CN105481262A - Method for plating X-ray parabolic reflector surface with high-reflective film - Google Patents

Method for plating X-ray parabolic reflector surface with high-reflective film Download PDF

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Publication number
CN105481262A
CN105481262A CN201510943548.4A CN201510943548A CN105481262A CN 105481262 A CN105481262 A CN 105481262A CN 201510943548 A CN201510943548 A CN 201510943548A CN 105481262 A CN105481262 A CN 105481262A
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CN
China
Prior art keywords
glass substrate
parabola
target
ray
ultrasonic cleaning
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201510943548.4A
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Chinese (zh)
Inventor
张颖
苑永涛
李海龙
程云涛
刘红
方敬忠
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Institute of Optics and Electronics of CAS
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Institute of Optics and Electronics of CAS
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Publication date
Application filed by Institute of Optics and Electronics of CAS filed Critical Institute of Optics and Electronics of CAS
Priority to CN201510943548.4A priority Critical patent/CN105481262A/en
Publication of CN105481262A publication Critical patent/CN105481262A/en
Pending legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/06Surface treatment of glass, not in the form of fibres or filaments, by coating with metals
    • C03C17/09Surface treatment of glass, not in the form of fibres or filaments, by coating with metals by deposition from the vapour phase
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00Coatings on glass
    • C03C2217/20Materials for coating a single layer on glass
    • C03C2217/25Metals
    • C03C2217/257Refractory metals
    • C03C2217/26Cr, Mo, W
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2218/00Methods for coating glass
    • C03C2218/10Deposition methods
    • C03C2218/15Deposition methods from the vapour phase
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2218/00Methods for coating glass
    • C03C2218/30Aspects of methods for coating glass not covered above
    • C03C2218/31Pre-treatment

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The invention discloses a method for plating an X-ray parabolic reflector surface with high-reflective film. The method comprises the steps of, firstly, cleaning a glass substrate; secondly, clamping the glass substrate with a specific clamp and baking the glass substrate; thirdly, coating the glass substrate with Cr film; fourthly, coating the Cr film with Ir film. The method has the advantages that reflectivity and the target use rate are high, film coatings are uniform and film adsorption capacity is high.

