CN103046016A - Method for coating film on surface of X-ray reflector - Google Patents
Method for coating film on surface of X-ray reflector Download PDFInfo
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- CN103046016A CN103046016A CN201310023048XA CN201310023048A CN103046016A CN 103046016 A CN103046016 A CN 103046016A CN 201310023048X A CN201310023048X A CN 201310023048XA CN 201310023048 A CN201310023048 A CN 201310023048A CN 103046016 A CN103046016 A CN 103046016A
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Abstract
The invention relates to a method for coating a film on a surface of an X-ray reflector, and the method can be used for solving the problems of high interface roughness between films and mixing and diffusion between the films in the prior art. The method comprises the following steps: 1, washing a glass base; 2, heating and keeping the glass base warm, and carrying out backwash cleaning on the surface of the glass base; 3, coating a titanium film on the surface of the glass base; 4, carrying out backwash spurting on the surface of the titanium film; 5, coating a carbon film on the surface of the titanium film; 6, carrying out backwash spurting on the surface of the carbon film; and 7, cutting off the power supply, cooling down to room temperature and finishing the film preparation on the surface of the X-ray. The method is applicable to the field of thin film engineering.
Description
Technical field
The present invention relates to the method for X ray reflection mirror surface coating.
Background technology
Inertial confinement fusion ICF(Inertial Confinement Fusion) is the miniature pellet that uses the fusionable material such as light laser bombardment deuterium tritium to form, pellet is ionized, form high-temperature plasma on every side at pellet.Plasma body outwards explodes, and produces huge radial pressure, makes the center produce high temperature and pressure, causes nuclear fusion reaction.For to the diagnosing of the high-temperature plasma of inside, the X ray emission of using plasma self is as the foundation of diagnosis, is present the most frequently used method.Wherein the X ray reflection mirror is the critical elements of inertial confinement fusion X-ray spectrum diagnosis.
The main method of X ray reflection mirror surface coating is magnetron sputtering method.Bonding force when the method is coated with speculum between rete and substrate is good, and sedimentation rate and deposited particles energy are easy to control, and sputter rate is high.The ubiquitous problem of X ray reflection mirror that adopts at present this kind method plated film to obtain is that reflectivity is very fast with X ray energy increase decay, and high energy cut-off threshold values is low, and is almost nil to the sigmatron reflectivity, directly affects the accuracy of diagnositc system.Its major cause be between the rete that is coated with of X ray reflection mirror surface interface roughness large (interface roughness is about 0.4nm ~ 0.55nm) and the phenomenon that has the phase mutual diffusion between the rete, directly cause the X ray reflection specular reflectivity low, even can't reflect sigmatron.
Summary of the invention
The present invention will solve the method for existing X ray reflection mirror surface coating to exist between interface roughness is large between rete problem and rete and have the problem of mixing with diffusion, and proposes a kind of method of X ray reflection mirror surface coating.
The method of a kind of X ray reflection mirror surface coating among the present invention is carried out according to the following steps:
One, substrate of glass is used acetone ultrasonic cleaning 15min ~ 30min, cleaned 15min ~ 30min with dehydrated alcohol again, use at last washed with de-ionized water 15min ~ 30min post-drying;
Two, substrate of glass is placed on the rotary heating platform in the magnetron sputtering vacuum storehouse, make the substrate center over against the center of titanium target, will be evacuated in the vacuum storehouse by vacuum acquiring system, vacuum tightness reaches 1.0 * 10 in the hole capital after selling all securities of taking seriously
-4Pa ~ 9.9 * 10
-4During Pa, start heating unit, be heated to 25 ℃ ~ 650 ℃, and insulation 10min ~ 120min; Pass into Ar gas, when pressure is 3Pa ~ 5Pa in the hole capital after selling all securities of taking seriously, apply the negative voltage of 200V ~ 800V to the rotary heating platform, substrate of glass is carried out backwash clean 10min ~ 20min;
Three, backwash clean complete after, apply the direct supply starter to the titanium target, sputtering power is 60W ~ 200W, control Ar airshed is 60sccm ~ 150sccm, make that gas pressure intensity is 0.1Pa ~ 2Pa in the vacuum storehouse, behind pre-sputter 3min ~ 5min, remove baffle plate, beginning is to substrate surface titanizing film 10min ~ 90min;
Four, deposited the titanium film after, close dc sputtering power, apply the negative voltage of 200V ~ 800V to the rotary heating platform, carry out backwash sputter 10min ~ 20min to Surface of Titanium Film;
Five, running target source, make the central position of carbon target face the center of substrate of glass, apply the radio-frequency power supply starter to the carbon target, radio frequency power is 60W ~ 200W, control Ar airshed is 30sccm ~ 70sccm, makes that gas pressure intensity is 0.1Pa ~ 2Pa in vacuum the storehouse in, in advance behind sputter 3min ~ 5min, remove baffle plate, beginning is to Surface of Titanium Film plating carbon film 60min ~ 180min;
Six, deposited the carbon film after, close radio-frequency power supply, apply the negative voltage of 200V ~ 800V to the rotary heating platform, carry out backwash sputter 10min ~ 20min to the carbon film surface;
Seven, after backwash is finished, cover substrate with baffle plate, close all power supplys, treat to make when temperature is down to 20 ℃ ~ 25 ℃ in the vacuum storehouse X ray reflection mirror superficial film.
