CN102288561A - Method for detecting trace impurity in damaged layer of polished sub-surface of optical glass - Google Patents
Method for detecting trace impurity in damaged layer of polished sub-surface of optical glass Download PDFInfo
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- CN102288561A CN102288561A CN2011101920500A CN201110192050A CN102288561A CN 102288561 A CN102288561 A CN 102288561A CN 2011101920500 A CN2011101920500 A CN 2011101920500A CN 201110192050 A CN201110192050 A CN 201110192050A CN 102288561 A CN102288561 A CN 102288561A
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- zymoprotein
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Abstract
The invention discloses a method for detecting a trace impurity in a damaged layer of a polished sub-surface of optical glass. The method comprises the following steps of: preparing a water solution which comprises rare-earth metal, and adjusting a pH value; mixing the water solution and a laccase solution, putting a mixed solution sample into a constant-temperature water bath, and thus obtaining the percentage of enzyme protein residual activity of each sample by determining an enzyme protein activity value and a standard enzyme activity after reaction; according to the percentage and the concentration, corresponding to the percentage, of the rare-earth metal in each solution sample, fitting a relation curve; introducing etching liquid into a total surface of a glass sample to be detected or an unmasked local area to be detected by using a liquid-moving machine, detecting etching depth and collecting etching remained liquid after etching reaction; and adjusting the pH value of the etching remained liquid, mixing the etching remained liquid and the laccase solution, detecting the percentage of the enzyme protein residual activity in the etching remained liquid, and calculating the concentration of the trace impurity according to the relation curve. The method has the advantages of accurate and reliable detection result and flexible and quick detection process.
Description
Technical field
The present invention relates to the detection method of trace impurity in a kind of optical glass, relate in particular to the detection method of trace impurity in a kind of optical glass polishing damage layer.
Background technology
In high light environment such as laser fusion, superpower laser, the polishing impurity strong absorption laser photon energy that embeds in the optical glass, the damage from laser of initiation matrix and film material, the serviceable life of greatly having reduced optical element.Introduce the polishing impurity that concentration is successively decreased along the degree of depth by resedimentation at subsurface stratum in the polishing process, maximum insert depth is in sub-micron to micro-meter scale, and impurity content is extremely low, peak concentration is in the ppm magnitude, and detection methods such as spectroscopy and inductively coupled plasma atomic emission spectrometry are all powerless to this.At present, optical element polishing impurity concentration generally acknowledges that effective detection method is a secondary ion mass spectrometry, this method uses the ion microprobe bombardment successively to degrade sample surfaces, and detection elements secondary ion intensity is with the variation of bombardment time, and then the depth profiling result of acquisition sample.But secondary ion mass spectrometry depends on the high precision measurement instrument, detects with high costsly, and detection efficiency is low, and the surveyed area of this method limited (100 μ m * 100 μ m), can't realize glass surface or determine the detection in zone on it.Therefore, to those skilled in the art, be necessary to develop the detection method of the trace polishing impurity concentration that a kind of versatility is stronger, cost is lower, in optics processing occasion, to apply.
Summary of the invention
The technical problem to be solved in the present invention is to overcome the deficiencies in the prior art, provide a kind of testing result accurately, reliable, the testing process detection method of trace impurity in the sub-surface damage layer of optical glass polishing fast flexibly.
