CN107870162A - The method for improving optical element damage threshold under nanosecond frequency tripled laser irradiation - Google Patents
The method for improving optical element damage threshold under nanosecond frequency tripled laser irradiation Download PDFInfo
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- CN107870162A CN107870162A CN201711061321.2A CN201711061321A CN107870162A CN 107870162 A CN107870162 A CN 107870162A CN 201711061321 A CN201711061321 A CN 201711061321A CN 107870162 A CN107870162 A CN 107870162A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/55—Specular reflectivity
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/59—Transmissivity
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/55—Specular reflectivity
- G01N2021/558—Measuring reflectivity and transmission
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Abstract
The invention provides a kind of method for improving optical element damage threshold under nanosecond frequency tripled laser irradiation, belong to laser material technical field.Method provided by the invention is by reducing optical element to a certain optimum temperature so that the damage threshold of optical element is maximum at such a temperature, in combination with hydrofluoric acid chemistry etch techniques, finally realizes effective lifting of optic element damage threshold value.This method effectively increases optical element optic element damage threshold value under nanosecond frequency tripled laser irradiation, and the resisting laser damage ability of optical element this problem important in inhibiting how is improved for solution.
Description
Technical field
The invention belongs to laser material technical field, and in particular to one kind improves optical element in nanosecond frequency tripled laser spoke
According to the method for lower damage threshold.
Background technology
Device of high power laser is widely used in the fields such as new energy, new material, national defense industry and basic physicses research,
But the damage of optical element is " bottleneck " problem that device of high power laser power output is further lifted all the time.Fused quartz and K9
Optical glass extensively and is largely used in device of high power laser because it has excellent optics, machinery and processing characteristics.
Therefore, the research to its strong laser induced damage is increasingly becoming focus and emphasis.
The research influenceed at present on temperature on the lower optic element damage threshold value of nanosecond frequency tripled laser irradiation, more only
Scattered report：
Document " Influence of ambient temperature on nanosecond and picosecond
Laser-induced bulk damage of fused silica " have studied the fused quartz under nanosecond frequency tripled laser irradiation
Damage threshold contrast in 295K and 80K.As a result show the damage threshold in the fused quartz at a temperature of 80K than being lifted during normal temperature
About 8%, but this article only have studied the damage threshold under two kinds of different temperatures of 295K and 80K, and temperature effect can not be illustrated to swashing
The affecting laws of luminescent material damage threshold, and the lifting when fused quartz damage threshold is compared to normal temperature at a temperature of low temperature 80K
Very little.
Document " research of the temperature effect to material properties influence under Irradiation of High " have studied in nanosecond frequency tripled laser
Damage threshold contrast of the lower fused quartz of irradiation in 296K and 220K.Result of study shows the damage of the fused quartz at a temperature of 220K
Lifting about 10% when hindering threshold value than normal temperature.Similar with the studies above, this article only have studied two kinds of different temperatures of 296K and 220K
Under damage threshold, affecting laws of the temperature effect to laser material damage threshold can not be illustrated, and melted at a temperature of 220K
Lifting when quartz damage threshold value is compared to normal temperature also unobvious.
Document " Temperature dependence of laser-induced damage threshold in
Silica glass " to nanosecond frequency tripled laser irradiation under quartz glass laser damage threshold temperature dependency is ground
Study carefully, but because it tests the limitation of temperature range, the research think the damage threshold of laser material with the reduction of temperature and
Improve constantly, do not find a critical-temperature be present so that laser material reaches damage threshold lifting most at such a temperature
Big value.
This experimental method by system experimental studies have found that temperature effect to the lower optics of nanosecond frequency tripled laser irradiation
The affecting laws of element damage threshold value, concurrent existing in a specific temperature, optical element is being received under this specified temp
Damage threshold lifting amplitude under second frequency tripled laser irradiation is maximum.
The content of the invention
The purpose of the present invention is to overcome the technical problem of above-mentioned prior art, there is provided one kind improves optical element in nanosecond three
The method of the lower damage threshold of double-frequency laser irradiation.
