CN105127142B - A kind of laser film element super-smooth surface fused quartz optical substrate ultrasonic cleaning method - Google Patents
A kind of laser film element super-smooth surface fused quartz optical substrate ultrasonic cleaning method Download PDFInfo
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- CN105127142B CN105127142B CN201510585073.6A CN201510585073A CN105127142B CN 105127142 B CN105127142 B CN 105127142B CN 201510585073 A CN201510585073 A CN 201510585073A CN 105127142 B CN105127142 B CN 105127142B
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- ultrasonic
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- optical substrate
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
- B08B3/12—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B11/00—Cleaning flexible or delicate articles by methods or apparatus specially adapted thereto
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- Cleaning By Liquid Or Steam (AREA)
- Cleaning Or Drying Semiconductors (AREA)
Abstract
The present invention relates to a kind of laser film element super-smooth surface fused quartz optical substrate method for suppersonic cleaning, belong to optical technical field.The cleaning method is comprised the following steps：Before formal ultrasonic cleaning, minimum ultrasonic power, optimal ultrasonic time of the low-frequency range 80KHz supersonic frequencies to the effective removal of micrometer size granule are obtained with the substrate experiment of 1 μm ~ 3 μm artificial oxidation's silicon beads of spin coating；The optimal proportion of ammoniacal liquor, hydrogen peroxide and pure water, optimal ultrasonic time is obtained with reference to AFM when obtaining Mid Frequency 400KHz supersonic frequencies using the substrate experiment of 0.3 μm~1 μm artificial oxidation's silicon bead of spin coating；After two aspects of summary obtain optimal ultrasonic cleaning parameter, implementation carries out ultrasonic wave and finely cleans to ultra-smooth fused quartz optical substrate.The advantage of the invention is that realizing ultrasonic cleaning efficient to fused quartz optical substrate, quantitative by methods described, ultrasonic wave is avoided while realizing that substrate high-cleanness, high is cleaned and excessively cleans the super-smooth surface damage and fatigue of materials caused to base component.
Description
Technical field
Used the present invention relates to the ultrasonic cleaning method before a kind of fused quartz optical substrate plated film, particularly laser film element
Super-smooth surface fused quartz optical substrate ultrasonic cleaning method.
Background technology
Laser film is the key element in high power laser system, be realize system optics performance key factor it
One, optical thin film element is again the weak link of most easy damaged in laser system, and base-plate cleaning is used as Laser Films system
Standby primary operation directly determines the final resisting laser damage ability of element.Substrate surface pollutant after general polishing is mainly wrapped
Include organic contamination, soluble contaminant, solid particle pollution etc..Organic contamination can be removed by the cleaning agent immersion way commonly used
And soluble contaminant, and the solid grain contamination of substrate surface is then difficult to remove completely, and the yardstick covering of these particulates is from receiving
Rice is stronger to absorption affinity between micrometer range, with substrate, plethora defect is formed during follow-up thin-film-coating, as element
The induction source of damage from laser, therefore optical substrate needs effectively cleaned for residual particulates before plated film.
Conventional cleaning method has wipe method, RCA ablutions, ultrasonic cleaning process at present.Wherein wipe method to micron with
On large scale particle it is more effective, and be difficult to remove the particle of nanoscale；RCA cleanings belong to Chemical cleaning, can reduce
Absorption affinity between particle and substrate, but the heavy corrosion of substrate can be caused if the concentration of improper chemical solution is controlled,
Cause the increase of surface roughness；Ultrasonic wave clean by the physics of ultrasonic wave, chemical action remove substrate surface from micron to
The particle of nanoscale scope, the mass and automation for realizing substrate is cleaned, but when ultrasound parameter selects improper, then can be because
Substrate surface pollutant is not enough caused for cleaning dynamics cannot be cleaned up, or cause substrate surface because cleaning dynamics are excessive
Produce the physical damnifications such as cut, pit.
