CN108863093A - A method of control fused quartz static state acid etching deposit - Google Patents
A method of control fused quartz static state acid etching deposit Download PDFInfo
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- CN108863093A CN108863093A CN201810798186.8A CN201810798186A CN108863093A CN 108863093 A CN108863093 A CN 108863093A CN 201810798186 A CN201810798186 A CN 201810798186A CN 108863093 A CN108863093 A CN 108863093A
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- fused quartz
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
- C03C15/02—Surface treatment of glass, not in the form of fibres or filaments, by etching for making a smooth surface
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
Abstract
The invention discloses a kind of methods for controlling fused quartz static state acid etching deposit, this method is spread using the concentration of short time acid etching process hexafluorosilicic acid root, fused quartz element is carried out spray after acid etching and removing residual ion is removed in ultrasonic cleaning, acid etching, spray, ultrasonic this process of rinsing are repeated several times again, realize the etching of the fused quartz of certain depth, not only avoid the appearance of deposit, maintain face shape, and improve laser damage threshold, it realizes fused quartz polishing layer and defect layer effectively completely removes, and deposit-free generates；This method have many advantages, such as it is easy to operate, controllable, do not destroy optical component surface shape and roughness, be economical.
Description
Technical field
The invention belongs to optical materials and optical element technology field, specifically disclose a kind of control fused quartz static state acid etching
The method for carving deposit.
Background technique
Fused quartz transmissive element opposite shape index and the laser damage threshold tool that large-scale high power solid-state laser device uses
There is very high requirement.The fused quartz element that traditional processing mode obtains includes polishing layer impurity, embedded pollutant, subsurface defect
(containing micro-crack, hole point etc.), in order to improve laser damage threshold, it is necessary to remove these impurity and defect, current most effective hand
Section is to be etched using the solution of hydrofluoric acid containing to element.The solution of acid etching mainly has two kinds, and it is molten that one is hydrofluoric acid
Liquid, another kind are containing NH4The hydrofluoric acid buffer solution (BHF) of F, also referred to as BOE solution.Because the latter's etch-rate is very steady
Fixed, fused quartz surface etches more smooth compared to pure hydrofluoric acid solution after etching, and the hydrofluoric acid buffering with same etch-rate is molten
HF content is low in liquid (meaning less volatility and toxicity), so usually selecting the latter in fused quartz etching process.But
It is in etching process due to NH4 +Cations are high, and precipitating (deposition is generated easily in conjunction with reaction product hexafluorosilicic acid radical ion
Object), cause fused quartz element surface face shape to be destroyed and fused quartz element threshold for resisting laser damage is greatly lowered.
The fused quartz element of traditional processing typically at least needs to etch a few micrometers, subsurface defect density could be reduced
To certain degree.The deposit that long-time Static Etch generates will lead to threshold value decline.It is generated to reduce etching for a long time
Deposit, being proved to effective method at present is to introduce ultrasonic wave or mega sonic wave during the reaction.Inside hydrofluoric acid
Using mega sonic wave/ultrasonic wave, there are following technical problems：1) etching solution temperature rise effect bring caused by sound field etches
Unevenly, 2) the hydrofluoric acid corrosion resistance ability of vibration plate coating material, the 3) circulating filtration in cleaning reaction process, 4) mega sonic wave produces
The problems such as raw stationary field, interference, turbulent flow, makes local etching is too fast face shape deterioration either regional area is caused to transport too slow lead
The requirement of optical index is not achieved in the deposition for causing deposit, the element after causing the increasing substantially and etch of cost.Do not surpass
The etching of sound and million sound, i.e. Static Etch, short time etching opposite shape does not influence, but prolonged etching will cause threshold value
Decline and surface deposits must generate, as shown in Figure 1.So key is to be accurately controlled to etching process,
Under the premise of can guarantee element etch depth, the generation of surface deposits is reduced.
Summary of the invention
It is excellent it is an object of the invention to solve at least the above problems and/or defect, and provide at least to will be described later
Point.
The present invention proposes a kind of static acid etching cooperation ultrasound of multiple short time (accumulation etching period, etch certain depth)
High-purity water cleaning method avoids deposit from generating, and increases substantially the ability of fused quartz element resisting laser damage, reduces surface erosion
The holding of the inhomogeneities and face shape at quarter can be directed to bigbore optical element.