Technical problem proposed by the invention so solves：
A kind of method for improving optical element damage threshold under nanosecond frequency tripled laser irradiation, comprises the following steps：
Step 1：Pretreatment is carried out to laboratory sample and prepares laboratory sample；
The pretreatment mode has following three kinds：
Processing mode 1：Acid etch is not carried out to laboratory sample, specific operation process is as follows：Laboratory sample is used first
High purity water is rinsed, and is then reused absolute alcohol and is carried out dewater treatment；
Processing mode 2：Static acid etch, specific operation process are as follows：Laboratory sample is rushed using high purity water first
Wash, then laboratory sample is put into etching solution and stands 10 minutes progress chemical etchings；
Wherein, etching solution is buffered hydrofluoric acid solution, and its configuration quality fraction is respectively 1% hydrogen fluoride and 15% fluorine
Change ammonium, etching reuses high purity water flushing sample after finishing taking-up, removes sample surfaces residual buffer solution, finally use no watery wine
Progress greatly row dewater treatment；
Processing mode 3：Dynamic acid etch (AMP), specific operation process is as follows：Laboratory sample is sprayed using high purity water first
Leaching cleaning；Laboratory sample is positioned in weak lye again and is cleaned by ultrasonic using 40-270kHz ultrasonic assistants, removes surface
Pollutant；Then take out and be cleaned by ultrasonic under 40-270kHz ultrasonic assistants using high purity water, remove remained on surface alkali
Liquid；Secondly laboratory sample is positioned in etching solution and carries out mega sonic wave auxiliary etch 20 minutes；Finally carried out using high purity water
Ultrasonic cleaning and cleaning showers, sample surfaces residual acid solution is removed, and be statically placed in clean environment and spontaneously dry；
Wherein, etching solution is buffered hydrofluoric acid solution, and its configuration quality fraction is respectively 2.4% hydrogen fluoride and 12%
Ammonium fluoride, megasonic frequency 1.3MHz, and etching solution temperature control is maintained at 26-28 DEG C in etching process.
Step 2：The specimen holder laboratory sample prepared in step 1 being put into vacuum chamber；Vacuum chamber connects vavuum pump
And low-temperature control system.
Step 3：Nd：YAG laser launches main laser, and main laser is divided into transmission and reflection two-beam after spectroscope；Instead
Penetrate light to be received by bulk absorption, for measuring laser energy value in real time；Irradiated after transmitted light line focus lens focus in experiment sample
After product on surface；He-Ne lasers produce detection light, detection light by after the window glass of chopper and vacuum chamber with main laser
Transmitted light coincided with the rear surface of laboratory sample a bit, detect light caused by reflected light popped one's head in by window glass by energy
Receive, the signal popped one's head in by lock-in amplifier, chopper and energy realizes the real-time monitoring of laser -induced damage.
Step 4：The energy value of ascending regulation main laser, irradiates the same point in laboratory sample in a manner of pulse
On, the reading of lock-in amplifier, the judgment basis damaged using the unexpected reduction of reading as laboratory sample are observed, and record
Each main laser energy value.
According to international standard ISO11254, this method uses N-on-1 methods.N-on-1 measuring methods refer to ascending
Increasing action in the pulsed laser energy in the same test point of element, until it is damaged, and between the time acted on every time
Every can not fix.
The beneficial effects of the invention are as follows：
The present invention can effectively improve damage threshold of the optical element under nanosecond frequency tripled laser irradiation, so as to certain
How solved in degree makes device of high power laser output further lift this problem.
Brief description of the drawings
Fig. 1 is experiment light path schematic diagram；
Fig. 2 is fused quartz LIDT-T graphs of a relation, wherein the static acid etches (c) of (a) AMP (b) are without acid etch；
Fig. 3 is K9 glass LIDT-T graphs of a relation, wherein (a) static acid etch (b) is without acid etch；
Fig. 4 is the not chemically treated sample damage threshold comparison figure with being handled under optimum temperature through acid etch under normal temperature,
Wherein (a) fused quartz (b) K9 glass, LIDT represent Laser-induced damage threshold, unit：J/cm2。
Embodiment
The present invention is further detailed with reference to embodiment and accompanying drawing.
The laboratory sample that the present embodiment uses is respectively the model of fused quartz glass and K9 glass, wherein fused quartz glass
JGS1 far ultraviolet optical quartz glasses, all samples specification are 30mm × 30mm × 4mm.As shown in figure 1, experimental facilities is main
Including：Nd：YAG laser, model Beamtech SGR-20 Nd：YAG, output energy are 500mJ@355nm；Low temperature is set
It is standby, including vacuum cavity and low-temperature control system；Bulk absorption, for real-time monitored laser irradiation energy；Damaging judge system
System, mainly include He-Ne lasers, lock-in amplifier, chopper and energy probe；Vavuum pump, condenser lens and light splitting
Mirror；Two-dimensional movement platform and stepping machine controller, for moving laboratory sample and regulation condenser lens.