Principle of work of the present invention: the Ar ion that utilizes magnetron sputtering itself to provide, bombard into membrane interface, so that unstable ion or defective and foreign ion are fled from the film growth surface, increase simultaneously the locomotivity of film forming atom, prepare Stability Analysis of Structures densification, smooth surface, interface roughness is little and interface high-quality rete clearly.
The present invention comprises following advantage:
1, become membrane interface owing to Ar ion bombardment in the preparation process, effectively improved the reflector interface roughness, interface roughness is 0.05nm ~ 0.15nm, and the rete density is high, and the rete interface is clear;
2, in the preparation process because Ar ion bombardment film surface, the speculum rete of preparing is high with the substrate bonding strength, sticking power is large, deposition is even;
3, the inventive method is at the multilayer film of glass basic surface preparation, and each thicknesses of layers is easy to control, can prepare as required the multilayer film of various Thickness Ratios to satisfy the Practical Project requirement;
4, the inventive method is compared with traditional magnetically controlled sputter method at the speculum of glass basic surface preparation, and reflectivity has improved 10% ~ 15%.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the method for a kind of X ray reflection mirror surface coating in the present embodiment is carried out according to the following steps:
One, substrate of glass is used acetone ultrasonic cleaning 15min ~ 30min, cleaned 15min ~ 30min with dehydrated alcohol again, use at last washed with de-ionized water 15min ~ 30min post-drying;
Two, substrate of glass is placed on the rotary heating platform in the magnetron sputtering vacuum storehouse, make the substrate center over against the center of titanium target, will be evacuated in the vacuum storehouse by vacuum acquiring system, vacuum tightness reaches 1.0 * 10 in the hole capital after selling all securities of taking seriously
-4Pa ~ 9.9 * 10
-4During Pa, start heating unit, be heated to 25 ℃ ~ 650 ℃, and insulation 10min ~ 120min; Pass into Ar gas, when pressure is 3Pa ~ 5Pa in the hole capital after selling all securities of taking seriously, apply the negative voltage of 200V ~ 800V to the rotary heating platform, substrate of glass is carried out backwash clean 10min ~ 20min;
Three, backwash clean complete after, apply the direct supply starter to the titanium target, sputtering power is 60W ~ 200W, control Ar airshed is 60sccm ~ 150sccm, make that gas pressure intensity is 0.1Pa ~ 2Pa in the vacuum storehouse, behind pre-sputter 3min ~ 5min, remove baffle plate, beginning is to substrate surface titanizing film 10min ~ 90min;
Four, deposited the titanium film after, close dc sputtering power, apply the negative voltage of 200V ~ 800V to the rotary heating platform, carry out backwash sputter 10min ~ 20min to Surface of Titanium Film;
Five, running target source, make the central position of carbon target face the center of substrate of glass, apply the radio-frequency power supply starter to the carbon target, radio frequency power is 60W ~ 200W, control Ar airshed is 30sccm ~ 70sccm, makes that gas pressure intensity is 0.1Pa ~ 2Pa in vacuum the storehouse in, in advance behind sputter 3min ~ 5min, remove baffle plate, beginning is to Surface of Titanium Film plating carbon film 60min ~ 180min;
Six, deposited the carbon film after, close radio-frequency power supply, apply the negative voltage of 200V ~ 800V to the rotary heating platform, carry out backwash sputter 10min ~ 20min to the carbon film surface;
Seven, after backwash is finished, cover substrate with baffle plate, close all power supplys, treat to make when temperature is down to 20 ℃ ~ 25 ℃ in the vacuum storehouse X ray reflection mirror superficial film.
