CN113655010A - Method for evaluating performance of low-pressure oxygen plasma for cleaning organic pollutants - Google Patents
Method for evaluating performance of low-pressure oxygen plasma for cleaning organic pollutants Download PDFInfo
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- 239000002957 persistent organic pollutant Substances 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 48
- 238000004140 cleaning Methods 0.000 title claims abstract description 31
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 24
- 239000001301 oxygen Substances 0.000 title claims abstract description 24
- 210000002381 plasma Anatomy 0.000 claims abstract description 34
- 238000002834 transmittance Methods 0.000 claims abstract description 14
- 238000011156 evaluation Methods 0.000 claims abstract description 13
- 238000012360 testing method Methods 0.000 claims abstract description 13
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 11
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 125000004430 oxygen atom Chemical group O* 0.000 claims abstract description 5
- 230000008569 process Effects 0.000 claims description 28
- 230000008859 change Effects 0.000 claims description 16
- 239000000356 contaminant Substances 0.000 claims description 13
- 230000003287 optical effect Effects 0.000 claims description 12
- 238000012545 processing Methods 0.000 claims description 12
- 239000011248 coating agent Substances 0.000 claims description 10
- 238000000576 coating method Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 6
- 239000003570 air Substances 0.000 claims description 3
- 239000012528 membrane Substances 0.000 claims description 3
- 238000009832 plasma treatment Methods 0.000 claims description 3
- 238000002310 reflectometry Methods 0.000 claims description 3
- 239000004215 Carbon black (E152) Substances 0.000 abstract description 3
- 239000003344 environmental pollutant Substances 0.000 abstract description 3
- 229930195733 hydrocarbon Natural products 0.000 abstract description 3
- 150000002430 hydrocarbons Chemical class 0.000 abstract description 3
- 231100000719 pollutant Toxicity 0.000 abstract description 3
- 229910052739 hydrogen Inorganic materials 0.000 abstract 2
- 239000001257 hydrogen Substances 0.000 abstract 2
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical group CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- 239000002245 particle Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000006117 anti-reflective coating Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 230000005281 excited state Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000005350 fused silica glass Substances 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/088—Investigating volume, surface area, size or distribution of pores; Porosimetry
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
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Abstract
The invention discloses a performance evaluation method for cleaning organic pollutants by low-pressure oxygen plasmas, which comprises the following steps: obtaining the space concentration of the specific hydrocarbon organic pollutants by utilizing the peak transmittance; rewriting the determined equivalent concentration of the specific hydrocarbon organic pollutants according to the number of hydrogen atoms distributed by the number of carbon atoms; and the evaluation coefficient determined by fitting and constructed by the chemical reaction constant, the space concentration of the active oxygen atoms and the number of hydrogen atoms distributed according to the number of carbon atoms. The evaluation coefficient of the low-pressure oxygen plasma is obtained by using the carbon-hydrogen pollutant equivalent space concentration based on the transmittance test, and the method can be used for evaluating the cleaning performance of the low-pressure oxygen plasma in different states on specific carbon-hydrogen organic pollutants in the porous antireflection film.
Description
Technical Field
The invention relates to the technical field of plasma cleaning, in particular to a performance evaluation method for cleaning organic pollutants by using low-pressure oxygen plasmas.
Background
In high power and high energy laser devices, organic contaminants in the porous antireflective coating of the high flux optical element can seriously affect the light transmission performance and the laser damage threshold of the element. The low-pressure oxygen plasma can effectively treat organic pollutants, but the cleaning effect on different types of organic pollutants is different, and meanwhile, the state of the oxygen plasma can be changed under different process conditions, so that the cleaning performance is changed. Therefore, the performance of the low-pressure oxygen plasma required by cleaning of the specific organic pollutants is determined, so that the high-efficiency cleaning of the organic pollutants is conveniently achieved, and the method has an important supporting function for the low-pressure oxygen plasma in engineering application of removing the organic pollutants on the surface of the optical element.
