CN109851231A - A kind of antireflective, resisting laser damage glass and preparation method thereof - Google Patents
A kind of antireflective, resisting laser damage glass and preparation method thereof Download PDFInfo
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- CN109851231A CN109851231A CN201910069841.0A CN201910069841A CN109851231A CN 109851231 A CN109851231 A CN 109851231A CN 201910069841 A CN201910069841 A CN 201910069841A CN 109851231 A CN109851231 A CN 109851231A
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Abstract
The invention discloses a kind of antireflective, resisting laser damage glass and preparation method thereof, glass includes substrate, and the surface of substrate is equipped with composite film, and for composite film by sequentially including internal layer, middle layer and outer layer except interior, the internal layer is SiO2Layer, middle layer SiO2+ZrO2Layer, outer layer ZrO2Layer.The present invention can effectively improve the antireflective and resisting laser damage ability of glass.
Description
Technical field
The present invention relates to glass art more particularly to a kind of antireflectives, resisting laser damage glass and preparation method thereof.
Background technique
Thin film damage restricts laser system to be developed to high life, high power direction；The damage of film is mainly due to inhaling
Caused by the increase of stress caused by receiving and temperature increase, since optical film materials may include various impurity during the preparation process,
Defect, these impurity, defect have sizable absorption coefficient, and after impurity, defect absorb laser illumination energy, temperature is suddenly
It increases, so that impurity particle is melted or is gasified, very big local thermal stress is generated in impurity surrounding optical material, when the stress is super
When crossing the tensile strength of optical material, i.e., destruction, and the steam pressure that impurity vaporization generates are cracked in optical thin film
The degree of destruction can be increased.Optical thin film restricts all the time as the weak link for being easiest to be damaged in laser system
Laser system develop to high life, high power direction.Under light laser effect, optical module may be broken in a short time
It is bad.For a long time, laser is always to limit laser to develop to high power, high-energy direction to the destruction of optical pellicle
" bottleneck ", and the main reason for influence Laser Films component service life.Thus how to further increase optically thin
The resisting laser damage ability of film is pendulum urgent problem to be solved in face of thin film work person.In conjunction with damage from laser mechanism above-mentioned,
Optical film materials as light laser field, it is necessary to consider: to the transparency of incident light, scattered power, machinable durability, chemistry
The bulk properties such as stability and resisting laser damage ability.The resisting laser damage ability for how further increasing optical module, draws
Extensive concern and the further investigation of people are played.Meanwhile device of high power laser uses the preparation of optical coating to coating performance
Requirement it is harsher, complicated Film Design requires film same with favorable optical performance and resisting laser damage performance
When, the Stress match between film layer is also solved the problems, such as very well.
Summary of the invention
The purpose of the present invention is to provide a kind of film layer bond strengths big, antireflective, resisting laser damage glass and its preparation
Method.
To achieve the above object, the invention adopts the following technical scheme:
The surface of a kind of antireflective, resisting laser damage glass, including substrate, substrate is equipped with composite film, composite film
By sequentially including internal layer, middle layer and outer layer except interior, the internal layer is SiO2Layer, middle layer SiO2+ZrO2Layer, outer layer are
ZrO2Layer.
The SiO2Layer with a thickness of 30-50nm.
The SiO2+ZrO2Layer with a thickness of 20-30nm.
The ZrO2Layer with a thickness of 50-80nm.
The substrate with a thickness of 3-7mm.
Antireflective of the present invention, resisting laser damage glass preparation method the following steps are included:
1) substrate is surface-treated；
2) it prepares internal layer: substrate is sent into coating chamber, SiO is formed using radio frequency magnetron sputtering method2Layer, the temperature of substrate
It is 25-60 DEG C, back bias voltage 50-150V, operating air pressure 0.2-1Pa, substrate revolving speed 2-8rpm, silicon target electric current 2-4A, O2Flow 2-
6sccm, argon flow 5-25sccm, sputtering time 10-30min, radio-frequency power 100-200W, silicon target and substrate spacing
From for 30-60mm；
3) it prepares middle layer first layer: continuing rf magnetron sputtering and form SiO2+ZrO2Layer, wherein SiO2With ZrO2Matter
Measure ratio are as follows: 50wt%:50wt%；The temperature of substrate is 25-60 DEG C, back bias voltage 50-150V, operating air pressure 0.2-1Pa, and substrate turns
Fast 2-8rpm, silicon target electric current 2-4A, zirconium target current 2-4A, O2Flow 2-6sccm, argon flow 5-25sccm, sputtering time
For 10-30min, radio-frequency power 100-200W, silicon target, zirconium target and base distance between plates are 30-60mm；
4) it prepares the middle layer second layer: continuing rf magnetron sputtering and form SiO2+ZrO2Layer, wherein SiO2With ZrO2Matter
Measure ratio are as follows: 70wt%:30wt%；The temperature of substrate is 25-60 DEG C, back bias voltage 50-150V, operating air pressure 0.2-1Pa, and substrate turns
Fast 2-8rpm, silicon target electric current 6-8A, zirconium target current 2-3A, O2Flow 2-6sccm, argon flow 5-25sccm, sputtering time
For 10-30min, radio-frequency power 100-200W, silicon target, zirconium target and base distance between plates are 30-60mm；
5) it prepares outer layer: continuing rf magnetron sputtering and form ZrO2Layer, the temperature of substrate are 25-60 DEG C, back bias voltage 50-
150V, operating air pressure 0.2-1Pa, substrate revolving speed 2-8rpm, zirconium target current 2-4A, O2Flow 2-6sccm, argon flow 5-
25sccm, sputtering time 10-30min, radio-frequency power 100-200W, zirconium target and base distance between plates are 30-60mm.