In order to realize these purposes and other advantages according to the present invention, a kind of control fused quartz static state acid etching is provided
The method of deposit, includes the following steps：
Step 1: fused quartz is put into buffered hydrofluoric acid etching liquid, temperature is 23 ± 1 DEG C, and the single reactive ion etching time is small
In 20min, 1.5 μm/h-2 μm/h of mean etch rate；
Step 2: the fused quartz after step 1 is etched carries out high purity water spray rinsing, spray pressure is not less than 0.2Mpa,
Temperature is 30 ± 2 DEG C, flow 120L/min, and the time is not less than 10min, removes the extra acid solution on surface and a large amount of
SiF6 2-；
Step 3: the fused quartz after step 2 is rinsed, which is put into the groove body equipped with high purity water, carries out ultrasonic rinsing, temperature
It is 35 DEG C, ultrasonic power density is not less than 5W/L, and 220KHz is cleaned by ultrasonic 15min or more, and 270KHz cleans 15min or more, always
Meter ultrasonic cleaning is not less than 30 minutes, further removes SiF6 2-Ion；
Step 4: the fused quartz after step 3 is rinsed is put into the groove body equipped with high purity water, temperature is 55 ± 2 DEG C, is surpassed
Acoustic frequency is 270KHz, and ultrasonic power density is not less than 5W/L, lifts at a slow speed, removes the extra water of optical element surface；
Step 5: fused quartz is rotated clockwise 90 °, ultrasonic cleaning groove body is drained and is rejoined high purity water simultaneously
It is heated to corresponding temperature；
Step 6: repeating step 1 to step 5, and each etching period is identical in step 1, and etching number is 4
It is one group that multiple, i.e. fused quartz, which etch 4 times, is at least etched 1 time；Tired etch depth is etched at 4 μm or more until meeting.
Preferably, the resistivity of the high purity water>15MΩ.cm.
Preferably, the pull rate lifted at a slow speed in the step 4 is 1mm/s.
Preferably, the mass fraction of hydrofluoric acid is 0.8-1.2%, NH in the buffered hydrofluoric acid etching liquid4F and
NH4C2H4NH4F2Mass fraction 8-12%.
Preferably, in the step 1, the reactive ion etching time is 15min；1.8 μm/h of mean etch rate.
Preferably, in the step 2, spray pressure is 0.5~1.5Mpa；Time is 15min.
Preferably, in the step 3, ultrasonic power density is 10W/L, and 220KHz is cleaned by ultrasonic 20min, 270KHz
Clean 20min；In the step 4, ultrasonic power density 10W/L.
Preferably, in the step 1, a nanometer gas is passed through into buffered hydrofluoric acid etching liquid during reactive ion etching
Bubble；The nano bubble is any one or the combination of several of them in oxygen, ozone, nitrogen, argon gas or carbon dioxide；It is described to receive
The diameter of rice bubble is 0.1~100um；The Ventilation Rate of the nano bubble is 50~100mL/min.
It preferably, further include following procedure before the step 1：Fused quartz is put into supercritical device, in temperature
5min~10min is impregnated in the supercritical acetone-water system that degree is 350 DEG C~370 DEG C and pressure is 8MPa~14MPa；It is described
Supercritical acetone-water system in the volume ratio of acetone and water be 5:1.
Preferably, further include after being impregnated in supercritical acetone-water system：By fused quartz be sent into atmos low-temperature etc. from
In daughter device, fused quartz is set to be in 50~100mm at the jet exit of atmos low-temperature plasma, and spray fused quartz
Exit rotation, rotation speed are 30~60r/min；According to the air-flow of 5~15L/h in atmos low-temperature plasma device
Amount is passed through gas, applies operating voltage, forms plasma jet, controls the jet exit of atmos low-temperature plasma device
Movement speed in 5~10mm/s, make plasma jet injection on the fused quartz of rotation, to fused quartz processing 5~
10min；The operating voltage is provided using high-voltage ac power, and the operating voltage is the alternating voltage of 35~100kV, frequency
For 100~300kHz；The gas is the mixing of one or more of air, rare gas/oxygen, oxygen, nitrogen.