Description

A kind of method of X-ray parabolic mirror plated surface high-reflecting film
Technical field
The present invention relates to the technical field of X ray reflection mirror plated film, be specifically related to a kind of method of X-ray parabolic mirror plated surface high-reflecting film.
Background technology
X-ray pulsar is a kind of high speed rotation neutron star of radiation ray, and its rotation period is very stable, and the long-term stability of part millisecond pulsar can match in excellence or beauty atomic clock.According to photon time of arrival that detector measures with estimate position, through series of computation, the information such as the attitude of spacecraft, position, speed can be determined.So pulsar navigation can make spacecraft break away from dependence to artificial beacon, realize high-precision autonomous deep space navigation.Therefore, a kind of reflecting optics effectively collecting X-ray is studied significant.
Summary of the invention
Problem that the present invention will solve that the target rate of utilization that existing X ray reflection mirror method for plating film on surface exists is low, roughness is higher, adhesive force is not strong etc., and a kind of X ray reflection mirror method for plating film on surface based on duplicature system proposed.
The technical solution used in the present invention is: a kind of method of X-ray parabolic mirror plated surface high-reflecting film, carries out according to the following steps:
1) by parabola glass substrate glass cleaner ultrasonic cleaning 10 ~ 30min, then use acetone ultrasonic cleaning 10 ~ 30min, then use dehydrated alcohol ultrasonic cleaning 10 ~ 30min, finally dry by deionized water ultrasonic cleaning;
2) by the specific holder of parabola glass substrate, whole substrate interior surface is unobstructed, is placed in below magnetron sputtering coater heater strip, is evacuated to 1.0 × 10 -4pa ~ 9.9 × 10 -4pa, starts heating unit, 100 ~ 300 DEG C of baking 30min ~ 3h;
3) Ar gas is passed into, when vacuum chamber internal gas pressure reaches 0.1 ~ 3Pa, parabola glass substrate is moved to directly over Cr target, volts DS 300 ~ 500V is applied to Cr rotary target, target head rotating speed 4 ~ 15r/min, pre-sputtering 5 ~ 20min, opens baffle plate, starts to parabola glass substrate internal surface plated film 1 ~ 5min;
4) parabola glass substrate is moved to directly over Ir target, vacuum chamber internal gas pressure is still 0.1 ~ 3Pa, volts DS 300 ~ 600V is applied to Ir rotary target, target head rotating speed 4 ~ 15r/min, pre-sputtering 5 ~ 20min, open baffle plate, start to parabola glass substrate internal surface plated film 10 ~ 20min;
5), after Ir deposition, close baking power supply, in time being down to 20 ~ 25 DEG C, namely obtain X-ray parabolic mirror superficial film.
The present invention's advantage is compared with prior art:
(1), the present invention relative to the scheme of patent CN103046016A, Ir element is higher than the X ray reflection rate of C element.Film layer structure is simple, and Ir surfaceness is less than 0.1nm, after experience 80 high/low temperature loop tests (-40 DEG C ~ 80 DEG C), rete without anyly coming off, cracking phenomena appearance.
(2), the present invention adopts tubular rotary target, relative to planar target, has even film layer, the advantage of target rate of utilization high (~ 90%).
(3), the present invention adopts this clamp structure, and interior surfaces of glass is blocked without any, all can plate film and usable reflection X-ray.Relative to target up, glass substrate in below without fixture scheme, the dust that this programme has stopped inside cavity drops down onto the possibility of glass substrate surface, and make the film prepared brighter and cleaner, reflectivity is higher.
Accompanying drawing explanation
Fig. 1 is glass chip clamp schematic diagram.
Embodiment
The present embodiment is only used to further illustrate the present invention, and can not be interpreted as limiting the scope of the invention.
Embodiment 1
Adopt the borosilicate glass plated film that 0.2mm is thick, use glass cleaner, acetone, dehydrated alcohol and deionized water ultrasonic cleaning 10min successively, 10min, 10min, 10min.Be evacuated to 9.9 × 10 -4during Pa, start to toast 3h with 100 DEG C.Pass into Ar gas again, make chamber internal gas pressure reach 0.1Pa.Moved to directly over Cr target by parabola glass substrate, add 300V volts DS in Cr target, rotary target rotating speed 4r/min, pre-sputtering 5min, opens baffle plate, plating Cr film 1min.Move to directly over Ir target by parabola glass substrate again, keep logical Ar gas, in chamber, gas is still pressed as 0.1Pa, adds 300V voltage in Ir target, rotary target rotating speed 4r/min, and pre-sputtering 5min, opens baffle plate, plating Ir film 10min.
Embodiment 2
Adopt the borosilicate glass plated film that 0.2mm is thick, use glass cleaner, acetone, dehydrated alcohol and deionized water ultrasonic cleaning 20min successively, 20min, 20min, 20min.Be evacuated to 5 × 10 -4during Pa, start to toast 100min with 200 DEG C.Pass into Ar gas again, make chamber internal gas pressure reach 1Pa.Moved to directly over Cr target by parabola glass substrate, add 410V volts DS in Cr target, rotary target rotating speed 10r/min, pre-sputtering 10min, opens baffle plate, plating Cr film 3min.Move to directly over Ir target by parabola glass substrate again, keep logical Ar gas, chamber internal gas pressure is still 1Pa, adds 470V voltage in Ir target, rotary target rotating speed 10/min, and pre-sputtering 10min, opens baffle plate, plating Ir film 12min.
Embodiment 3
Adopt the borosilicate glass plated film that 0.2mm is thick, use glass cleaner, acetone, dehydrated alcohol and deionized water ultrasonic cleaning 30min successively, 30min, 30min, 30min.Be evacuated to 1.0 × 10 -4during Pa, start to toast 30min with 300 DEG C.Pass into Ar gas again, make chamber internal gas pressure reach 3Pa.Moved to directly over Cr target by parabola glass substrate, add 500V volts DS in Cr target, rotary target rotating speed 15r/min, pre-sputtering 20min, opens baffle plate, plating Cr film 5min.Move to directly over Ir target by parabola glass substrate again, keep logical Ar gas, chamber internal gas pressure is still 3Pa, adds 600V voltage in Ir target, rotary target rotating speed 15/min, and pre-sputtering 20min, opens baffle plate, plating Ir film 20min.