At present, the evaluation of the performance state of low-pressure plasma is mainly performed by direct description of physical parameters, and the particle state in the plasma is generally measured based on a probe method or a spectroscopic method, and the measurement mainly comprises measurement of electrons and measurement of excited particles in a specific state, so as to evaluate the excitation state of the plasma. The measurement of electrons comprises the measurement of electron temperature, electron density, electron velocity distribution and the like, reflects the overall state of the plasma, but is irrelevant to the organic pollutants to be cleaned, and cannot be used for representing the removal capacity of the low-pressure oxygen plasma on the organic pollutants. The measurement of the excited particles in a specific state can determine the excitation concentration of the specific particles, which can reflect the removal capability of the particles to organic pollutants in plasma, but the active groups participating in the removal reaction of the organic pollutants in the low-pressure oxygen plasma are numerous, and especially the active oxygen atoms in different excited states have direct effects on the removal of the pollutants, so that the low-pressure oxygen plasma cannot be used for evaluating the performance of the low-pressure oxygen plasma in the cleaning process of the organic pollutants.
Disclosure of Invention
An object of the present invention is to solve at least the above problems and/or disadvantages and to provide at least the advantages described hereinafter. To achieve these objects and other advantages in accordance with the purpose of the invention, there is provided a method for evaluating performance of low pressure oxygen plasma cleaning of organic contaminants, comprising:
step one, testing the peak wavelength and the peak transmittance of the position A of the optical element without the pollution of the antireflection film;
step two, testing the change of the peak transmittance of the antireflection film in the low-pressure oxygen plasma treatment process;
calculating the change of the organic pollutant space concentration along with the processing time;
calculating the change of the equivalent space concentration of the organic pollutants along with the processing time;
fifthly, performing exponential fitting on the change of the equivalent space concentration along with the processing time;
and step six, using an index coefficient alpha obtained by index fitting as a cleaning performance evaluation index.
Wherein, preferably, in the step one, the process is as follows:R f =1-T f (ii) a In the formula: peak transmittanceT f Measured by an optical element coated with the antireflection film in an uncontaminated state by a spectrophotometer or a calibrated energy meter,R f the remaining reflectance.
Wherein, in the second step, the process is preferably as follows: the mixture of air, organic pollutants and coating materials is used as a film layer; according to the residual reflectivity of the filmR f Calculating to obtain the refractive index of the film layern f ：R f =(n 0 n g -n f 2)/(n 0 n g +n f 2 ) (ii) a In the formula:n 0 is a refractive index of air and is,n g the refractive index of the coating material; and then calculating the porosity of the film layer according to a mixed refractive index formulaf i ：n m 2 =[∑n i 2 f i /(n i 2 +1)]/[∑f i /(n i 2 +1)](ii) a In the formula:n i is the first in the mixtureiThe refractive index of the seed medium is,n m for mixing refractive indices, i.e.n m =n f 。
Among them, preferably, in step three, it includes:
s31, testing the change of the peak wavelength and the peak transmittance of the polluted antireflection film-coated optical element at the position A in the processing process; the testing time interval is not less than 5 times;
s32, calculating the space concentration C of the organic pollutants1(ii) a The process is as follows: calculating the mixed refractive index of the polluted film layer through the first step and the second stepn m (ii) a Mixed refractive index through contaminated film layern m And refractive indices of air, organic contaminants, and coating materials, respectivelyn i Calculating to obtain the current porosity of the film layerf i (ii) a The porosity through the membrane layerf i And original porosityf i Calculating the space filling rate of the organic pollutants in the film layer; calculating the space concentration of the organic pollutants according to the space filling rate, the molar mass and the density of the organic pollutantsC 1。
Wherein, preferably, in the fourth step, the process is as follows: rewriting organic contaminants to the expression of the number of hydrogen atoms as a function of the number of carbon atoms, i.e.CH2nIn the form of (a) a (b),ndetermined by the chemical formula of the contaminant; then according to the spatial concentration of the organic pollutantsC 1Calculate the correspondingCH2nSteric concentration of radicalsC 2Due to the chemical formula of the organic pollutantsC x H y Then, thenCH2nThe method comprises the following steps:n=y/ 2xthe following can be obtained:C 2 =C 1 *x。
among them, it is preferable that in the fifth stepThe process is as follows: the equivalent spatial concentration of the organic pollutants by adopting a least square methodC 2 Exponential fit was performed over time.
