only has the advantages of high hardness, good scratch resistance and corrosion resistance, but also has good transmittance in the optical working band of the OEPS-27 photoelectric system.

Specific embodiment two: this embodiment is described in conjunction with Fig. 1, the difference between this embodiment and specific embodiment one is that a second amorphous diamond film layer 4 is added on the upper surface of the amorphous diamond film layer 3, and the second amorphous diamond film layer The diamond film layer 4 is plated on the outer surface of the amorphous diamond film layer 3 . Other compositions and connection methods are the same as those in Embodiment 1. The advantage of adding the second amorphous diamond film layer 4 is to further improve the surface hardness and anti-scratch performance.

Embodiment 3: This embodiment differs from Embodiment 1 in that it includes at least two amorphous diamond film layers. Other compositions and connection methods are the same as those in Embodiment 1.

Specific embodiment four: the preparation method of the glass ball cover with the amorphous diamond film of the photoelectric detection system of the present embodiment, it is characterized in that the steps of preparation method are as follows:

Step 1: Wash the ball cover glass substrate 1 in an ultrasonic cleaner with acetone for 15 minutes, then wash the ball cover glass substrate 1 with alcohol in an ultrasonic cleaner for 15 minutes, and finally rinse it with deionized water and dry it at room temperature;

Step 2: Using single crystal silicon as the target material, place the cleaned and dried dome glass substrate 1 on the sample heating table in the magnetron sputtering vacuum chamber, and extract the air in the vacuum chamber through the vacuum system to make the vacuum degree of the vacuum chamber reach 1.5×10 ^-4 Pa～2.0×10 ^-4 Pa, then heat the dome glass substrate 1 to 600°C and keep it warm for 60 minutes. Pa ~ 6.0Pa, plus 400V ~ 500V DC voltage to perform ionization backsplash on the surface of the dome glass substrate 1, and the ionization backsplash time is 10min ~ 20min;

Step 3: After ionization and backsputter cleaning, apply 170W RF power to the monocrystalline silicon target for ignition, control the flow rate of argon gas to 25 sccm, pre-sputter the monocrystalline silicon target for 3 minutes to 5 minutes, and reduce the air pressure in the vacuum chamber Lower and keep it at 1.2Pa, remove the baffle between the single crystal silicon target and the dome glass substrate 1 to deposit the silicon film interlayer 2, control the sputtering time range from 15s to 40s, and the range of film thickness 10nm to 30nm; turn off the power after the deposition is completed, and when the temperature in the vacuum chamber drops to room temperature, take out the dome glass substrate 1 coated with the silicon film intermediate layer 2, and finish coating the dome glass substrate 1 with the silicon film middle layer. Layer 2.

Step 4: Fix the dome glass substrate 1 coated with the silicon film intermediate layer 2 on the sample chuck of the filtered cathode vacuum arc vacuum chamber and turn it to the etching position, and evacuate the filtered cathode vacuum arc vacuum chamber to a vacuum degree After the pressure is 1.5×10 ^-4 ~ 2.0×10 ^-4 Pa, argon gas with a purity of 99.999% is introduced, and the flow rate is controlled at 8 sccm, so that the vacuum degree in the vacuum chamber reaches 1.5×10 ^-2 ~ 2.0×10 ^-2 Pa. The Kaufmann ion gun etched and cleaned the surface of the sample, the etching energy of argon ions was 800-1100eV, and the etching time was 7 minutes;

Step 5: After the etching is completed, turn the sample plate to the deposition position after an interval of 10 to 20 minutes, set the arc current to 60A, the pulse frequency to 1500Hz, and the pulse width to 25μs, and continuously control the dome cover coated with the silicon film intermediate layer 2 The glass substrate 1 pulse bias voltage ranges from -3000V to -80V, deposits the amorphous diamond film layer 3, controls the deposition time range from 100 to 150s, and the film thickness range from 40nm to 60nm. After the nitrogen gas is fed, the door of the chamber is opened to take out the dome glass substrate 1 coated with the amorphous diamond film layer 3 on the silicon film intermediate layer 2 . The preparation method of the silicon film intermediate layer 2 has a good combination with the dome glass substrate 1 and the amorphous diamond film layer 3, which overcomes the inability of the conventional method to firmly coat the amorphous diamond film layer on the dome glass substrate 1. However, the multi-layer amorphous diamond film is prepared by continuously controlling the bias voltage of the dome glass substrate 1 coated with the silicon film intermediate layer 2, which achieves the purpose of reducing internal stress and enhancing the adhesion of the amorphous diamond film layer.

Embodiment 5: The difference between this embodiment and Embodiment 4 is that in step 5, the pulse bias voltage of the dome glass substrate 1 coated with the silicon film intermediate layer 2 is controlled to be -1000V～-500V. Other parameters and steps are the same as in Embodiment 4.

Embodiment 6: The difference between this embodiment and Embodiment 4 is that the deposition time of the amorphous diamond film layer 3 in Step 5 is 200s-250s. Other parameters and steps are the same as in Embodiment 4. Prolonging the deposition time of the amorphous diamond film layer 3 is to increase the thickness of the amorphous diamond film layer 3 to meet various application requirements.