The ultrasound parameter of the ultrasonic effect of influence mainly has supersonic frequency, ultrasonic power and ultrasonic time etc., known
In ultrasonic cleaning method, cleaning parameterses are obtained mainly by long-term experience, and this mode not only needs to consume the substantial amounts of time and goes
Attempt, gained technique cannot also be ensured of best available technique.Low for known 20KHz ~ 500KHz, middle band frequency it is super
Sound wave is cleaned, and the cavitation effect of ultrasonic wave provides main cleaning removal and acts on.Due to the presence of effect of boundary layer, different frequencies
Rate ultrasonic wave has selectivity to the place to go effect of particle, wherein 20KHz ~ 200KHz low-frequency ranges due to boundary layer it is thicker, it is main
The ultrasonic cavitation intensity acted in micron scale above particle, and this frequency range is big, while particle is removed
Easily cause and the defect of substrate super-smooth surface is damaged, therefore need to find suitable ultrasonic power in guarantor for this frequency range
Surface damage will not be produced while card cleaning efficiency；Mid Frequency for 200KHz ~ 500KHz, the relatively thin cavitation of boundary layer thickness
Effect to the following size granule of micron effectively, but generally cavitation intensity it is on the weak side, even if in Vltrasonic device Operation at full power according to
So occur that particle removes sordid phenomenon, therefore for Mid Frequency ultrasonic wave, it is necessary to find the side for lifting its cavitation effect
Method.Decomposing hydrogen dioxide solution is caused to discharge oxygen in hydrogen peroxide by the way that ammoniacal liquor is injected, by increasing capacitance it is possible to increase the cavitation nucleus in ultrasonic liquid
（The minute bubbles of micro-meter scale）, the effect of enhancing cavitation is played, but if the ratio of ammoniacal liquor is relatively low, cannot effectively lift cavitation
Intensity, and ammoniacal liquor ratio is higher causes hydrogen peroxide acutely to decompose a large amount of gases of release, gas can excessively hinder in liquid on the contrary
Cavitation, weakens the cleaning action to substrate, therefore be also required to find stoicheiometry of the effective method to quantify solution.This
Outward, no matter low frequency ultrasound or mid-frequency ultrasonic, ultrasonic time is also the key factor that influence is cleaned by ultrasonic effect, and ultrasonic time is not
Foot can cause that base-plate cleaning is not clean, and ultrasonic time is long, and substrate surface physical damnification, therefore ultrasonic time can be caused also to need
Quantitative analysis is realized before cleaning and is confirmed.
Therefore, the present invention regarding to the issue above, proposes a kind of laser film element super-smooth surface fused quartz optics base
Plate ultrasonic cleaning method, for the preparation of high damage threshold laser film element provides the strong branch of optical substrate cleaning link
Support.
The content of the invention
It is cleaned by ultrasonic with super-smooth surface fused quartz optical substrate the purpose of the present invention is to propose to a kind of laser film element
Method.
Laser film element proposed by the present invention super-smooth surface fused quartz optical substrate ultrasonic cleaning method, specific step
It is rapid as follows, including ultrasound parameter optimization and ultrasonic cleaning two parts content：
(1) the fused quartz substrate that will scribble 1 ~ 3 μm of silica bead is put into 80KHz ultrasound pure water grooves, and ultrasonic time sets
It is set to 3 minutes, ultrasonic power output is gradually reduced since 100% with 10% step-length, finds the ultrasound that cleaning efficiency is more than 90%
Lowest power；
(2) under the ultrasonic lowest power that step (1) confirms, it is 3 minutes, 6 minutes, 9 minutes that ultrasonic time is selected respectively
With 12 minutes, ultrasound terminate after using Leica microscopic fused quartz substrate surfaces, statistic diameters is more than 1 μm of hole shape defect
Quantity, confirms the minimum ultrasonic time of defect；
(3) the fused quartz substrate that will scribble 0.3 ~ 1 μm of silica bead is respectively put into 400KHz ultrasonic tanks, by ultrasonic work(
Rate is set to total power, and ultrasonic time is set to 3 minutes, injects hydrogen peroxide, is then injected separately into different amounts of ammoniacal liquor, finds clear