Wherein, preferably, in step six, the process is as follows:α=k CH2n *c o* n+2 (ii) a In the formula:k CH2n a chemical reaction constant is constructed for the organic pollutants according to the calculation of the number of carbon atoms;c o* is the spatial concentration of oxygen atoms;nthe number of hydrogen atoms is the number of carbon atoms.
The invention at least comprises the following beneficial effects:
the method for evaluating the performance of the low-pressure oxygen plasma cleaning porous antireflection film on the basis of the determination of the equivalent spatial concentration change of the organic pollutants during cleaning realizes the performance evaluation of the hydrocarbon organic pollutants in the low-pressure oxygen plasma cleaning porous antireflection film, can be used for evaluating the performance of a low-pressure plasma cleaning system for removing the organic pollutants on the surface of an optical element, evaluates the cleaning capacity of the low-pressure plasma cleaning system on specific pollutants, and is convenient for designing or selecting a proper plasma cleaning system according to requirements. Meanwhile, the evaluation coefficient established by the invention can be used for setting and applying the plasma cleaning process parameters by combining with the plasma emission spectrum data, and is particularly beneficial to the process parameter design of the plasma cleaning duration. Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Drawings
FIG. 1 is a flow chart of the present invention.
Detailed Description
The present invention is further described in detail below with reference to the attached drawings so that those skilled in the art can implement the invention by referring to the description text. It will be understood that terms such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
Example 1:
a performance evaluation method for cleaning organic pollutants by low-pressure oxygen plasmas comprises the following steps:
(as shown in FIG. 1), step one, testing the peak wavelength and the peak transmittance of the optical element A without the pollution of the antireflection film; the process is as follows:R f =1-T f (ii) a In the formula: peak transmittanceT f Measured by an optical element coated with the antireflection film in an uncontaminated state by a spectrophotometer or a calibrated energy meter,R f the remaining reflectance.
Step two, testing the change of the peak transmittance of the antireflection film in the low-pressure oxygen plasma treatment process; the process is as follows: the mixture of air, organic pollutants and coating materials is used as a film layer; according to the residual reflectivity of the filmR f Calculating to obtain the refractive index of the film layern f ：R f =(n 0 n g -n f 2)/(n 0 n g +n f 2 ) (ii) a In the formula:n 0 is a refractive index of air and is,n g the refractive index of the coating material; and then calculating the porosity of the film layer according to a mixed refractive index formulaf i ：n m 2 =[∑n i 2 f i /(n i 2 +1)]/[∑f i /(n i 2 +1)](ii) a In the formula:n i is the first in the mixtureiThe refractive index of the seed medium is,n m for mixing refractive indices, i.e.n m =n f 。
Calculating the change of the organic pollutant space concentration along with the processing time; it includes:
s31, testing the change of the peak wavelength and the peak transmittance of the polluted antireflection film-coated optical element at the position A in the processing process; the testing time interval is not less than 5 times;
s32, calculatingSpatial concentration of contaminants C1(ii) a The process is as follows: calculating the mixed refractive index of the polluted film layer through the first step and the second stepn m (ii) a Mixed refractive index through contaminated film layern m And refractive indices of air, organic contaminants, and coating materials, respectivelyn i Calculating to obtain the current porosity of the film layerf i (ii) a The porosity through the membrane layerf i And original porosityf i Calculating the space filling rate of the organic pollutants in the film layer; calculating the space concentration of the organic pollutants according to the space filling rate, the molar mass and the density of the organic pollutantsC 1。
Calculating the change of the equivalent space concentration of the organic pollutants along with the processing time; the process is as follows: rewriting organic contaminants to the expression of the number of hydrogen atoms as a function of the number of carbon atoms, i.e.CH2nIn the form of (a) a (b),ndetermined by the chemical formula of the contaminant; then according to the spatial concentration of the organic pollutantsC 1Calculate the correspondingCH2nSteric concentration of radicalsC 2Due to the chemical formula of the organic pollutantsC x H y Then, thenCH2nThe method comprises the following steps:n=y/2xthe following can be obtained:C 2 =C 1 *x。
fifthly, performing exponential fitting on the change of the equivalent space concentration along with the processing time; the process is as follows: the equivalent spatial concentration of the organic pollutants by adopting a least square methodC 2 Exponential fit was performed over time.