The step of substrate is surface-treated in step 1): substrate is successively ultrasonic respectively in deionized water, ethyl alcohol
30min is cleaned, then with being dried with nitrogen.
The invention adopts the above technical scheme has following technical effect that
1, silica (SiO2) layer has refractive index low, and there is chemical property to stablize, and film adhesion is strong, energy and substrate
Surface generates the features such as good combination, while being ideal reflection-reducing material, has high rejection rate in infrared light district, visible
The transmitance of light Qu Yougao；Zirconium dioxide (ZrO2) layer is with materials with high melting point, higher dielectric constant and refractive index, simultaneously also
There are good mechanical performance and chemical inertness, it is low in the visible absorption near infrared region, there is high threshold for resisting laser damage, from
And effectively improve the antireflective and resisting laser damage ability of glass.
2, there is silicon dioxide layer, silica/titanium dioxide zirconium layer in middle layer and outer layer, titanium dioxide zirconium layer has hardness
The ability of high, strong resisting laser damage and the transparent range of very wide spectrum；Therefore, titanium dioxide zirconium layer can make glass surface have
There is the energy function of splendid antireflective and resisting laser damage.
3, there is identical ingredient to carry out asymptotic transition zone between two neighboring film layer, promote stress in thin film relaxation and effectively mention
Bond strength between high adjacent film layers.
Detailed description of the invention
The present invention is described in further details below in conjunction with the drawings and specific embodiments:
Fig. 1 is the structural diagram of the present invention.
Specific embodiment
As shown in Figure 1, a kind of antireflective of the present invention, resisting laser damage glass, including substrate 1, the surface of substrate 1 are equipped with
Composite film, for composite film by sequentially including internal layer 2, middle layer 3 and outer layer 4 except interior, the internal layer 2 is SiO2Layer, it is intermediate
Layer 3 is SiO2+ZrO2Layer, outer layer 4 are ZrO2Layer.
Wherein, substrate with a thickness of 3-7mm, SiO2Layer with a thickness of 30-50nm, SiO2+ZrO2Layer with a thickness of 20-
30nm, ZrO2
Layer with a thickness of 50-80nm.
Embodiment 1: antireflective of the present invention, resisting laser damage glass preparation method the following steps are included:
1) substrate is surface-treated: substrate is successively cleaned by ultrasonic 30min respectively in deionized water, ethyl alcohol, so
Afterwards with being dried with nitrogen；
2) it prepares internal layer: substrate is sent into coating chamber, SiO is formed using radio frequency magnetron sputtering method2Layer, the temperature of substrate
It is 25 DEG C, back bias voltage 50V, operating air pressure 0.2Pa, substrate revolving speed 2rpm, silicon target electric current 2A, O2Flow 2sccm, argon flow are
5sccm, sputtering time 10min, radio-frequency power 100W, silicon target and base distance between plates are 30mm；
3) it prepares middle layer first layer: continuing rf magnetron sputtering and form SiO2+ZrO2Layer, wherein SiO2With ZrO2Matter
Measure ratio are as follows: 50wt%:50wt%；The temperature of substrate is 25 DEG C, back bias voltage 50V, operating air pressure 0.2Pa, substrate revolving speed 2rpm, silicon
Target current 2A, zirconium target current 2A, O2Flow 2sccm, argon flow 5sccm, sputtering time 10min, radio-frequency power are
100W, silicon target, zirconium target and base distance between plates are 30mm；
4) it prepares the middle layer second layer: continuing rf magnetron sputtering and form SiO2+ZrO2Layer, wherein SiO2With ZrO2Matter
Measure ratio are as follows: 70wt%:30wt%；The temperature of substrate is 25 DEG C, back bias voltage 50V, operating air pressure 0.2Pa, substrate revolving speed 2rpm, silicon
Target current 6A, zirconium target current 2A, O2Flow 2sccm, argon flow 5sccm, sputtering time 10min, radio-frequency power are
100W, silicon target, zirconium target and base distance between plates are 30mm；
5) it prepares outer layer: continuing rf magnetron sputtering and form ZrO2Layer, the temperature of substrate are 25 DEG C, back bias voltage 50V, work
Air pressure 0.2Pa, substrate revolving speed 2rpm, zirconium target current 2A, O2Flow 2sccm, argon flow 5sccm, sputtering time are
10min, radio-frequency power 100W, zirconium target and base distance between plates are 30mm.