Wash the proportioning of pure water when efficiency is more than 90%, hydrogen peroxide, ammoniacal liquor；
(4) under being more than 90% pure water, hydrogen peroxide, the proportioning of ammoniacal liquor in the cleaning efficiency that step (3) confirms, each is frequently
It is 3 minutes, 6 minutes, 9 minutes and 12 minutes that rate selects ultrasonic time respectively, and ultrasound is observed after terminating using AFM
Fused quartz base plate surface roughness, finds most short ultrasonic time of the cleaning efficiency more than 90%；
(5) the fused quartz substrate of cleaning will be needed to be placed into pure water, according to step（1）The ultrasonic lowest power of middle determination
And step（2）Described ultrasonic time implements first stage ultrasonic cleaning to fused quartz substrate, to remove fused quartz substrate surface
Micrometer size granule；
(6）The fused quartz substrate cleaned the need for step (5) Suo Shu is placed into pure water and dioxygen water mixed liquid, according to
Step（3）Pure water, hydrogen peroxide, the proportioning of ammoniacal liquor add ammoniacal liquor when the cleaning efficiency of middle determination is more than 90%, and according to step
（4）The most short ultrasonic time of middle determination is implemented second stage and is cleaned by ultrasonic to substrate, to remove substrate surface Asia metrical scale particle；
(7）The fused quartz substrate that step (6) is obtained is placed into pure water groove, 80KHz is respectively adopted and 170KHz is each
Ultrasound 1 minute, changes water, and again each ultrasonic 1 minute using 80KHz and 170KHz, slow lifting obtains clean, dry molten stone
English substrate, completes surface clean.
In the present invention, the step（1）The peak power output of the supersonic generator that middle ultrasonic pure water groove is used for
400W。
In the present invention, the step（2）Middle silica bead size is any in 3 μm, 2 μm, 1 μm, 0.6 μm or 0.3 μm
Kind；The distribution density of silica bead is controlled in 30~50/mm2。
In the present invention, the step（3）It is pure that the purity of middle ammoniacal liquor and hydrogen peroxide is analysis.
The present invention especially realizes the quantification of optical substrate surface clean, for the improvement of base-plate cleaning technique provides data branch
Support, it is to avoid substrate inside and surface produce defect due to overclean, it is ensured that substrate has damage threshold high.
Brief description of the drawings
Fig. 1 low-frequency ranges are to micro-meter scale bead difference ultrasonic time lower surface defect MIcrosope image：3 points of (a) ultrasound
Clock, (b) ultrasound 6 minutes, (c) ultrasound 12 minutes；
Fig. 2 Mid Frequencies are to the afm image under micro-meter scale bead difference ultrasonic time：A () ultrasound 3 minutes, (b) surpasses
Sound 6 minutes, (c) ultrasound 9 minutes.
Specific embodiment
The present invention is elaborated with example below in conjunction with the accompanying drawings：
Embodiment 1：Firstly the need of the optimal ultrasonic cleaning for finding ultra-smooth fused quartz substrate before formal cleaning is implemented
Parameter, particular content is as follows.
On the φ 30mm fused quartz optical substrates of clean surface spin coating size uniformity, uniform mixing diameter be respectively 1 μm,
2 μm, 3 μm of silica beads, the substrate of bead is scribbled using Leica microscopics, confirms that substrate surface bead is evenly distributed,
The distribution density of Taking Pictures recording bead surface bead；Then the substrate that bead will be scribbled is put into 80KHz ultrasonic tanks, ultrasonic time
It is set to 3 minutes, ultrasonic power output is gradually reduced since 100% with 10% step-length, each ultrasound is aobvious using Leica after terminating
Micro mirror sees substrate surface bead density, and the bead density before contrast cleaning is so as to obtain the cleaning efficiency after ultrasound every time, such as table 1
The shown optimal ultrasonic power for 80KHz is 60%；Under the minimum ultrasonic power of above-mentioned confirmation, ultrasonic time is selected respectively
It it is 3 minutes, 6 minutes, 12 minutes, ultrasound cheated shape defect situation, such as Fig. 1 after terminating using Leica microscopics substrate surface
It is shown；Be can confirm that by above-mentioned experiment and be not to be exceeded 6 minutes for the fused quartz substrate ultrasonic time to be cleaned.