And step six, using an index coefficient alpha obtained by index fitting as a cleaning performance evaluation index. The process is as follows:α= k CH2n *c o* n+2 (ii) a In the formula:k CH2n a chemical reaction constant is constructed for the organic pollutants according to the calculation of the number of carbon atoms;c o* is the spatial concentration of oxygen atoms;nthe number of hydrogen atoms is the number of carbon atoms.
Example 2:
(see table 1) sol-gel silica antireflection film based on fused silica substrate, the refractive index of the coating material is 1.44; according to the result of uncontaminated state, the original porosity of the filmf i About 0.48980; if the contaminant is DBP (dibutyl phthalate) the chemical formula is C16H22O4Molecular weight of 278.34, refractive index of 1.4911, density of 1.053g/cm 3; from time to CH density (equivalent spatial concentration C)2) Fitting to obtain 0.00002269s-1Evaluation coefficient of (2)αThe method is used for evaluating the cleaning capability of the low-pressure plasma cleaning system on the DBP, and is convenient for subsequent requirement design or selection of a proper plasma cleaning system.
TABLE 1
The number of apparatuses and the scale of the process described herein are intended to simplify the description of the present invention. Applications, modifications and variations of the present invention will be apparent to those skilled in the art. While embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable in various fields of endeavor to which the invention pertains, and further modifications may readily be made by those skilled in the art, it being understood that the invention is not limited to the details shown and described herein without departing from the general concept defined by the appended claims and their equivalents.
Claims (7)
1. A performance evaluation method for cleaning organic pollutants by low-pressure oxygen plasmas is characterized by comprising the following steps:
step one, testing the peak wavelength and the peak transmittance of an antireflection film plated on an optical element in an uncontaminated state at the position A;
step two, testing the change of the peak transmittance of the antireflection film in the low-pressure oxygen plasma treatment process;
calculating the change of the organic pollutant space concentration along with the processing time;
calculating the change of the equivalent space concentration of the organic pollutants along with the processing time;
fifthly, performing exponential fitting on the change of the equivalent space concentration along with the processing time;
and step six, using an index coefficient alpha obtained by index fitting as a cleaning performance evaluation index.
2. The method of claim 1, wherein the first step comprises the steps of:R f =1-T f (ii) a In the formula: peak transmittanceT f Measured by an optical element coated with the antireflection film in an uncontaminated state by a spectrophotometer or a calibrated energy meter,R f the remaining reflectance.