Principle of work of the present invention: the Ar ion that utilizes magnetron sputtering itself to provide, bombard into membrane interface, so that unstable ion or defective and foreign ion are fled from the film growth surface, increase simultaneously the locomotivity of film forming atom, prepare Stability Analysis of Structures densification, smooth surface, interface roughness is little and interface high-quality rete clearly.
The present invention comprises following advantage:
1, become membrane interface owing to Ar ion bombardment in the preparation process, effectively improved the reflector interface roughness, interface roughness is 0.05nm ~ 0.15nm, and the rete density is high, and the rete interface is clear;
2, in the preparation process because Ar ion bombardment film surface, the speculum rete of preparing is high with the substrate bonding strength, sticking power is large, deposition is even;
3, the inventive method is at the multilayer film of glass basic surface preparation, and each thicknesses of layers is easy to control, can prepare as required the multilayer film of various Thickness Ratios to satisfy the Practical Project requirement;
4, the inventive method is compared with traditional magnetically controlled sputter method at the speculum of glass basic surface preparation, and reflectivity has improved 10% ~ 15%.
Embodiment two: present embodiment and embodiment one are different be in the step 1 with substrate of glass with acetone ultrasonic cleaning 20min ~ 25min, clean 20min ~ 25min with dehydrated alcohol again, use at last washed with de-ionized water 20min ~ 25min post-drying.Other step and parameter are identical with embodiment one.
Embodiment three: present embodiment and embodiment one are different be in the step 1 with substrate of glass with acetone ultrasonic cleaning 24min, clean 24min with dehydrated alcohol again, use at last washed with de-ionized water 24min post-drying.Other step and parameter are identical with embodiment one.
Embodiment four: present embodiment is different from one of embodiment one to three is to take seriously in the step 2 that vacuum tightness reaches 2.0 * 10 in the hole capital after selling all securities
-4Pa ~ 8.0 * 10
-4During Pa, start heating unit, be heated to 100 ℃ ~ 600 ℃, and insulation 30min ~ 90min.Other step and parameter are identical with one of embodiment one to three.
Embodiment five: present embodiment is different from one of embodiment one to three is to take seriously in the step 2 that vacuum tightness reaches 5.0 * 10 in the hole capital after selling all securities
-4During Pa, start heating unit, be heated to 300 ℃, and insulation 60min.Other step and parameter are identical with one of embodiment one to three.
Embodiment six: present embodiment is different from one of embodiment one to five is to take seriously in the hole capital after selling all securities pressure in the step 2 when being 3.5Pa ~ 4.5Pa, apply the negative voltage of 600V ~ 700V to the rotary heating platform, substrate of glass is carried out backwash clean 12min ~ 18min.Other step and parameter are identical with one of embodiment one to five.
Embodiment seven: present embodiment is different from one of embodiment one to five is to take seriously in the step 2 when pressure is 4Pa in the hole capital after selling all securities, applies the negative voltage of 650V to the rotary heating platform, substrate of glass is carried out backwash clean 15min.Other step and parameter are identical with one of embodiment one to five.
Embodiment eight: what present embodiment was different from one of embodiment one to seven is that control Ar airshed is 80sccm ~ 120sccm in the step 3, make that gas pressure intensity is 0.5Pa ~ 1.5Pa in the vacuum storehouse, behind pre-sputter 3.5min ~ 4.5min, remove baffle plate, beginning is to substrate surface titanizing film 25min ~ 75min.Other step and parameter are identical with one of embodiment one to seven.
Embodiment nine: what present embodiment was different from one of embodiment one to eight is the negative voltage that applies 300V ~ 700V in the step 4 to the rotary heating platform, carries out backwash sputter 12min ~ 18min to Surface of Titanium Film.Other step and parameter are identical with one of embodiment one to eight.
Embodiment ten: what present embodiment was different from one of embodiment one to nine is that control Ar airshed is 40sccm ~ 60sccm in the step 5, make that gas pressure intensity is 0.5Pa ~ 1.5Pa in the vacuum storehouse, behind pre-sputter 3.5min ~ 4.5min, remove baffle plate, beginning is to Surface of Titanium Film plating carbon film 90min ~ 150min.Other step and parameter are identical with one of embodiment one to nine.
Embodiment 11: what present embodiment was different from one of embodiment one to ten is the negative voltage that applies 300V ~ 700V in the step 6 to the rotary heating platform, carries out backwash sputter 12min ~ 18min to the carbon film surface.Other step and parameter are identical with one of embodiment one to ten.