Table 1：
| Ultrasonic power | 100% | 80% | 60% | 40% | 20% |
| Cleaning efficiency | 97% | 95% | 83% | 60% | 35% |
Separately take spin coating size uniformity on the φ 30mm fused quartz optical substrates of clean surface, mixed uniformly a diameter of 0.3 μ
M, 0.6 μm, 1 μm of silica bead, the substrate of bead is scribbled using Leica microscopics, confirms the distribution of substrate surface bead
Uniformly, take pictures, record bead surface bead distribution density；The intermediate frequency that 0.3 ~ 1 μm of bead substrate is respectively put into 400Khz will be scribbled
In ultrasonic tank, ultrasonic time is set to 3 minutes, successively injects the mixed liquor of the pure water, hydrogen peroxide and ammoniacal liquor that are matched in table 2,
Each ultrasound uses Leica microscopes to see substrate surface bead density after terminating, the bead density before contrast cleaning is so as to obtain
The ultrasonic cleaning efficiency of different ratio solution, as shown in table 2, pure water, hydrogen peroxide and ammoniacal liquor optimum solvent proportioning are 60：10 ：
Cleaning efficiency highest when 1；Under the optimum solvent proportioning of above-mentioned confirmation, each frequency selects ultrasonic time for 3 minutes, 6 respectively
Minute, 9 minutes, 12 minutes, ultrasound observed base plate surface roughness after terminating using AFM, as shown in Figure 2；Pass through
Above-mentioned experiment can confirm that and is not to be exceeded 9 minutes for the fused quartz substrate 400KHz ultrasonic times to be cleaned.
Table 2：
After optimal clean parameter is obtained, next start to be cleaned by ultrasonic fused quartz substrate：
The fused quartz substrate of cleaning will be needed to be placed into pure water, according to the ultrasonic power and ultrasonic time pair of above-mentioned determination
Substrate implements first stage ultrasonic cleaning, to remove substrate surface micrometer size granule；The fused quartz substrate of cleaning will be needed to put
Insert in pure water and dioxygen water mixed liquid, according to step（1）The proportioning of middle determination adds ammoniacal liquor, and according to step（1）Middle determination
Ultrasonic time second stage implemented to substrate be cleaned by ultrasonic, to remove substrate surface Asia metrical scale particle；Substrate is placed into
It is ultrasonic 1 minute using 80Khz and 400Khz in pure water groove, water is changed, it is ultrasonic 1 minute using 80Khz and 400Khz again,
Slow lifting, obtains clean, dry fused quartz substrate, completes surface clean.
The above-mentioned description to embodiment is technological thought and feature to illustrate the invention, it is therefore intended that the technical field
Those of ordinary skill be understood that and apply the present invention.Person skilled in the art obviously easily can implement to these
Example makes various modifications, and General Principle described herein is applied in other embodiment without by creative labor
It is dynamic.Therefore, the invention is not restricted to embodiment here, those skilled in the art's announcement of the invention is done for the present invention
The improvement and modification for going out all are included within the scope of the present invention.