The present invention is include at least the following beneficial effects：The present invention utilizes the diffusion of acid etching process hexafluorosilicic acid root, one
Fix time it is interior fused quartz element is carried out spray and removing residual ion is removed in ultrasonic cleaning, then this process is repeated several times, realizes certain
The etching of the fused quartz of depth not only avoids the appearance of deposit, maintains face shape, and improve laser damage threshold；It is real
Showed the effectively complete removal of fused quartz polishing layer and defect layer, and deposit-free generates, this method have it is easy to operate, economical,
It can control, not destroy the advantages that optical component surface shape and roughness.
Further advantage, target and feature of the invention will be partially reflected by the following instructions, and part will also be by this
The research and practice of invention and be understood by the person skilled in the art.
Detailed description of the invention：
Fig. 1 is short time the dynamic of the invention repeatedly etch period of acid etching and the relational graph (wavelength of laser damage threshold
355nm, pulsewidth 3ns)；
Fig. 2 is the photo in kind of the fused quartz of the multiple acid etching of short time dynamic of the invention；
Fig. 3 is the dark field photo of the fused quartz of the static state acid etching for a long time of comparative example 1；
Fig. 4 is the atomic force microscopy of the fused quartz of the static state acid etching for a long time of comparative example 1；
Fig. 5 is that single acid etching process reaction product ion concentration changes schematic diagram；
Fig. 6 is that spray rinsing process reaction product ion concentration changes schematic diagram；
Fig. 7 is that ultrasonic rinse cycle reaction product ions concentration changes schematic diagram.
Specific embodiment：
Present invention will be described in further detail below with reference to the accompanying drawings, to enable those skilled in the art referring to specification text
Word can be implemented accordingly.
It should be appreciated that such as " having ", "comprising" and " comprising " term used herein do not allot one or more
The presence or addition of a other elements or combinations thereof.
Embodiment 1：
A method of control fused quartz static state acid etching deposit includes the following steps：
Step 1: 50mm × 50mm × 5mm fused quartz is put into buffered hydrofluoric acid etching liquid, temperature is 23 DEG C, single
The reactive ion etching time is 15min, 1.5 μm/h of mean etch rate；
Step 2: the fused quartz after step 1 is etched carries out high purity water spray rinsing, spray pressure 0.5Mpa, temperature is
30 DEG C, flow 120L/min, time 15min, remove surface extra acid solution and a large amount of SiF6 2-；
Step 3: the fused quartz after step 2 is rinsed, which is put into the groove body equipped with high purity water, carries out ultrasonic rinsing, temperature
It is 35 DEG C, ultrasonic power density 10W/L, 220KHz are cleaned by ultrasonic 20min, and 270KHz cleans 20min, further removes SiF6 2-
Ion；
Step 4: the fused quartz after step 3 is rinsed is put into the groove body equipped with high purity water, temperature is 55 DEG C, supersonic frequency
Rate is 270KHz, and the speed of ultrasonic power density 10W/L, 1mm/s lift at a slow speed, removes the extra water of optical element surface；
Step 5: fused quartz is rotated clockwise 90 °, ultrasonic cleaning groove body is drained and is rejoined high purity water simultaneously
It is heated to corresponding temperature；
Step 6: repeating step 1 to step 5, and each etching period is identical in step 1, and etching number is 4
It is for 4 times one group that multiple, i.e. fused quartz, which etch, and (completing step 1 to step 4 is to etch for 1 time, then rotates clockwise 90 ° of progress
Etch next time, complete to be etched to 1 group 4 times), 1 group is etched, is reduced since depth difference leads to the uneven bring pair of diffusion
The influence of face shape；It is 4 μm until meeting the tired etch depth of etching；
The resistivity of the high purity water>15MΩ.cm；The mass fraction of hydrofluoric acid is in the buffered hydrofluoric acid etching liquid
0.8%, NH4F and NH4C2H4NH4F2Mass fraction 8%.