For solving the problems of the technologies described above, the technical scheme that the present invention proposes is the detection method of trace impurity in a kind of optical glass polishing sub-surface damage layer, may further comprise the steps:
(1) solution preparation: prepare the aqueous solution that contains rare earth ion or rare-earth oxide of a series of variable concentrations, and adjust its pH value; The aqueous solution that this is a series of is mixed with laccase solution respectively, obtains a series of solution example;
(2) measure zymoprotein residual activity number percent: a series of solution example that step (1) is obtained places the water bath with thermostatic control insulation reaction, reaction back obtains zymoprotein activity value in each solution example by measuring the solution optical absorption intensity, obtains the standard enzyme vigor by measuring described laccase solution optical absorption intensity again; According to zymoprotein activity value that has recorded and standard enzyme vigor, obtain the zymoprotein residual activity number percent (zymoprotein residual activity number percent C%=zymoprotein activity value/standard enzyme vigor * 100%) of each solution example;
(3) matched curve: each when corresponding with it solution example middle rare earth concentration of metal of zymoprotein residual activity percentage of each solution example of measuring according to step (2) simulates the relation curve of zymoprotein residual activity number percent-rare earth metal concentration;
(4) etching glass to be measured: (known etching solution all can on the full surface of glass sample to be measured or at the introducing etching solution in zone local to be measured of mask not to use pipettor, generally with hydrofluorite or highly basic), (preferred 30s～5min) back was taken out and was cleaned the fixed interval time, detect the etch depth of glass sample to be measured, and collect the surplus liquid of etching behind the etching reaction;
(5) detect the surplus liquid of etching: adjust the pH value of the surplus liquid of described etching, and it is mixed with laccase solution, according to the method for measuring zymoprotein residual activity number percent in the step (2), detect the zymoprotein residual activity number percent in the surplus liquid of this etching then; At last according to the relation curve that obtains in this zymoprotein residual activity percent value and the step (3), calculate under the described etch depth concentration of trace impurity in the optical glass polishing sub-surface damage layer.
Above-mentioned optical glass polishes in the detection method of trace impurity in the sub-surface damage layer, the aqueous solution that contains rare earth ion or rare-earth oxide of described a series of variable concentrations preferably comprises the rare earth metal aqueous solution of five kinds of variable concentrations at least, wherein, the mass percent of the rare earth metal aqueous solution of least concentration is lower than 10
-6Ppm, the mass percent of the rare earth metal aqueous solution of maximum concentration is higher than 10
-3Ppm.Can make the relation curve equation of follow-up foundation have more rationality and representativeness like this.
The detection method of trace impurity in the above-mentioned optical glass polishing sub-surface damage layer, in described step (1) and the step (5), the pH value preferably is controlled at 4～6 after adjusting.
The detection method of trace impurity is preferably mainly formulated by laccase, guaiacol substrate (is the enzymatic activity that reaction substrate is determined laccase with the guaiacol) and sodium succinate damping fluid in the described laccase solution in the above-mentioned optical glass polishing sub-surface damage layer; The concentration of described laccase is 50mg/l～100mg/l, and the concentration of described guaiacol substrate is 50ml/l～200ml/l.
The detection method of trace impurity in the above-mentioned optical glass polishing sub-surface damage layer, in the described step (2), the temperature of water bath with thermostatic control is controlled at 20 ℃～50 ℃, and the time of insulation reaction is 20min～60min.
In the above-mentioned optical glass polishing sub-surface damage layer in the detection method of trace impurity, the spectrophotometer of selecting for use during described mensuration solution optical absorption intensity is preferably measured in 400nm～700nm wavelength coverage.
In the detection method of trace impurity, described rare earth metal is preferably cerium or lanthanum in the above-mentioned optical glass polishing sub-surface damage layer.
The detection method of trace impurity in the above-mentioned optical glass polishing sub-surface damage layer, when described rare earth metal was cerium, the functional equation of described relation curve was: Y=0.37501-0.02497InX, R
2=0.98641.
Technique scheme of the present invention mainly is based on following principle: biological study shows that rare earth ion and oxide thereof have had strong inhibitory effects to the zymoprotein activity under extremely low concentration, and we are with Ce
4+And La
3+Be example, its concentration is respectively 10
-3When ppm and 1ppm, the residual activity of laccase is respectively 90.7% and 64.4%, and Fe
3+, Al
3+Deng metallic ion laccase activity is not obviously influenced.The polishing of considering optical element mostly is rare-earth oxide with material, we creatively utilize the rejection characteristic of rare-earth oxide to laccase activity in view of the above, obtain the typical curve of laccase residual activity number percent and rare-earth oxide concentration relationship earlier; And then employing photoresist mask glass surface specific region, and introduce a small amount of etching solution in masked areas not by pipettor, realize successively degrading of the definite zone of glass surface to be measured (not masked areas), with this size that obtains glass surface or determine rare-earth oxide impurity concentration in the regional affected layer on it, and then also can obtain the regularity of distribution of impurity concentration along depth direction.