Claims (4)
1. a kind of laser film element super-smooth surface fused quartz optical substrate ultrasonic cleaning method, it is characterised in that specific step
It is rapid as follows：
(1) the fused quartz optical substrate that will scribble 1 ~ 3 μm of silica bead is put into 80KHz ultrasound pure water grooves, and ultrasonic time sets
It is set to 3 minutes, ultrasonic power output is gradually reduced since 100% with 10% step-length, finds the ultrasound that cleaning efficiency is more than 90%
Lowest power；
(2) under the ultrasonic lowest power that step (1) confirms, it is 3 minutes, 6 minutes, 9 minutes and 12 that ultrasonic time is selected respectively
Minute, ultrasound cheats shape defect more than 1 μm after terminating using Leica microscopic fused quartz optical substrates surface, statistic diameters
Quantity, confirms the minimum ultrasonic time of defect；
(3) the fused quartz optical substrate that will scribble 0.3 ~ 1 μm of silica bead is respectively put into 400KHz ultrasonic tanks, by ultrasonic work(
Rate is set to total power, and ultrasonic time is set to 3 minutes, injects hydrogen peroxide, is then injected separately into different amounts of ammoniacal liquor, finds clear
Wash the proportioning of pure water when efficiency is more than 90%, hydrogen peroxide, ammoniacal liquor；
(4) under being more than 90% pure water, hydrogen peroxide, the proportioning of ammoniacal liquor in the cleaning efficiency that step (3) confirms, each frequency point
Not Xuan Ze ultrasonic time be 3 minutes, 6 minutes, 9 minutes and 12 minutes, ultrasound terminate after using AFM observation melt stone
English optical substrate surface roughness, finds most short ultrasonic time of the cleaning efficiency more than 90%；
(5) the fused quartz optical substrate of cleaning will be needed to be placed into pure water, according to step（1）The ultrasonic lowest power of middle determination
And step（2）Described ultrasonic time implements first stage ultrasonic cleaning to fused quartz optical substrate, to remove fused quartz optics
Substrate surface micrometer size granule；
(6）The fused quartz optical substrate cleaned the need for step (5) Suo Shu is placed into pure water and dioxygen water mixed liquid, according to
Step（3）Pure water, hydrogen peroxide, the proportioning of ammoniacal liquor add ammoniacal liquor when the cleaning efficiency of middle determination is more than 90%, and according to step
（4）The most short ultrasonic time of middle determination is implemented second stage and is cleaned by ultrasonic to fused quartz optical substrate, to remove fused quartz optics
Substrate surface Asia metrical scale particle；
(7）The fused quartz optical substrate that step (6) is obtained is placed into pure water groove, 80KHz is respectively adopted and 170KHz is each
Ultrasound 1 minute, changes water, and again each ultrasonic 1 minute using 80KHz and 170KHz, slow lifting obtains clean, dry molten stone
English optical substrate, completes surface clean.
2. laser film element according to claim 1 super-smooth surface fused quartz optical substrate ultrasonic cleaning method,
It is characterized in that：The step（1）The peak power output of the supersonic generator that middle ultrasonic pure water groove is used is 400W.
3. laser film element according to claim 1 super-smooth surface fused quartz optical substrate ultrasonic cleaning method,
It is characterized in that：The step（2）Middle silica bead size is any one in 3 μm, 2 μm or 1 μm；The distribution of silica bead
Density domination is in 30~50/mm2。
4. laser film element according to claim 1 super-smooth surface fused quartz optical substrate ultrasonic cleaning method,
It is characterized in that：The step（3）It is pure that the purity of middle ammoniacal liquor and hydrogen peroxide is analysis.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101665911A (en) * | 2008-09-04 | 2010-03-10 | 浙江师范大学 | Method for preparing giant magnetoresistance films by vacuum vapor deposition method |
| CN102002673A (en) * | 2010-09-17 | 2011-04-06 | 陕西师范大学 | Preparation method of nanocrystalline silicon-aluminum oxide/silicon oxide thermoelectric film material |
| CN102965614A (en) * | 2012-11-23 | 2013-03-13 | 同济大学 | Preparation method of laser film |
| CN103952670A (en) * | 2014-02-13 | 2014-07-30 | 同济大学 | Laser film quantification research method based on artificial defects |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2014080346A (en) * | 2012-10-18 | 2014-05-08 | Jnc Corp | Cleaning method of polycrystal silicon obtained by zinc reduction method |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101665911A (en) * | 2008-09-04 | 2010-03-10 | 浙江师范大学 | Method for preparing giant magnetoresistance films by vacuum vapor deposition method |
| CN102002673A (en) * | 2010-09-17 | 2011-04-06 | 陕西师范大学 | Preparation method of nanocrystalline silicon-aluminum oxide/silicon oxide thermoelectric film material |
| CN102965614A (en) * | 2012-11-23 | 2013-03-13 | 同济大学 | Preparation method of laser film |
| CN103952670A (en) * | 2014-02-13 | 2014-07-30 | 同济大学 | Laser film quantification research method based on artificial defects |
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