Embodiment 2：
A method of control fused quartz static state acid etching deposit includes the following steps：
Step 1: 50mm × 50mm × 5mm fused quartz is put into buffered hydrofluoric acid etching liquid, temperature is 24 DEG C, single
The reactive ion etching time is 20min, 2 μm/h of mean etch rate；
Step 2: the fused quartz after step 1 is etched carries out high purity water spray rinsing, spray pressure 0.6Mpa, temperature is
32 DEG C, flow 120L/min, time 20min, remove surface extra acid solution and a large amount of SiF6 2-；
Step 3: the fused quartz after step 2 is rinsed, which is put into the groove body equipped with high purity water, carries out ultrasonic rinsing, temperature
It is 35 DEG C, ultrasonic power density 10W/L, 220KHz are cleaned by ultrasonic 25min, and 270KHz cleans 25min, further removes SiF6 2-
Ion；
Step 4: the fused quartz after step 3 is rinsed is put into the groove body equipped with high purity water, temperature is 55 DEG C, supersonic frequency
Rate is 270KHz, and the speed of ultrasonic power density 12W/L, 1mm/s lift at a slow speed, removes the extra water of optical element surface；
Step 5: fused quartz is rotated clockwise 90 °, ultrasonic cleaning groove body is drained and is rejoined high purity water simultaneously
It is heated to corresponding temperature；
Step 6: repeating step 1 to step 5, and each etching period is identical in step 1, and etching number is 4
It is one group that multiple, i.e. fused quartz, which etch 4 times, etches 2 groups, is reduced since depth difference leads to the uneven bring opposite of diffusion
The influence of shape；It is 5 μm until meeting the tired etch depth of etching；
The resistivity of the high purity water>15MΩ.cm；The mass fraction of hydrofluoric acid is in the buffered hydrofluoric acid etching liquid
1.2%, NH4F and NH4C2H4NH4F2Mass fraction 12%.
Embodiment 3：
A method of control fused quartz static state acid etching deposit includes the following steps：
Step 1: 430mm × 430mm × 20mm fused quartz is put into buffered hydrofluoric acid etching liquid, temperature is 24 DEG C, single
Secondary response etch period is 20min, 1.8 μm/h of mean etch rate；
Step 2: the fused quartz after step 1 is etched carries out high purity water spray rinsing, spray pressure 0.6Mpa, temperature is
32 DEG C, flow 120L/min, time 18min, remove surface extra acid solution and a large amount of SiF6 2-；
Step 3: the fused quartz after step 2 is rinsed, which is put into the groove body equipped with high purity water, carries out ultrasonic rinsing, temperature
It is 35 DEG C, ultrasonic power density 12W/L, 220KHz are cleaned by ultrasonic 25min, and 270KHz cleans 20min, further removes SiF6 2-
Ion；
Step 4: the fused quartz after step 3 is rinsed is put into the groove body equipped with high purity water, temperature is 57 DEG C, supersonic frequency
Rate is 270KHz, and the speed of ultrasonic power density 12W/L, 1mm/s lift at a slow speed, removes the extra water of optical element surface；
Step 5: fused quartz is rotated clockwise 90 °, ultrasonic cleaning groove body is drained and is rejoined high purity water simultaneously
It is heated to corresponding temperature；
Step 6: repeating step 1 to step 5, and each etching period is identical in step 1, and etching number is 4
It is for 4 times one group that multiple, i.e. fused quartz, which etch, and (completing step 1 to step 4 is to etch for 1 time, then rotates clockwise 90 ° of progress
Etch next time, complete to be etched to 1 group 4 times), 1 group is etched, is reduced since depth difference leads to the uneven bring pair of diffusion
The influence of face shape；It is 4 μm until meeting the tired etch depth of etching；
By treated, fused quartz passes through 351nm wavelength laser, pulse width 5ns, clear field 1150cm2, average logical
Measure 5.97J/cm2, 50 hair of examination is amounted to, 5 impaired locis occurs in surface, wherein 3 d>120um damage, 2 50um damages.
The face deformation for etching front and back and degree of impairment are as described in Fig. 5 and table 1.
The resistivity of the high purity water>15MΩ.cm；The mass fraction of hydrofluoric acid is in the buffered hydrofluoric acid etching liquid
1%, NH4F and NH4C2H4NH4F2Mass fraction 10%.
Embodiment 4：
In the step 1, nano bubble is passed through into buffered hydrofluoric acid etching liquid during reactive ion etching；It is described to receive
Rice bubble is oxygen；The diameter of the nano bubble is 0.1um；The Ventilation Rate of the nano bubble is 50mL/min.Using
Effective complete removal of fused quartz polishing layer and defect layer is furthermore achieved in the process, further decreases fused quartz after etching
Surface roughness.
Remaining technological parameter and process with it is identical in embodiment 1.
Embodiment 5：
In the step 1, nano bubble is passed through into buffered hydrofluoric acid etching liquid during reactive ion etching；It is described to receive
Rice bubble is ozone；The diameter of the nano bubble is 0.2um；The Ventilation Rate of the nano bubble is 80mL/min.
