CN103017713B - Measuring method for damage layer thickness of optical material subsurface - Google Patents
Measuring method for damage layer thickness of optical material subsurface Download PDFInfo
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- CN103017713B CN103017713B CN201210509908.6A CN201210509908A CN103017713B CN 103017713 B CN103017713 B CN 103017713B CN 201210509908 A CN201210509908 A CN 201210509908A CN 103017713 B CN103017713 B CN 103017713B
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Abstract
The invention relates to the technical field of optical precision measurements, particularly relates to a method for measuring a damage layer thickness of a hard brittle optical material subsurface. The method for measuring the damage layer thickness of the hard brittle optical material subsurface utilizes the corrosivity of HF acid to corrode processing samples and base body samples (referring to work pieces which have been completely eliminated the surface damages) under the same conditions, meanwhile marks the corrosion time and the corrosion operation sequence in segmentation. If starting from the n+1 time period, the corrosion rate of the processing samples is equal to that of the base body samples, and then the processing samples can be considered to be corroded to the base body, and to effectively reducing the experiment error accumulation caused by experimental environment factors or multi-step repeated operations, a correction factor Ki is introduced, the corresponding accumulation corrosion depth in n time periods is the damage layer thickness of the surface. The method for measuring the damage layer thickness of the hard brittle optical material subsurface has the advantages of being simple and quick in measuring process, high in measuring accuracy, and low in the requirement for measuring equipment.
Description
Technical field
The present invention relates to technical field of optical precision measurement, especially a measuring method for thickness of subsurface damaged layer of bucky optical material, specifically a kind ofly introduces improving measuring accuracy, eliminating environmental factor and human factor to the measuring method of the optical material sub-surface damage layer thickness that measuring accuracy affects of correction factor.
Background technology
Last century, the seventies rose, and lot of domestic and foreign scientist has carried out the subsurface stratum Damage Evaluation technical research of optical work.Current sub-surface damage evaluation method mainly contains the differential etch of chemical corrosion liquid, angle polishing method, MRF spotting method, cross section microscopy etc.MRF spotting method measures sub-surface damage, form MRF spot by the method for MRF at sample surface, (acid of optical material, alkali can be corroded again by corrosion, such as HF acid), crackle in spot is expanded, make it directly to observe under the microscope, the depth capacity that crackle can occur is demarcated as sub-surface damage layer depth.The differential corrosion rule of chemical corrosion liquid demarcates the sub-surface damage degree of depth of workpiece by sample and matrix in the difference that corrosion rate changes, and its measured value is more realistic in theory.
The measuring accuracy of the differential etch of chemical corrosion liquid not easily ensures, the measuring accuracy of experimental situation factor and testing tool is larger on experimental result impact.MRF spotting method is measured sub-surface damage and is not taken into account by metamorphic layer, so it measures the needs that crackle layer depth can not meet reaction actual conditions completely, the selection of the parameter (degree of depth, position, angle) of polishing spot is larger on experimental result impact.
Summary of the invention
For the above-mentioned defect existing for background technology, the object of this invention is to provide a kind of method measuring sub-surface damage layer thickness, be called chemical corrosion liquid substep etch.The method utilizes chemical mordant to the corrosivity of optical element, by carrying out the corrosion of same experimental situation substep to processing exemplar and matrix exemplar, depth measurement tools is adopted to scan corrosion surface, measurement plane is demarcated the corrosion depth in region, calculate its corrosion rate, introduce the environmental change of adjusted coefficient K i to the difference corrosion stage simultaneously and do suitable correction, improve measuring accuracy, with the damage layer on the sub-surface of the variation tendency indirect calibration optical element of corrosion rate, having can through engineering approaches, the feature that quick, practical, precision is high.
Technical scheme of the present invention is:
Measure a method for thickness of subsurface damaged layer of bucky optical material, in its feature, it comprises the following steps:
(1) preparation of matrix exemplar: the container holding chemical corrosion liquid is placed in isoperibol, is placed in chemical corrosion liquid by matrix exemplar and is no less than 2 hours, guarantees that its sub-surface damage layer is removed completely, obtains matrix exemplar B for comparison;
(2) matrix exemplar B and processing exemplar A is cleaned and dried: the to be detected processed sample A measure-alike with matrix exemplar B length and width and matrix exemplar B is put into supersonic wave cleaning machine at the same time or separately and cleans, take out, put into drying box and dry;
(3) assembly parts of matrix exemplar B and processed sample A are prepared respectively; By the processed sample A to be detected upper surface being attached to plastic base plate parallel with the lower surface of matrix exemplar B through cleaning-drying, the upper surface of plastic base plate is as the reference field measuring corrosion depth; Meanwhile, divide formation two symmetrical region A1 and A2, B1 and B2 respectively at processed sample A to be detected and matrix exemplar B upper surface, respectively touch one of them region with plastics compressing tablet, obtain sample assembly parts, for next step substep corrosion is prepared; The effect of plastics compressing tablet is to stop same sample surface two regions to be corroded simultaneously, above-mentioned two regions are made to carry out substep corrosion, corrosion environment is each time identical, but etching time total separately differs a time period, make in i+1 etching operation, the i-th+1 time, the firstth district corrosion depth and i-th time, the secondth district corrosion depth of a time period first can be corroded, and i-th time, the secondth district, i-th time, corrosion depth in theory with the first district corrosion depth is equal, and actual measured value differs greatly, this causes due to experimental implementation error;