In the present embodiment, the focal length of condenser lens is 165mm；Main laser uses parameter as wavelength 355nm, pulsewidth 6ns
Nanosecond frequency tripled laser；
Step 1：Following three kinds of modes are taken to enter respectively using the laboratory sample of identical processing technology production same batch
Row pretreatment：
Processing mode 1：Acid etch is not carried out to laboratory sample, specific operation process is as follows：Laboratory sample is used first
High purity water is rinsed, and is then reused absolute alcohol and is carried out dewater treatment；
Processing mode 2：Static acid etch, specific operation process are as follows：Laboratory sample is rushed using high purity water first
Wash, then laboratory sample is put into etching solution and stands 10 minutes progress chemical etchings；
Wherein, etching solution is buffered hydrofluoric acid solution, and its configuration quality fraction is respectively 1% hydrogen fluoride and 15% fluorine
Change ammonium, etching reuses high purity water flushing sample after finishing taking-up, removes sample surfaces residual buffer solution, finally use no watery wine
Progress greatly row dewater treatment；
Processing mode 3：Dynamic acid etch, specific operation process are as follows：It is first that laboratory sample is clear using high-purity Water spray
Wash；Laboratory sample is positioned in weak lye again and is cleaned by ultrasonic using 40-270kHz ultrasonic assistants, removes the dirt on surface
Contaminate thing；Then take out and be cleaned by ultrasonic under 40-270kHz ultrasonic assistants using high purity water, remove remained on surface alkali lye；
Secondly laboratory sample is positioned in etching solution and carries out mega sonic wave auxiliary etch 20 minutes；Finally ultrasound is carried out using high purity water
Cleaning and cleaning showers, sample surfaces residual acid solution is removed, and be statically placed in clean environment and spontaneously dry；
Wherein, etching solution is buffered hydrofluoric acid solution, and its configuration quality fraction is respectively 2.4% hydrogen fluoride and 12%
Ammonium fluoride, megasonic frequency 1.3MHz, and etching solution temperature control is maintained at 26-28 DEG C in etching process.
Step 2：The specimen holder laboratory sample prepared in step 1 being put into vacuum chamber；Vacuum chamber connects vavuum pump
And low-temperature control system；
Vacuum measurement level is 10torr in the vacuum chamber that the present embodiment uses.
Step 3：Nd：YAG laser launches main laser, and main laser is divided into transmission and reflection two-beam after spectroscope；Instead
Penetrate light to be received by bulk absorption, for measuring laser energy value in real time；Irradiated after transmitted light line focus lens focus in experiment sample
After product on surface；He-Ne lasers produce detection light, detection light by after the window glass of chopper and vacuum chamber with main laser
Transmitted light coincided with a bit on the rear surface of laboratory sample, its caused reflected light by window glass by energy probe connect
Receive, the signal popped one's head in by lock-in amplifier, chopper and energy realizes the real-time monitoring of laser -induced damage.
Step 4：The energy value of ascending regulation main laser, irradiates the same point in laboratory sample in a manner of pulse
On, the reading of lock-in amplifier, the judgment basis damaged using the unexpected reduction of reading as laboratory sample are observed, and record
Each main laser energy value；The 1% unexpected reduction for being determined as reading is more than with reading change.
Because laser has energy hunting in itself, each energy irradiation repeats three hairs, often between hair time between the time
Every more than 5 seconds.By the equidistant mobile example of stepper, spacing is 2mm between each test point in this experiment.Complete normal temperature
Under (296K) test after cooled by temperature control system, be down to experiment design temperature after keep a period of time after, carry out
The measurement of laser damage threshold.This experiment in, fused quartz sample experiments design temperature be respectively 296K, 266K, 236K,
206K, 176K, 146K, 116K and 86K, K9 glass experiment design temperature be respectively 296K, 254K, 212K, 170K, 128K and
86K, laser facula 0.08mm.
Measured respectively in this experiment under the irradiation of nanosecond frequency tripling (355nm@6ns) laser after different pretreatments
Fused quartz (JGS1) glass (being pre-processed without acid treatment, static acid etch and dynamic acid etch (AMP)) and K9 glass are (without acid
Etching and the pretreatment of static acid etch) rear surface laser induced damage threshold value at different temperatures.