Remaining technological parameter and process with it is identical in embodiment 3.
Embodiment 6：
It further include following procedure before the step 1：Fused quartz is put into supercritical device, is 360 DEG C in temperature
With pressure be 12MPa supercritical acetone-water system in impregnate 10min；Acetone and water in the supercritical acetone-water system
Volume ratio be 5:1.Using the treatment process, the pretreatment to fused quartz is realized, eliminates the fault of construction of fused quartz, into one
Step reduces the surface roughness of fused quartz after etching.
Remaining technological parameter and process with it is identical in embodiment 1.
Embodiment 7：
It further include following procedure before the step 1：Fused quartz is put into supercritical device, is 360 DEG C in temperature
With pressure be 12MPa supercritical acetone-water system in impregnate 10min；Acetone and water in the supercritical acetone-water system
Volume ratio be 5:1.
Remaining technological parameter and process with it is identical in embodiment 3.
Embodiment 8：
Further include after being impregnated in supercritical acetone-water system：Fused quartz is sent into atmos low-temperature plasma device
In, so that fused quartz is in 100mm at the jet exit of atmos low-temperature plasma, and make to rotate at fused quartz jet exit,
Rotation speed is 60r/min；Throughput in atmos low-temperature plasma device according to 15L/h is passed through gas, applies work
Make voltage, form plasma jet, controls the movement speed of the jet exit of atmos low-temperature plasma device in 10mm/
S makes plasma jet injection on the fused quartz of rotation, handles 5min to fused quartz；The operating voltage is handed over using high pressure
Galvanic electricity source provides, and the operating voltage is the alternating voltage of 100kV, frequency 200kHz；The gas is air and ammonia
Mixing；Using the process, the pretreatment to fused quartz is realized, eliminates the fault of construction of fused quartz, molten stone is furthermore achieved
Effective complete removal of English polishing layer and defect layer further decreases the surface roughness of fused quartz after etching.
Remaining technological parameter and process with it is identical in embodiment 6.
Embodiment 9：
Further include after being impregnated in supercritical acetone-water system：Fused quartz is sent into atmos low-temperature plasma device
In, so that fused quartz is in 50mm at the jet exit of atmos low-temperature plasma, and make to rotate at fused quartz jet exit, rotation
Rotary speed is 45r/min；Throughput in atmos low-temperature plasma device according to 12L/h is passed through gas, applies work
Voltage forms plasma jet, controls the movement speed of the jet exit of atmos low-temperature plasma device in 10mm/s,
Make plasma jet injection on the fused quartz of rotation, 8min is handled to fused quartz；The operating voltage uses high-voltage alternating
Power supply provides, and the operating voltage is the alternating voltage of 85kV, frequency 150kHz；The gas is the mixed of oxygen and ammonia
It closes.
Remaining technological parameter and process with it is identical in embodiment 7.
Embodiment 10：
In the step 1, nano bubble is passed through into buffered hydrofluoric acid etching liquid during reactive ion etching；It is described to receive
Rice bubble is ozone；The diameter of the nano bubble is 0.2um；The Ventilation Rate of the nano bubble is 80mL/min.
Remaining technological parameter and process with it is identical in embodiment 9.
Comparative example 1：
Step 1: 50mm × 50mm × 5mm fused quartz is put into buffered hydrofluoric acid etching liquid, temperature is 23 DEG C, reaction
Etch period is 60min, 1.5 μm/h of mean etch rate；It is 4 μm until meeting the tired etch depth of etching；
Step 2: the fused quartz after step 1 is etched carries out high purity water spray rinsing, spray pressure 0.5Mpa, temperature is
30 DEG C, flow 120L/min, time 60min, remove surface extra acid solution and a large amount of SiF6 2-；
Step 3: the fused quartz after step 2 is rinsed, which is put into the groove body equipped with high purity water, carries out ultrasonic rinsing, temperature
It is 35 DEG C, ultrasonic power density 10W/L, 220KHz are cleaned by ultrasonic 80min, and 270KHz cleans 80min, further removes SiF6 2-
Ion；
Step 4: the fused quartz after step 3 is rinsed is put into the groove body equipped with high purity water, temperature is 55 DEG C, supersonic frequency
Rate is 270KHz, and the speed of ultrasonic power density 10W/L, 1mm/s lift at a slow speed, removes the extra water of optical element surface.