Claims (5)

1. a method for X-ray parabolic mirror plated surface high-reflecting film, is characterized in that: comprise the following steps:
1) by parabola glass substrate glass cleaner ultrasonic cleaning 10 ~ 30min, then use acetone ultrasonic cleaning 10 ~ 30min, then use dehydrated alcohol ultrasonic cleaning 10 ~ 30min, finally dry with deionized water ultrasonic cleaning 10 ~ 30min;
2) by the specific holder of parabola glass substrate, whole substrate interior surface is unobstructed, is placed in below magnetron sputtering coater heater strip, is evacuated to 1.0 × 10 -4pa ~ 9.9 × 10 -4pa, starts heating unit, 100 ~ 300 DEG C of baking 30min ~ 3h;
3) Ar gas is passed into, when vacuum chamber internal gas pressure reaches 0.1 ~ 3Pa, parabola glass substrate is moved to directly over Cr target, volts DS 300 ~ 500V is applied to Cr rotary target, target head rotating speed 4 ~ 15r/min, pre-sputtering 5 ~ 20min, opens baffle plate, starts to parabola glass substrate internal surface plated film 1 ~ 5min;
4) parabola glass substrate is moved to directly over Ir target, vacuum chamber internal gas pressure is still 0.1 ~ 3Pa, volts DS 300 ~ 600V is applied to Ir rotary target, target head rotating speed 4 ~ 15r/min, pre-sputtering 5 ~ 20min, open baffle plate, start to parabola glass substrate internal surface plated film 10 ~ 20min;
5), after Ir deposition, close baking power supply, in time being down to 20 ~ 25 DEG C, namely obtain X-ray parabolic mirror superficial film.
2. the method for X-ray parabolic mirror plated surface high-reflecting film according to claim 1, it is characterized in that: described step 1) in by parabola glass substrate glass cleaner ultrasonic cleaning 20min, use acetone ultrasonic cleaning 20min again, then use dehydrated alcohol ultrasonic cleaning 20min, finally dry with deionized water ultrasonic cleaning 20min.
3. the method for X-ray parabolic mirror plated surface high-reflecting film according to claim 1, is characterized in that: described step 2) in parabola glass substrate is placed in below magnetron sputtering coater heater strip, be evacuated to 5.0 × 10 -4pa, starts heating unit, 200 DEG C of baking 100min.
4. the method for X-ray parabolic mirror plated surface high-reflecting film according to claim 1, is characterized in that: described step 3) in operating air pressure be 1Pa, use Cr rotary target, target head rotating speed 10r/min, apply volts DS 410V, pre-sputtering 10min, plated film time 3min.
5. the method for X-ray parabolic mirror plated surface high-reflecting film according to claim 1, is characterized in that: described step 4) in operating air pressure be 1Pa, use Ir rotary target, target head rotating speed 10r/min, apply volts DS 470V, pre-sputtering 10min, plated film time 12min.
CN201510943548.4A 2015-12-16 2015-12-16 Method for plating X-ray parabolic reflector surface with high-reflective film Pending CN105481262A (en)

Priority Applications (1)

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CN201510943548.4A CN105481262A (en) 2015-12-16 2015-12-16 Method for plating X-ray parabolic reflector surface with high-reflective film

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Application Number Priority Date Filing Date Title
CN201510943548.4A CN105481262A (en) 2015-12-16 2015-12-16 Method for plating X-ray parabolic reflector surface with high-reflective film

Publications (1)

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CN105481262A true CN105481262A (en) 2016-04-13

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03107104A (en) * 1989-09-20 1991-05-07 Ise Shinku Kogaku Kk Heat ray absorptive reflecting mirror
CN103046016A (en) * 2013-01-22 2013-04-17 哈尔滨工业大学 Method for coating film on surface of X-ray reflector

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03107104A (en) * 1989-09-20 1991-05-07 Ise Shinku Kogaku Kk Heat ray absorptive reflecting mirror
CN103046016A (en) * 2013-01-22 2013-04-17 哈尔滨工业大学 Method for coating film on surface of X-ray reflector

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
KAI-WING CHAN等: "Coating Thin Mirror Segments for Lightweight X-ray Optics", 《PROC. OF SPIE》 *
王蓓等: "4.48nm正入射软X射线激光用Cr/C多层膜高反射镜的研制", 《光学学报》 *

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Application publication date: 20160413