Embodiment 2: antireflective of the present invention, resisting laser damage glass preparation method the following steps are included:
1) substrate is surface-treated: substrate is successively cleaned by ultrasonic 30min respectively in deionized water, ethyl alcohol, so
Afterwards with being dried with nitrogen；
2) it prepares internal layer: substrate is sent into coating chamber, SiO is formed using radio frequency magnetron sputtering method2Layer, the temperature of substrate
It is 60 DEG C, back bias voltage 150V, operating air pressure 1Pa, substrate revolving speed 8rpm, silicon target electric current 4A, O2Flow 6sccm, argon flow are
25sccm, sputtering time 30min, radio-frequency power 200W, silicon target and base distance between plates are 60mm；
3) it prepares middle layer first layer: continuing rf magnetron sputtering and form SiO2+ZrO2Layer, wherein SiO2With ZrO2Matter
Measure ratio are as follows: 50wt%:50wt%；The temperature of substrate is 60 DEG C, back bias voltage 150V, operating air pressure 1Pa, substrate revolving speed 8rpm, silicon
Target current 4A, zirconium target current 4A, O2Flow 6sccm, argon flow 25sccm, sputtering time 30min, radio-frequency power are
200W, silicon target, zirconium target and base distance between plates are 60mm；
4) it prepares the middle layer second layer: continuing rf magnetron sputtering and form SiO2+ZrO2Layer, wherein SiO2With ZrO2Matter
Measure ratio are as follows: 70wt%:30wt%；The temperature of substrate is 60 DEG C, back bias voltage 150V, operating air pressure 1Pa, substrate revolving speed 8rpm, silicon
Target current 8A, zirconium target current 3A, O2Flow 6sccm, argon flow 25sccm, sputtering time 30min, radio-frequency power are
200W, silicon target, zirconium target and base distance between plates are 60mm；
5) it prepares outer layer: continuing rf magnetron sputtering and form ZrO2Layer, the temperature of substrate are 60 DEG C, back bias voltage 150V, work
Make air pressure 1Pa, substrate revolving speed 8rpm, zirconium target current 4A, O2Flow 6sccm, argon flow 25sccm, sputtering time are
30min, radio-frequency power 200W, zirconium target and base distance between plates are 60mm.
Embodiment 3: antireflective of the present invention, resisting laser damage glass preparation method the following steps are included:
1) substrate is surface-treated: substrate is successively cleaned by ultrasonic 30min respectively in deionized water, ethyl alcohol, so
Afterwards with being dried with nitrogen；
2) it prepares internal layer: substrate is sent into coating chamber, SiO is formed using radio frequency magnetron sputtering method2Layer, the temperature of substrate
It is 45 DEG C, back bias voltage 100V, operating air pressure 0.6Pa, substrate revolving speed 5rpm, silicon target electric current 3A, O2Flow 4sccm, argon flow
For 15sccm, sputtering time 20min, radio-frequency power 150W, silicon target and base distance between plates are 45mm；
3) it prepares middle layer first layer: continuing rf magnetron sputtering and form SiO2+ZrO2Layer, wherein SiO2With ZrO2Matter
Measure ratio are as follows: 50wt%:50wt%；The temperature of substrate is 45 DEG C, back bias voltage 100V, operating air pressure 0.6Pa, substrate revolving speed 5rpm,
Silicon target electric current 3A, zirconium target current 3A, O2Flow 4sccm, argon flow 15sccm, sputtering time 20min, radio-frequency power are
150W, silicon target, zirconium target and base distance between plates are 45mm；
4) it prepares the middle layer second layer: continuing rf magnetron sputtering and form SiO2+ZrO2Layer, wherein SiO2With ZrO2Matter
Measure ratio are as follows: 70wt%:30wt%；The temperature of substrate is 45 DEG C, back bias voltage 100V, operating air pressure 0.6Pa, substrate revolving speed 5rpm,
Silicon target electric current 7A, zirconium target current 2.5A, O2Flow 4sccm, argon flow 15sccm, sputtering time 20min, radio-frequency power
For 150W, silicon target, zirconium target and base distance between plates are 45mm；
5) it prepares outer layer: continuing rf magnetron sputtering and form ZrO2Layer, the temperature of substrate are 45 DEG C, back bias voltage 100V, work
Make air pressure 0.6Pa, substrate revolving speed 5rpm, zirconium target current 3A, O2Flow 4sccm, argon flow 15sccm, sputtering time are
20min, radio-frequency power 150W, zirconium target and base distance between plates are 45mm.