The experimental results are shown inthe following table for fused quartz (JGS1) glass：
The experimental results are shown inthe following table for K9 glass：
After handling above-mentioned fused quartz (JGS1) glass and K9 glass experimental results, nanosecond frequency tripled laser spoke is obtained
According to lower fused quartz (JGS1) glass (being pre-processed without acid treatment, static acid etch and dynamic acid etch (AMP)) and K9 glass is (not
Pre-processed through acid etch and static acid etch) damage threshold and temperature relation, as shown in Figures 2 and 3.It is pre- through three kinds of differences
Rear surface damage threshold value of fused quartz (JGS1) glass under nanosecond frequency tripled laser irradiation after processing is equal with the reduction of temperature
Show the trend of first increases and then decreases, damage threshold lifting is maximum when near 170K, and with it is carried out before experiment it is pre-
Processing mode is unrelated.During compared to normal temperature (296K), its damage threshold improve respectively 21.12% (dynamic acid etch),
19.03% (static acid etch) and 12.22% (no acid etch), maximum lift amplitude is during compared with without acid etch normal temperature (296K)
66.06%.K9 glass after two kinds of different pretreatments under nanosecond frequency tripled laser irradiation after surface damage threshold value with temperature
The reduction of degree equally shows the trend of first increases and then decreases, is when the lifting of its damage threshold is maximum unlike fused quartz
It is unrelated with the pretreatment mode carried out before experiment to it near 212K, and equally.During compared to normal temperature (296K), its damage threshold
Value improves 24.36% (static acid etch) and 20.27% (no acid etch) respectively, during compared with without acid etch normal temperature (296K) most
Big lifting amplitude is 31.08%.For not chemical through handling (institute of the present invention through acid etch under processing and optimum temperature under normal temperature
State method) fused quartz (a) and K9 glass (b) damage threshold contrast, as shown in Figure 4.
Claims (8)
1. improve the method for optical element damage threshold under nanosecond frequency tripled laser irradiation, it is characterised in that including following step
Suddenly：
Step 1：Pretreatment is carried out to laboratory sample and prepares laboratory sample；
Step 2：The specimen holder laboratory sample prepared in step 1 being put into vacuum chamber；Vacuum chamber connects vavuum pump and low
Temperature control system；
Step 3：Nd：YAG laser launches main laser, and main laser is divided into transmission and reflection two-beam after spectroscope；Reflected light
Received by bulk absorption, for measuring laser energy value in real time；Irradiated after transmitted light line focus lens focus after laboratory sample
On surface；He-Ne lasers produce detection light, and detection light passes through saturating with main laser after the window glass of chopper and vacuum chamber
Penetrate light to coincide with the rear surface of laboratory sample a bit, detect reflected light caused by light and connect by window glass by energy probe
Receive, the signal popped one's head in by lock-in amplifier, chopper and energy realizes the real-time monitoring of laser -induced damage；
Step 4：The energy value of ascending regulation main laser, is irradiated in a manner of pulse in the same point of laboratory sample,
The reading of lock-in amplifier, the judgment basis damaged using the unexpected reduction of reading as laboratory sample are observed, and is recorded every
Secondary main laser energy value.
2. the method according to claim 1 for improving optical element damage threshold under nanosecond frequency tripled laser irradiation, its
It is characterised by, the pretreatment mode is：
Processing mode 1：Acid etch is not carried out to laboratory sample, specific operation process is as follows：Laboratory sample is used first high-purity
Water is rinsed, and is then reused absolute alcohol and is carried out dewater treatment.
3. the method according to claim 1 for improving optical element damage threshold under nanosecond frequency tripled laser irradiation, its
It is characterised by, the pretreatment mode is：
Processing mode 2：Static acid etch, specific operation process are as follows：Laboratory sample is rinsed using high purity water first, so
Laboratory sample is put into etching solution afterwards and stands 10 minutes progress chemical etchings；Etching reuses high purity water punching after finishing taking-up
Sample is washed, sample surfaces residual buffer solution is removed, finally carries out dewater treatment using absolute alcohol.
4. the method according to claim 1 for improving optical element damage threshold under nanosecond frequency tripled laser irradiation, its
It is characterised by, the pretreatment mode is：
Processing mode 3：Dynamic acid etch, specific operation process are as follows：Laboratory sample is used into high purity water cleaning showers first；Again
Laboratory sample is positioned in weak lye and is cleaned by ultrasonic using 40-270kHz ultrasonic assistants, removes the pollutant on surface；
Then take out and be cleaned by ultrasonic under 40-270kHz ultrasonic assistants using high purity water, remove remained on surface alkali lye；Secondly will
Laboratory sample, which is positioned in etching solution, carries out mega sonic wave auxiliary etch 20 minutes；Finally using high purity water carry out be cleaned by ultrasonic and
Cleaning showers, sample surfaces residual acid solution is removed, and be statically placed in clean environment and spontaneously dry.
5. the method according to claim 3 for improving optical element damage threshold under nanosecond frequency tripled laser irradiation, its
It is characterised by, the etching solution is buffered hydrofluoric acid solution, and its configuration quality fraction is respectively 1% hydrogen fluoride and 15% fluorine
Change ammonium.