3. The method of claim 1, wherein in step two, the process comprises: the mixture of air, organic pollutants and coating materials is used as a film layer; according to the residual reflectivity of the filmR f Calculating to obtain the refractive index of the film layern f ：R f =(n 0 n g -n f 2)/(n 0 n g +n f 2 ) (ii) a In the formula:n 0 is a refractive index of air and is,n g the refractive index of the coating material; and then calculating the porosity of the film layer according to a mixed refractive index formulaf i ：n m 2 =[∑n i 2 f i /(n i 2 +1)]/[∑f i /(n i 2 +1)](ii) a In the formula:n i is the first in the mixtureiThe refractive index of the seed medium is,n m for mixing refractive indices, i.e.n m =n f 。
4. The method of claim 1, wherein the step three comprises:
s31, testing the change of the peak wavelength and the peak transmittance of the polluted antireflection film-coated optical element at the position A in the processing process, wherein the testing times are 5 times;
s32, calculating the space concentration C of the organic pollutants1(ii) a The process is as follows: calculating the mixed refractive index of the polluted film layer through the first step and the second stepn m (ii) a Mixed refractive index through contaminated film layern m And refractive indices of air, organic contaminants, and coating materials, respectivelyn i Calculating to obtain the current porosity of the film layerf i (ii) a The porosity through the membrane layerf i And original porosityf i Calculating the space filling rate of the organic pollutants in the film layer; calculating the space concentration of the organic pollutants according to the space filling rate, the molar mass and the density of the organic pollutantsC 1。
5. The method for evaluating the performance of cleaning organic pollutants by using low-pressure oxygen plasma according to claim 1, wherein in the fourth step, the process comprises the following steps: rewriting organic contaminants to the expression of the number of hydrogen atoms as a function of the number of carbon atoms, i.e.CH2nIn the form of (a) a (b),ndetermined by the chemical formula of the contaminant; then according to the spatial concentration of the organic pollutantsC 1Calculate the correspondingCH2nSteric concentration of radicalsC 2Due to the chemical formula of the organic pollutantsC x H y Then, thenCH2nThe method comprises the following steps:n=y/2xthe following can be obtained:C 2 =C 1 *x。
6. the low pressure oxygen plasma cleaning of claim 1The method for evaluating the performance of the organic pollutants is characterized in that in the fifth step, the process is as follows: the equivalent spatial concentration of the organic pollutants by adopting a least square methodC 2 Exponential fit was performed over time.
7. The method of claim 1, wherein in step six, the process comprises:α=k CH2n *c o* n+2 (ii) a In the formula:k CH2n a chemical reaction constant is constructed for the organic pollutants according to the calculation of the number of carbon atoms;c o* is the spatial concentration of oxygen atoms;nthe number of hydrogen atoms is the number of carbon atoms.
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| CN202111388212.8A CN114112843B (en) | 2021-10-18 | 2021-11-22 | Performance evaluation method for cleaning organic pollutants by low-pressure oxygen plasma |
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| JPH0721459B2 (en) * | 1988-04-07 | 1995-03-08 | 株式会社日立製作所 | Pseudo-pollutant stamping tool for cleaning performance evaluation |
| JP2011039327A (en) * | 2009-08-12 | 2011-02-24 | Hitachi Displays Ltd | Detergency evaluation method and method for manufacturing liquid crystal display device |
| JP2011193985A (en) * | 2010-03-18 | 2011-10-06 | Asahi Kasei Kuraray Medical Co Ltd | Leak test method for hollow fiber membrane type medical instrument |
| KR101005636B1 (en) * | 2010-03-26 | 2011-01-05 | 정장근 | Purification system for removing noxious gases and all maloder by using underwater plasma generation apparatus |
| KR101306939B1 (en) * | 2011-11-25 | 2013-09-10 | 주식회사 시노펙스 | Filtration membrane cleaning apparatus and method |
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| CN107271402A (en) * | 2017-07-28 | 2017-10-20 | 中国工程物理研究院激光聚变研究中心 | Molecular state organic pollution on-Line Monitor Device and detection method in confined space |
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| CN114112954B (en) * | 2021-10-18 | 2024-04-19 | 中国工程物理研究院激光聚变研究中心 | Process duration calculation method for cleaning organic pollutants by low-pressure oxygen plasma |
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