The resistivity of the high purity water>15MΩ.cm；The mass fraction of hydrofluoric acid is in the buffered hydrofluoric acid etching liquid
1.2%, NH4F and NH4C2H4NH4F2Mass fraction 12%.
Embodiment 1 is compared with comparative example 1, and the single etch of (1 etching, 60min) will cause face for a long time in comparative example 1
The deterioration of shape and surface deposits generate (as shown in Fig. 3 optical photograph and Fig. 4 atomic force microscopy) so as to cause swashing
The decline of light injury threshold, but the 1 single etch time of embodiment is used not only to improve laser deflection for 4 etchings of 15min
Value, and reduce the deterioration of face shape, and the deposit on control surface, as shown in Fig. 1~2；Wherein, it will be seen from figure 1 that etching
The threshold for resisting laser damage of preceding fused quartz is 12J/cm2, it usually needs removal subsurface defect layer depth be at least 2 μm (
This etch-rate process needs at least 60min, and processing quality is poorer, and etch depth can accordingly increase), it can be seen that with etching
Up-trend is integrally presented in the increase threshold value of time, but if single acid etching time is too long, as shown in the figure from 105min to
135min, from 135min to 165min, single acid etching time 30min will lead to the decline of laser damage threshold, according to multiple
Experiment, determines that single acid etching time no more than 20min, otherwise will lead to the decline of laser damage threshold.
Fig. 5 is that single acid etching process reaction product ion concentration changes schematic diagram；With the carry out reaction product of etching
Ion concentration gradually increases；
Fig. 6 is that spray rinsing process reaction product ion concentration changes schematic diagram；Reaction production is carried out with spray rinsing
Object ion concentration is gradually reduced；
Fig. 7 is that ultrasonic rinse cycle reaction product ions concentration changes schematic diagram；Reaction production is carried out with ultrasound rinsing
Object ion concentration is gradually reduced.
Wherein, table 1 shows the index of correlation in Examples 1 to 10 after fused quartz etching；Before fused quartz etching：PV (λ=
632.8nm) it is 0.674；Surface roughness Rq (nm) (face A) is 0.604；Surface roughness Rq (nm) (face B) is 0.598；
Table 1
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed
With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily
Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited
In specific details and legend shown and described herein.
Claims (10)
1. a kind of method for controlling fused quartz static state acid etching deposit, which is characterized in that include the following steps：
Step 1: fused quartz is put into buffered hydrofluoric acid etching liquid, temperature is 23 ± 1 DEG C, and the single reactive ion etching time is less than
20min, 1.5 μm/h-2 μm/h of mean etch rate；
Step 2: the fused quartz after step 1 is etched carries out high purity water spray rinsing, spray pressure is not less than 0.2Mpa, temperature
Be 30 ± 2 DEG C, flow 120L/min, the time be not less than 10min, remove surface extra acid solution and a large amount of SiF6 2-；
Step 3: the fused quartz after step 2 is rinsed, which is put into the groove body equipped with high purity water, carries out ultrasonic rinsing, temperature 35
DEG C, ultrasonic power density is not less than 5W/L, and 220KHz is cleaned by ultrasonic 15min or more, and 270KHz cleans 15min or more, amounts to super
Sound cleaning is not less than 30 minutes, further removes SiF6 2-Ion；
Step 4: the fused quartz after step 3 is rinsed is put into the groove body equipped with high purity water, temperature is 55 ± 2 DEG C, supersonic frequency
Rate is 270KHz, and ultrasonic power density is not less than 5W/L, lifts at a slow speed, removes the extra water of optical element surface；
Step 5: fused quartz is rotated clockwise 90 °, ultrasonic cleaning groove body is drained and is rejoined high purity water and heated
To corresponding temperature；
Step 6: repeating step 1 to step 5, and each etching period is identical in step 1, and the multiple that number is 4 is etched,
It is one group that i.e. fused quartz, which etches 4 times, is at least etched 1 time；Tired etch depth is etched at 4 μm or more until meeting.
2. the method for control fused quartz static state acid etching deposit as described in claim 1, which is characterized in that the high purity water
Resistivity>15MΩ.cm.
3. the method for control fused quartz static state acid etching deposit as described in claim 1, which is characterized in that the step 4
In the pull rate lifted at a slow speed be 1mm/s.