6. the method according to claim 4 for improving optical element damage threshold under nanosecond frequency tripled laser irradiation, its
It is characterised by, the etching solution is buffered hydrofluoric acid solution, and its configuration quality fraction is respectively 2.4% hydrogen fluoride and 12%
Ammonium fluoride, megasonic frequency 1.3MHz, and etching solution temperature control is maintained at 26-28 DEG C in etching process.
7. the method according to claim 1 for improving optical element damage threshold under nanosecond frequency tripled laser irradiation, its
It is characterised by, the laboratory sample is fused quartz glass and K9 glass.
8. the method according to claim 7 for improving optical element damage threshold under nanosecond frequency tripled laser irradiation, its
It is characterised by, fused quartz glass experiment design temperature is respectively 296K, 266K, 236K, 206K, 176K, 146K, 116K and 86K,
K9 glass experiment design temperature is respectively 296K, 254K, 212K, 170K, 128K and 86K.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109115684A (en) * | 2018-09-07 | 2019-01-01 | 中国工程物理研究院激光聚变研究中心 | For determining the measurement method and measuring system of laser pre-treated energy level |
| CN110161038A (en) * | 2019-05-05 | 2019-08-23 | 长春理工大学 | A kind of test method for monitoring the damage from laser moment on-line |
| CN110161039A (en) * | 2019-05-05 | 2019-08-23 | 长春理工大学 | A kind of high power continuous laser damage threshold automatic testing equipment |
| CN110161042A (en) * | 2019-05-05 | 2019-08-23 | 长春理工大学 | A kind of high peak power pulse laser damage threshold automatic test approach |
| CN110161040A (en) * | 2019-05-05 | 2019-08-23 | 长春理工大学 | A kind of method of automatic test high power continuous laser damage threshold |
| CN110161037A (en) * | 2019-05-05 | 2019-08-23 | 长春理工大学 | A kind of high peak power pulse laser damage threshold automatic testing equipment |
| CN110161041A (en) * | 2019-05-05 | 2019-08-23 | 长春理工大学 | A kind of test device for monitoring the damage from laser moment on-line |
| CN112266179A (en) * | 2020-10-22 | 2021-01-26 | 中国科学院上海光学精密机械研究所 | Method for processing high damage threshold ultra-smooth surface of fused quartz glass |
| CN113484246A (en) * | 2021-07-06 | 2021-10-08 | 南开大学 | High-energy laser damage vacuum experiment system capable of measuring damage threshold |
| CN114974467A (en) * | 2022-03-02 | 2022-08-30 | 电子科技大学长三角研究院(湖州) | Method for evaluating laser damage threshold of fused quartz amorphous structure model by different oxygen-silicon ratios |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109115684A (en) * | 2018-09-07 | 2019-01-01 | 中国工程物理研究院激光聚变研究中心 | For determining the measurement method and measuring system of laser pre-treated energy level |
| CN110161038A (en) * | 2019-05-05 | 2019-08-23 | 长春理工大学 | A kind of test method for monitoring the damage from laser moment on-line |
| CN110161039A (en) * | 2019-05-05 | 2019-08-23 | 长春理工大学 | A kind of high power continuous laser damage threshold automatic testing equipment |
| CN110161042A (en) * | 2019-05-05 | 2019-08-23 | 长春理工大学 | A kind of high peak power pulse laser damage threshold automatic test approach |
| CN110161040A (en) * | 2019-05-05 | 2019-08-23 | 长春理工大学 | A kind of method of automatic test high power continuous laser damage threshold |
| CN110161037A (en) * | 2019-05-05 | 2019-08-23 | 长春理工大学 | A kind of high peak power pulse laser damage threshold automatic testing equipment |
| CN110161041A (en) * | 2019-05-05 | 2019-08-23 | 长春理工大学 | A kind of test device for monitoring the damage from laser moment on-line |
| CN112266179A (en) * | 2020-10-22 | 2021-01-26 | 中国科学院上海光学精密机械研究所 | Method for processing high damage threshold ultra-smooth surface of fused quartz glass |
| CN113484246A (en) * | 2021-07-06 | 2021-10-08 | 南开大学 | High-energy laser damage vacuum experiment system capable of measuring damage threshold |
| CN114974467A (en) * | 2022-03-02 | 2022-08-30 | 电子科技大学长三角研究院(湖州) | Method for evaluating laser damage threshold of fused quartz amorphous structure model by different oxygen-silicon ratios |
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