In order to verify beneficial effect of the present invention, carried out following experiment:
Experiment one: a kind of method of X ray reflection mirror surface coating:
One, is the substrate of glass acetone ultrasonic cleaning 24min of 40mm * 40mm * 2mm with specification, cleans 24min with dehydrated alcohol again, use at last washed with de-ionized water 24min post-drying;
Two, substrate of glass is placed on the rotary heating platform in the magnetron sputtering vacuum storehouse, make the substrate center over against the center of titanium target, will be evacuated in the vacuum storehouse by vacuum acquiring system, vacuum tightness reaches 5.0 * 10 in the hole capital after selling all securities of taking seriously
-4During Pa, start heating unit, be heated to 300 ℃, and insulation 60min, pass into Ar gas, when pressure is 4Pa in the hole capital after selling all securities of taking seriously, apply the negative voltage of 650V to the rotary heating platform, substrate of glass is carried out backwash clean 15min;
Three, backwash clean complete after, apply the direct supply starter to the titanium target, sputtering power is 150W, control Ar airshed is 100sccm, makes that gas pressure intensity is 1Pa in vacuum the storehouse in, behind the pre-sputter 4min, removes baffle plate, begins to substrate surface titanizing film 60min;
Four, deposited the titanium film after, close dc sputtering power, apply the negative voltage of 650V to the rotary heating platform, carry out backwash sputter 15min to Surface of Titanium Film;
Five, deposited the titanium film after, cover substrate with baffle plate, close dc sputtering power, the running target source, make the central position of carbon target face the center of substrate of glass, apply the radio-frequency power supply starter to the carbon target, radio frequency power is 130W, and control Ar airshed is 50sccm, make that gas pressure intensity is 1Pa in the vacuum storehouse, behind the pre-sputter 4min, remove baffle plate, beginning is to Surface of Titanium Film plating carbon film 120min;
Six, deposited the carbon film after, close radio-frequency power supply, apply the negative voltage of 650V to the rotary heating platform, carry out backwash sputter 15min to the carbon film surface;
Seven, deposited the carbon film after, cover substrate with baffle plate, close all power supplys, treat to make when temperature is down to 24 ℃ in the vacuum storehouse X ray reflection mirror superficial film.
The X ray reflection mirror superficial film of preparation has in the experiment one: defective is few, large and the rete interface of density is advantage clearly, and film substrate bond strength is large, compare with traditional magnetically controlled sputter method, the interface roughness of X ray reflection mirror superficial film is reduced to 0.05nm ~ 0.15nm by 0.4nm ~ 0.55nm, and the reflectivity of X ray reflection mirror has improved 10% ~ 15%.
Claims (10)
1. the method for an X ray reflection mirror surface coating is characterized in that it realizes by following steps:
One, substrate of glass is used acetone ultrasonic cleaning 15min ~ 30min, cleaned 15min ~ 30min with dehydrated alcohol again, use at last washed with de-ionized water 15min ~ 30min post-drying;
Two, substrate of glass is placed on the rotary heating platform in the magnetron sputtering vacuum storehouse, make the substrate center over against the center of titanium target, will be evacuated in the vacuum storehouse by vacuum acquiring system, vacuum tightness reaches 1.0 * 10 in the hole capital after selling all securities of taking seriously
-4Pa ~ 9.9 * 10
-4During Pa, start heating unit, be heated to 25 ℃ ~ 650 ℃, and insulation 10min ~ 120min; Pass into Ar gas, when pressure is 3Pa ~ 5Pa in the hole capital after selling all securities of taking seriously, apply the negative voltage of 200V ~ 800V to the rotary heating platform, substrate of glass is carried out backwash clean 10min ~ 20min;
Three, backwash clean complete after, apply the direct supply starter to the titanium target, sputtering power is 60W ~ 200W, control Ar airshed is 60sccm ~ 150sccm, make that gas pressure intensity is 0.1Pa ~ 2Pa in the vacuum storehouse, behind pre-sputter 3min ~ 5min, remove baffle plate, beginning is to substrate surface titanizing film 10min ~ 90min;
Four, deposited the titanium film after, close dc sputtering power, apply the negative voltage of 200V ~ 800V to the rotary heating platform, carry out backwash sputter 10min ~ 20min to Surface of Titanium Film;
Five, running target source, make the central position of carbon target face the center of substrate of glass, apply the radio-frequency power supply starter to the carbon target, radio frequency power is 60W ~ 200W, control Ar airshed is 30sccm ~ 70sccm, makes that gas pressure intensity is 0.1Pa ~ 2Pa in vacuum the storehouse in, in advance behind sputter 3min ~ 5min, remove baffle plate, beginning is to Surface of Titanium Film plating carbon film 60min ~ 180min;
Six, deposited the carbon film after, close radio-frequency power supply, apply the negative voltage of 200V ~ 800V to the rotary heating platform, carry out backwash sputter 10min ~ 20min to the carbon film surface;
Seven, after backwash is finished, cover substrate with baffle plate, close all power supplys, treat to make when temperature is down to 20 ℃ ~ 25 ℃ in the vacuum storehouse X ray reflection mirror superficial film.