Compared with prior art, the invention has the advantages that: the present invention utilizes trace rare-earth oxide impurity in the optical glass polishing sub-surface damage layer zymoprotein free radical to be formed the influence of ability, the detection method of trace impurity in the optical glass sub-surface damage layer of a kind of low cost, high-level efficiency and procedure has been proposed, this detection method not only testing result is accurate, reliable, and testing process is quick, detection efficiency is higher, the detection cost is low, the surveyed area flexible and controllable can satisfy batch detection fully, detects flexibly, the demand of high Precision Detection.
Description of drawings
Fig. 1 is the process chart that optical glass polishes the detection method of trace impurity in the sub-surface damage layer in the embodiment of the invention.
Fig. 2 is the function relation curve of cerium oxide concentration and laccase albumen residual activity number percent in the embodiment of the invention.
Fig. 3 is the mode of operation synoptic diagram during to glass sample surface selectivity etching to be measured in the embodiment of the invention.
Fig. 4 be in the embodiment of the invention 1 glass sample impurity concentration to be measured along the scatter chart of depth direction.
Fig. 5 be in the embodiment of the invention 2 glass to be measured (K9) sample impurity concentration along the scatter chart of depth direction.
Marginal data
1, glass sample to be measured; 2, photoresist; 3, zone to be measured; 4, pipettor.
Embodiment
Below in conjunction with Figure of description and specific embodiment the present invention is further described.
Embodiment 1:
The detection method of trace impurity in a kind of optical glass polishing sub-surface damage layer of the present invention as shown in Figure 1 may further comprise the steps:
(1) solution preparation: the cerium oxide (CeO of five kinds of variable concentrations of preparation
2) (concentration value is respectively 10 to aqueous solution
-7Ppm, 10
-4Ppm, 10
-3Ppm, 10
-2Ppm and 10
-1And adjust each cerium oxide pH value of aqueous solution to 4.5 ppm); The cerium oxide aqueous solution of these five kinds of variable concentrations is respectively got 3mL, mix with isopyknic laccase solution respectively then, contain the crude enzyme liquid (fermentation liquor is got supernatant as crude enzyme liquid behind the centrifugal 10min of 10000r/min) of 0.6 mL, the guaiacol substrate of 1mmol/L and the sodium succinate damping fluid of 50mmol/L in the laccase solution, obtain five kinds of different solution examples;
(2) measure zymoprotein residual activity number percent: a series of solution example that step (1) is obtained places 25 ℃ water bath with thermostatic control insulation reaction 30min, the reaction back is by using spectrophotometer to measure solution optical absorption intensity (the enzyme reaction mixed liquor with 100 ℃ of deactivations is contrast) under the wavelength of 465nm, obtain the zymoprotein activity value in each solution example, obtain the standard enzyme vigor by measuring described laccase solution optical absorption intensity again; According to zymoprotein activity value that has recorded and standard enzyme vigor, obtain the zymoprotein residual activity number percent of each solution example;
(3) matched curve: the concentration value of cerium oxide in when corresponding with it each solution example of the zymoprotein residual activity percentage of each solution example of measuring according to step (2) simulates the relation curve of zymoprotein residual activity number percent-rare earth metal concentration as shown in Figure 2; The functional equation of this relation curve is as follows:
Y?=?0.37501－0.02497InX，?R
2?=?0.98641；
(4) etching glass to be measured: as shown in Figure 3, select for use Φ 100mm * 10mm specification through the quartz glass samples of cerium oxide polishing as glass sample 1 to be measured, adopt 2 pairs of glass samples 1 to be measured of photoresist to carry out mask earlier, central diameter 50mm circle zone not mask as to be measured regional 3, re-use pipettor 4 glass sample 1 to be measured not mask to be measured regional 3 introduce the 10mL etching solutions, take out behind the 1min at interval and clean, accumulative total etching period 10min(etching 10 times repeatedly), use contourgraph to detect glass sample to be measured etch depth each time, and collect the surplus liquid of etching behind the etching reaction each time;
(5) detect the surplus liquid of etching: the pH value to 4.5 of adjusting the surplus liquid of each etching, and it is mixed with isopyknic laccase solution (identical with the laccase solution of step (1) preparation), according to the method for measuring zymoprotein residual activity number percent in the step (2), detect the zymoprotein residual activity number percent in the surplus liquid of this etching then; At last according to the relation curve that obtains in this zymoprotein residual activity percent value and the step (3), calculate under the special etch degree of depth each time the concentration of trace impurity in the optical glass polishing sub-surface damage layer, obtain under etch depth after each etching as shown in Figure 4 and this degree of depth relation curve (being that impurity concentration is along the depth profile curve) of cerium oxide concentration in the quartz glass samples to be measured, finish whole testing process.