Specific embodiment seven: the difference between this embodiment and specific embodiment four is that the preparation method of depositing the second amorphous diamond film layer 4 on the amorphous diamond film layer 3 is as follows: after the deposition of the amorphous diamond film layer 3 is completed, an intermittent 10min ~20 minutes later, adjust the pulse bias voltage of the dome glass substrate 1 coated with the silicon film intermediate layer 2 to -200V ~ -80V, deposit the second amorphous diamond film layer 4, the deposition time ranges from 50s to 120s, and the thickness of the film layer The range of 20nm ~ 50nm. Other parameters and steps are the same as in Embodiment 4. The advantage of adding the second amorphous diamond film layer 4 is to further improve the surface hardness and anti-scratch performance.

Claims (7)

1. A glass dome cover with an amorphous diamond film for a photoelectric detection system, characterized in that it includes a dome cover glass substrate (1), a silicon film intermediate layer (2) and an amorphous diamond film layer (3); the silicon film intermediate layer (2) plated on the outer surface of the dome glass substrate (1), and the amorphous diamond film layer (3) is plated on the outer surface of the silicon film intermediate layer (2). 2. The glass dome cover with amorphous diamond film of the photoelectric detection system according to claim 1, characterized in that it also includes a second amorphous diamond film layer (4) on the upper surface of the amorphous diamond film layer (3) ), the second amorphous diamond film layer (4) is plated on the outer surface of the amorphous diamond film layer (3). 3. The glass dome cover with amorphous diamond film for photoelectric detection system according to claim 1, characterized in that it contains at least two layers of amorphous diamond film. 4. A method for preparing a glass ball cover with an amorphous diamond film for a photoelectric detection system, characterized in that the steps of the preparation method are as follows: Step 1: Clean the ball cover glass substrate (1) in an ultrasonic cleaner with acetone for 15 minutes, then clean the ball cover glass substrate (1) with alcohol in an ultrasonic cleaner for 15 minutes, and finally rinse it with deionized water and leave it at room temperature dry; Step 2: Using single crystal silicon as the target material, place the cleaned and dried dome glass substrate (1) on the sample heating table in the magnetron sputtering vacuum chamber, and extract the air in the vacuum chamber through the vacuum system to make the vacuum chamber temperature reaches 1.5×10 ^-4 Pa to 2.0×10 ^-4 Pa, then heat the dome glass substrate (1) to 600°C and keep it warm for 60 minutes. The air pressure rises to 5.0Pa～6.0Pa, and a DC voltage of 400V～500V is applied to ionize and splash back the surface of the dome glass substrate (1), and the time for ionizing backsplash is 10min～20min; Step 3: After ionization and backsputter cleaning, apply 170W RF power to the monocrystalline silicon target for ignition, control the flow rate of argon gas to 25 sccm, pre-sputter the monocrystalline silicon target for 3 minutes to 5 minutes, and reduce the air pressure in the vacuum chamber Lower and keep it at 1.2Pa, remove the baffle between the single crystal silicon target and the dome glass substrate (1) to deposit the silicon film interlayer (2), control the sputtering time in the range of 15s to 40s, the film The layer thickness ranges from 10nm to 30nm. After the deposition is completed, turn off the power, and when the temperature in the vacuum chamber drops to room temperature, take out the dome glass substrate (1) coated with the silicon film intermediate layer (2), and complete the dome glass substrate. A silicon film intermediate layer (2) is plated on the substrate (1); Step 4: Fix the dome glass substrate (1) coated with the silicon film intermediate layer (2) on the sample chuck of the filtered cathode vacuum arc vacuum chamber and turn it to the etching position, and pump the filtered cathode vacuum arc vacuum chamber into Vacuum until the vacuum degree is 1.5×10 ^-4 ~ 2.0×10 ^-4 Pa, then pass in argon gas with a purity of 99.999%, and control the flow rate to 8 sccm, so that the vacuum degree in the vacuum chamber reaches 1.5×10 ^-2 ~ 2.0×10 ^{- 2} Pa, use the Kaufman ion gun to etch and clean the surface of the sample, the etching energy of argon ions is 800-1100eV, and the etching time is 7min; Step 5: After the etching is completed, turn the sample plate to the deposition position after an interval of 10 to 20 minutes, set the arc current to 60A, the pulse frequency to 1500Hz, and the pulse width to 25μs, and continuously control the thickness of the middle layer (2) coated with silicon film. The dome cover glass substrate (1) has a pulse bias voltage ranging from -3000V to -80V to deposit an amorphous diamond film (3). After completion, feed nitrogen into the vacuum chamber, open the chamber door, and take out the dome glass substrate (1) coated with the amorphous diamond film layer (3) on the silicon film intermediate layer (2). 5. The method for preparing a glass dome cover with an amorphous diamond film for a photoelectric detection system according to claim 4, characterized in that in step five, the dome cover glass substrate (1) coated with a silicon film intermediate layer (2) is controlled The pulse bias voltage is -1000V～-500V. 6. The method for preparing a glass dome cover with an amorphous diamond film for a photoelectric detection system according to claim 4, characterized in that the deposition time of the amorphous diamond film layer (3) in step 5 is 200s-250s. 7. The method for preparing the glass dome cover with the amorphous diamond film of the photoelectric detection system according to claim 4, characterized in that the second amorphous diamond film layer (4) is deposited on the amorphous diamond film layer (3) The preparation method is as follows: after the deposition of the amorphous diamond film (3) is completed, after an interval of 10 minutes to 20 minutes, adjust the pulse bias voltage of the dome glass substrate (1) to -200V to -80V, and deposit the second amorphous diamond film ( 4), the thickness of the film layer ranges from 20nm to 50nm, and the deposition time ranges from 50s to 120s.

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