2. the method for a kind of X ray reflection mirror surface coating as claimed in claim 1, it is characterized in that in the step 1 substrate of glass usefulness acetone ultrasonic cleaning 20min ~ 25min, clean 20min ~ 25min with dehydrated alcohol again, use at last washed with de-ionized water 20min ~ 25min post-drying.
3. the method for a kind of X ray reflection mirror surface coating as claimed in claim 1 is characterized in that in the step 1 substrate of glass being used acetone ultrasonic cleaning 24min, cleans 24min with dehydrated alcohol again, uses at last washed with de-ionized water 24min post-drying.
4. such as the method for each described a kind of X ray reflection mirror surface coating in the claims 1 to 3, vacuum tightness reaches 2.0 * 10 in the hole capital after selling all securities that it is characterized in that taking seriously in the step 2
-4Pa ~ 8.0 * 10
-4During Pa, start heating unit, be heated to 100 ℃ ~ 600 ℃, and insulation 30min ~ 90min.
5. such as the method for each described a kind of X ray reflection mirror surface coating in the claims 1 to 3, vacuum tightness reaches 5.0 * 10 in the hole capital after selling all securities that it is characterized in that taking seriously in the step 2
-4During Pa, start heating unit, be heated to 300 ℃, and insulation 60min.
6. the method for a kind of X ray reflection mirror surface coating as claimed in claim 4, when the pressure that it is characterized in that in the step 2 taking seriously in the hole capital after selling all securities is 3.5Pa ~ 4.5Pa, apply the negative voltage of 600V ~ 700V to the rotary heating platform, substrate of glass is carried out backwash clean 12min ~ 18min.
7. the method for a kind of X ray reflection mirror surface coating as claimed in claim 4 when pressure is 4Pa in the hole capital after selling all securities that it is characterized in that taking seriously in the step 2, applies the negative voltage of 650V to the rotary heating platform, substrate of glass is carried out backwash clean 15min.
8. the method for a kind of X ray reflection mirror surface coating as claimed in claim 6, it is characterized in that control Ar airshed is 80sccm ~ 120sccm in the step 3, make that gas pressure intensity is 0.5Pa ~ 1.5Pa in the vacuum storehouse, behind pre-sputter 3.5min ~ 4.5min, remove baffle plate, beginning is to substrate surface titanizing film 25min ~ 75min.
9. the method for a kind of X ray reflection mirror surface coating as claimed in claim 6 is characterized in that applying to the rotary heating platform in the step 4 negative voltage of 300V ~ 700V carrying out backwash sputter 12min ~ 18min to Surface of Titanium Film.
10. the method for a kind of X ray reflection mirror surface coating as claimed in claim 8, it is characterized in that control Ar airshed is 40sccm ~ 60sccm in the step 5, make that gas pressure intensity is 0.5Pa ~ 1.5Pa in the vacuum storehouse, behind pre-sputter 3.5min ~ 4.5min, remove baffle plate, beginning is to Surface of Titanium Film plating carbon film 90min ~ 150min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105481262A (en) * | 2015-12-16 | 2016-04-13 | 中国科学院光电技术研究所 | Method for plating high-reflection film on surface of X-ray parabolic reflector |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101177779A (en) * | 2007-12-07 | 2008-05-14 | 哈尔滨工业大学 | Method for coating silicon film on surface of carborundum reflection mirror by employing magnetron sputtering |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101177779A (en) * | 2007-12-07 | 2008-05-14 | 哈尔滨工业大学 | Method for coating silicon film on surface of carborundum reflection mirror by employing magnetron sputtering |
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| Title |
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| HANS-JUERGEN STOCK,ET AL.: "Carbon/titanium multilayers as soft-x-ray mirrors for the water window", 《APPLIED OPTICS》 * |
| INOUE S,ET AL.: "Structure and mechanical properties of Ti/C multilayer films deposited by sputtering", 《JOURNAL OF THE JAPAN INSTITUTE OF METALS》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105481262A (en) * | 2015-12-16 | 2016-04-13 | 中国科学院光电技术研究所 | Method for plating high-reflection film on surface of X-ray parabolic reflector |
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