Embodiment 2:
The detection method of trace impurity in a kind of optical glass polishing sub-surface damage layer of the present invention as shown in Figure 1 may further comprise the steps:
(1)～(3): the step of present embodiment (1)～(3) are identical with embodiment 1;
(4) etching glass to be measured: as shown in Figure 3, select for use Φ 100mm * 10mm specification through the K9 glass sample of cerium oxide polishing as glass sample 1 to be measured, adopt 2 pairs of glass samples 1 to be measured of photoresist to carry out mask earlier, central diameter 50mm circle zone not mask as to be measured regional 3, re-use pipettor 4 glass sample 1 to be measured not mask to be measured regional 3 introduce the 10mL etching solutions, take out behind the 1min at interval and clean, accumulative total etching period 10min, use contourgraph to detect glass sample to be measured etch depth each time, and collect the surplus liquid of etching behind the etching reaction each time;
(5) detect the surplus liquid of etching: the pH value to 4.5 of adjusting the surplus liquid of each etching, and it is mixed with isopyknic laccase solution (identical with the laccase solution of step (1) preparation), according to the method for measuring zymoprotein residual activity number percent in the step (2), detect the zymoprotein residual activity number percent in the surplus liquid of this etching then; At last according to the relation curve that obtains in this zymoprotein residual activity percent value and the step (3), calculate under the special etch degree of depth each time the concentration of trace impurity in the optical glass polishing sub-surface damage layer, obtain under etch depth after each etching as shown in Figure 5 and this degree of depth relation curve (being that impurity concentration is along the depth profile curve) of cerium oxide concentration in the K9 glass sample to be measured, finish whole testing process.
Claims (8)
1. the detection method of trace impurity in the optical glass polishing sub-surface damage layer may further comprise the steps:
(1) solution preparation: prepare the aqueous solution that contains rare earth ion or rare-earth oxide of a series of variable concentrations, and adjust its pH value; The aqueous solution that this is a series of is mixed with laccase solution respectively, obtains a series of solution example;
(2) measure zymoprotein residual activity number percent: a series of solution example that step (1) is obtained places the water bath with thermostatic control insulation reaction, reaction back obtains zymoprotein activity value in each solution example by measuring the solution optical absorption intensity, obtains the standard enzyme vigor by measuring described laccase solution optical absorption intensity again; According to zymoprotein activity value that has recorded and standard enzyme vigor, obtain the zymoprotein residual activity number percent of each solution example;
(3) matched curve: each when corresponding with it solution example middle rare earth concentration of metal of zymoprotein residual activity percentage of each solution example of measuring according to step (2) simulates the relation curve of zymoprotein residual activity number percent-rare earth metal concentration;
(4) etching glass to be measured: use pipettor on the full surface of glass sample to be measured or at the introducing etching solution in zone local to be measured of mask not, fixed interval is taken out cleaning after the time, detect the etch depth of glass sample to be measured, and collect the surplus liquid of etching behind the etching reaction;
(5) detect the surplus liquid of etching: adjust the pH value of the surplus liquid of described etching, and it is mixed with laccase solution, according to the method for measuring zymoprotein residual activity number percent in the step (2), detect the zymoprotein residual activity number percent in the surplus liquid of this etching then; At last according to the relation curve that obtains in this zymoprotein residual activity percent value and the step (3), calculate under the described etch depth concentration of trace impurity in the optical glass polishing sub-surface damage layer.