4. the method for control fused quartz static state acid etching deposit as described in claim 1, which is characterized in that the buffering hydrogen
The mass fraction of hydrofluoric acid is 0.8-1.2%, NH in fluoric acid etching liquid4F and NH4C2H4NH4F2Mass fraction 8-12%.
5. the method for control fused quartz static state acid etching deposit as described in claim 1, which is characterized in that the step 1
In, the reactive ion etching time is 15min；1.8 μm/h of mean etch rate.
6. the method for control fused quartz static state acid etching deposit as described in claim 1, which is characterized in that the step 2
In, spray pressure is 0.5~1.5Mpa；Time is 15min.
7. the method for control fused quartz static state acid etching deposit as described in claim 1, which is characterized in that the step 3
In, ultrasonic power density is 10W/L, and 220KHz is cleaned by ultrasonic 20min, and 270KHz cleans 20min；In the step 4, ultrasound
Power density 10W/L.
8. the method for control fused quartz static state acid etching deposit as described in claim 1, which is characterized in that the step 1
In, nano bubble is passed through into buffered hydrofluoric acid etching liquid during reactive ion etching；The nano bubble be oxygen, ozone,
Any one or the combination of several of them in nitrogen, argon gas or carbon dioxide；The diameter of the nano bubble is 0.1~100um；Institute
The Ventilation Rate for stating nano bubble is 50~100mL/min.
9. the method for control fused quartz static state acid etching deposit as described in claim 1, which is characterized in that in the step
It further include following procedure before one：Fused quartz is put into supercritical device, in temperature be 350 DEG C~370 DEG C and pressure is
5min~10min is impregnated in the supercritical acetone-water system of 8MPa~14MPa；Acetone in the supercritical acetone-water system
Volume ratio with water is 5:1.
10. the method for control fused quartz static state acid etching deposit as claimed in claim 9, which is characterized in that overcritical
Further include after being impregnated in acetone-water system：Fused quartz is sent into atmos low-temperature plasma device, fused quartz is made to be in big
50~100mm at the jet exit of air pressure low temperature plasma, and make at fused quartz jet exit rotate, rotation speed be 30~
60r/min；Throughput in atmos low-temperature plasma device according to 5~15L/h is passed through gas, applies operating voltage,
Plasma jet is formed, the movement speed of the jet exit of atmos low-temperature plasma device is controlled in 5~10mm/s, makes
Plasma jet injection handles 5~10min to fused quartz on the fused quartz of rotation；The operating voltage is handed over using high pressure
Galvanic electricity source provides, and the operating voltage is the alternating voltage of 35~100kV, and frequency is 100~300kHz；The gas is sky
The mixing of one or more of gas, rare gas/oxygen, oxygen, nitrogen.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810798186.8A CN108863093B (en) | 2018-07-19 | 2018-07-19 | Method for controlling fused quartz static acid etching sediment |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810798186.8A CN108863093B (en) | 2018-07-19 | 2018-07-19 | Method for controlling fused quartz static acid etching sediment |
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| CN113248121A (en) * | 2021-06-18 | 2021-08-13 | 中国工程物理研究院激光聚变研究中心 | Post-processing method for improving damage threshold of fused quartz component |
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| US20030213428A1 (en) * | 2002-05-15 | 2003-11-20 | Rutgers, The State University Of New Jersey | Zinc oxide nanotip and fabricating method thereof |
| CN103449731A (en) * | 2013-09-06 | 2013-12-18 | 中国工程物理研究院激光聚变研究中心 | Method for improving damage threshold of fused quartz optical element |
| CN103922601A (en) * | 2014-03-18 | 2014-07-16 | 电子科技大学 | Surface treatment method for increasing fused silica element threshold value through wet etching-dry etching combination |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030213428A1 (en) * | 2002-05-15 | 2003-11-20 | Rutgers, The State University Of New Jersey | Zinc oxide nanotip and fabricating method thereof |
| CN103449731A (en) * | 2013-09-06 | 2013-12-18 | 中国工程物理研究院激光聚变研究中心 | Method for improving damage threshold of fused quartz optical element |
| CN103922601A (en) * | 2014-03-18 | 2014-07-16 | 电子科技大学 | Surface treatment method for increasing fused silica element threshold value through wet etching-dry etching combination |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113248121A (en) * | 2021-06-18 | 2021-08-13 | 中国工程物理研究院激光聚变研究中心 | Post-processing method for improving damage threshold of fused quartz component |
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