In order to verify film layer made from preparation method of the present invention, film layer in the various embodiments described above is tested for the property, it can
Know, the progressive film layer preparation of multilayer of the present invention and existing conventional monolayers ZrO2Film is to compare, progress technique, ultraviolet light transmittance,
Infrared reflectivity measurement, micro-structure, the detection of heat-insulated film plating layer, adhesion test and square resistance the result is as follows:
Claims (7)
1. a kind of antireflective, resisting laser damage glass, including substrate, the surface of substrate is equipped with composite film, composite film by
It sequentially include internal layer, middle layer and outer layer except interior, the internal layer is SiO2Layer, middle layer SiO2+ZrO2Layer, outer layer are
ZrO2Layer.
2. a kind of antireflective according to claim 1, resisting laser damage glass, it is characterised in that: the SiO2The thickness of layer
For 30-50nm.
3. a kind of antireflective according to claim 1, resisting laser damage glass, it is characterised in that: the SiO2+ZrO2Layer
With a thickness of 20-30nm.
4. a kind of antireflective according to claim 1, resisting laser damage glass, it is characterised in that: the ZrO2The thickness of layer
For 50-80nm.
5. a kind of antireflective according to claim 1, resisting laser damage glass, it is characterised in that: the thickness of the substrate
For 3-7mm.
6. the preparation method of glass according to claim 1, it is characterised in that: the preparation method comprises the following steps:
1) substrate is surface-treated；
2) it prepares internal layer: substrate is sent into coating chamber, SiO is formed using radio frequency magnetron sputtering method2Layer, the temperature of substrate are 25-
60 DEG C, back bias voltage 50-150V, operating air pressure 0.2-1Pa, substrate revolving speed 2-8rpm, silicon target electric current 2-4A, O2Flow 2-6sccm,
Argon flow is 5-25sccm, sputtering time 10-30min, radio-frequency power 100-200W, and silicon target is with base distance between plates
30-60mm；
3) it prepares middle layer first layer: continuing rf magnetron sputtering and form SiO2+ZrO2Layer, wherein SiO2With ZrO2Mass ratio
Are as follows: 50wt%:50wt%；The temperature of substrate is 25-60 DEG C, back bias voltage 50-150V, operating air pressure 0.2-1Pa, substrate revolving speed 2-
8rpm, silicon target electric current 2-4A, zirconium target current 2-4A, O2Flow 2-6sccm, argon flow 5-25sccm, sputtering time 10-
30min, radio-frequency power 100-200W, silicon target, zirconium target and base distance between plates are 30-60mm；
4) it prepares the middle layer second layer: continuing rf magnetron sputtering and form SiO2+ZrO2Layer, wherein SiO2With ZrO2Mass ratio
Are as follows: 70wt%:30wt%；The temperature of substrate is 25-60 DEG C, back bias voltage 50-150V, operating air pressure 0.2-1Pa, substrate revolving speed 2-
8rpm, silicon target electric current 6-8A, zirconium target current 2-3A, O2Flow 2-6sccm, argon flow 5-25sccm, sputtering time 10-
30min, radio-frequency power 100-200W, silicon target, zirconium target and base distance between plates are 30-60mm；
5) it prepares outer layer: continuing rf magnetron sputtering and form ZrO2Layer, the temperature of substrate are 25-60 DEG C, back bias voltage 50-150V, work
Make air pressure 0.2-1Pa, substrate revolving speed 2-8rpm, zirconium target current 2-4A, O2Flow 2-6sccm, argon flow 5-25sccm, splashes
Penetrating the time is 10-30min, and radio-frequency power 100-200W, zirconium target and base distance between plates are 30-60mm.
7. preparation method according to claim 6, it is characterised in that: the step being surface-treated in step 1) to substrate
It is rapid: substrate to be successively cleaned by ultrasonic 30min respectively in deionized water, ethyl alcohol, then with being dried with nitrogen.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112779535A (en) * | 2020-12-07 | 2021-05-11 | 上海航天设备制造总厂有限公司 | Laser ablation resistant coating for substrate surface and preparation method thereof |
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