2. the detection method of trace impurity in the optical glass polishing sub-surface damage layer according to claim 1, it is characterized in that, the aqueous solution that contains rare earth ion or rare-earth oxide of described a series of variable concentrations comprises the rare earth metal aqueous solution of five kinds of variable concentrations at least, wherein, the mass percent of the rare earth metal aqueous solution of least concentration is lower than 10
-6Ppm, the mass percent of the rare earth metal aqueous solution of maximum concentration is higher than 10
-3Ppm.
3. the detection method of trace impurity is characterized in that in described step (1) and the step (5), the pH value is controlled at 4～6 after adjusting in the optical glass polishing sub-surface damage layer according to claim 1.
4. the detection method of trace impurity in the optical glass polishing sub-surface damage layer according to claim 1, it is characterized in that, mainly formulated in the described laccase solution by laccase, guaiacol substrate and sodium succinate damping fluid, the concentration of described laccase is 50mg/l～100mg/l, and the concentration of described guaiacol substrate is 50ml/l～200ml/l.
5. the detection method of trace impurity is characterized in that in the described step (2), the temperature of water bath with thermostatic control is controlled at 20 ℃～50 ℃ in the optical glass polishing sub-surface damage layer according to claim 1, and the time of insulation reaction is 20min～60min.
6. the detection method of trace impurity is characterized in that in the optical glass according to claim 1 polishing sub-surface damage layer, and the spectrophotometer of selecting for use during described mensuration solution optical absorption intensity is to measure in 400nm～700nm wavelength coverage.
7. according to the detection method of trace impurity in each described optical glass polishing sub-surface damage layer in the claim 1～6, it is characterized in that described rare earth metal is cerium or lanthanum.
8. the detection method of trace impurity in the optical glass polishing sub-surface damage layer according to claim 7 is characterized in that when described rare earth metal was cerium, the functional equation of described relation curve was:
Y?=?0.37501－0.02497InX，?R
2?=?0.98641。
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103163154A (en) * | 2013-02-04 | 2013-06-19 | 西安交通大学 | Characterization method of hard brittle high-precision component sub-surface damage degree |
| CN108181333A (en) * | 2017-12-04 | 2018-06-19 | 南京腾元软磁有限公司 | A kind of process and evaluation method of refined non-crystalline solids alloy three-dimensional reconstruct transmission electron microscope sample |
| CN110617899A (en) * | 2019-09-04 | 2019-12-27 | 河南牧业经济学院 | Solid enzyme type time-temperature indicator and preparation method thereof |
| CN113029855A (en) * | 2021-03-12 | 2021-06-25 | 武汉理工大学 | Analysis method for segregation distribution of quartz crystal lattice impurity elements |
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| CN101949839A (en) * | 2010-09-03 | 2011-01-19 | 西安工业大学 | Device and method for measuring damage of optical surface subsurface layer |
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2011
- 2011-07-11 CN CN 201110192050 patent/CN102288561B/en not_active Expired - Fee Related
Patent Citations (2)
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103163154A (en) * | 2013-02-04 | 2013-06-19 | 西安交通大学 | Characterization method of hard brittle high-precision component sub-surface damage degree |
| CN103163154B (en) * | 2013-02-04 | 2015-05-27 | 西安交通大学 | Characterization method of hard brittle high-precision component sub-surface damage degree |
| CN108181333A (en) * | 2017-12-04 | 2018-06-19 | 南京腾元软磁有限公司 | A kind of process and evaluation method of refined non-crystalline solids alloy three-dimensional reconstruct transmission electron microscope sample |
| CN108181333B (en) * | 2017-12-04 | 2020-04-21 | 南京腾元软磁有限公司 | Process method and evaluation method for refining amorphous solid alloy three-dimensional reconstruction transmission electron microscope sample |
| CN110617899A (en) * | 2019-09-04 | 2019-12-27 | 河南牧业经济学院 | Solid enzyme type time-temperature indicator and preparation method thereof |
| CN113029855A (en) * | 2021-03-12 | 2021-06-25 | 武汉理工大学 | Analysis method for segregation distribution of quartz crystal lattice impurity elements |
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