(4) above-mentioned matrix exemplar B and processed sample A assembly parts are placed in the etching solution prepared simultaneously, put into water bath with thermostatic control, make described processed sample A and do not touched the region of covering by plastics compressing tablet in matrix exemplar B upper surface to be emerging in chemical corrosion liquid and to corrode, after corroding a time period, matrix exemplar B and processed sample A assembly parts are taken out, put into supersonic wave cleaning machine to clean and then take out, put into drying box and dry;
(5) measure processed sample A on matrix exemplar B and processed sample A assembly parts and matrix exemplar B respectively with step instrument to be corroded the erosion profile in region, draw the corrosion depth mean value of processed sample A and matrix exemplar B corrosion area respectively, calculate respective average corrosion rate;
(6) remove the plastics compressing tablet on matrix exemplar B and processed sample A assembly parts, they are put into chemical corrosion liquid repetition (4), the burn into cleaning described in (5) step, dry, measurement; Draw the corrosion depth mean value in processed sample A first district, the secondth district and matrix exemplar B first district, the secondth district respectively, calculate respective average corrosion rate;
(7) correction factor is calculated; Introduce the corrosion adjusted coefficient K i of processed sample A, i refers to i-th etching operation; K
1=1, K
2=P
a21/ P
a11, K
3=P
a22/ P
a12k
i=P
a2 (i-1)/ P
a1 (i-1), the actual corrosion depth that processed sample A is corresponding can use formula | P
a1i|=P
a1i× K
irepresent, P
a1ifor the corrosion depth that processed sample A1 region records at i-th etching operation; The correction principle of the corrosion depth in B1 region is the same, namely introduces matrix sample corrosion correction factor C
i, i refers to i-th etching operation, C
1=1, C
2=J
b21/ J
b11, C
3=J
b22/ J
b12c
i=J
b2 (i-1)/ J
b1 (i-1), the actual corrosion depth that matrix exemplar B is corresponding can use formula | J
b1i|=J
b1i× C
irepresent, J
b1ifor the corrosion depth that matrix sample B1 region records at i-th etching operation;
(8) calculating of sub-surface damage layer thickness; When through i+1 etching operation, meet following condition: (1) simultaneously | P
ai| ≠ | J
ai|; (2) | P
ai+1|=| J
ai+1|, then processed sample sub-surface damage layer depth is
namely, within the i-th+1 time etching operation time, the actual corrosion depth in A1 region equals the actual corrosion depth in B1 region, then processed sample sub-surface damage layer depth is the accumulated value of front i corrosion depth.
The present invention utilizes chemical corrosion liquid to the corrosivity of optical element, by carrying out the corrosion of same experimental situation substep to processing exemplar and matrix exemplar, adopt depth measurement tools to scan corrosion surface, measurement plane is demarcated the corrosion depth in region, calculate its corrosion rate.
Invention introduces adjusted coefficient K i, Ki is the different surf zone (2nd district and 1st district) of same sample, (the i-th-1 time etching operation) degree of depth of 2nd district corrosion and the ratio of 1 district's corrosion depth (i-th etching operation), the effect introducing adjusted coefficient K i is, while i-th etching operation is carried out to 1st district, i-1 etching operation is carried out to 2nd district, at this moment the corrosion environment in two regions is the same, while being equivalent to that current corrosion is carried out to the same area, be repeated the etching operation once going up a time period under identical experimental situation simultaneously, the factor of influence of experimental situation to experimental data is drawn from the data of the corrosion depth recorded, i.e. Ki, decrease the impact of change on experimental result of environment, described experimental situation comprises experimental temperature, etchant concentration and experimental implementation.
Described chemical corrosion liquid be HF acid or other can to optical material carry out lose separate corrosive liquid.
In repetition step (4), identical with the time period that processed sample A corrodes to matrix exemplar B, be convenience of calculation, etching time can be unified to be set as 5,10,15 or 20 minutes.
Of the present invention effective:
(1) sample preparation technique is simple, and any region of sample can be selected to test;
(2) quick, sensitive, do not introduce additional sub-surface damage;
(3) testing cost is low, is applicable to large-scale promotion.
Accompanying drawing explanation
Fig. 1 is experimental implementation schematic flow sheet
Fig. 2 is sample assembly parts schematic diagram
Fig. 3 is sample subregion schematic diagram
Fig. 4 processed sample 1 area data correction schematic diagram
Step schematic diagram measured by Fig. 5 three-dimensional appearance instrument
Attrition process glass sample comparison between corrosion schematic diagram before and after Fig. 6 correction
Abundant etching glass sample etches RATES schematic diagram before and after Fig. 7 correction
Embodiment
Below in conjunction with drawings and Examples, the present invention is further illustrated.
Measure a method for thickness of subsurface damaged layer of bucky optical material, it comprises the steps:
(1) configure chemical corrosion liquid, the container holding chemical corrosion liquid is placed in isoperibol; Matrix exemplar is placed in etching solution and is no less than 2 hours, guarantee that its sub-surface damage layer is removed completely, obtain matrix exemplar for comparison;
(2) by processed sample to be detected measure-alike for length and width with put into supersonic wave cleaning machine at the same time or separately through the matrix exemplar that the first step is fully corroded and clean, take out, put into drying box and dry;
(3) sample assembly parts are prepared; By the parallel upper surface being attached to plastic base plate of lower surface through the processed sample to be detected of cleaning-drying and the matrix exemplar through abundant corrosion, the upper surface of plastic base plate is as the reference field measuring corrosion depth; Meanwhile, divide two symmetrical regions respectively at processed sample to be detected with through the matrix exemplar upper surface of fully corrosion, respectively touch one of them region with plastics compressing tablet, obtain sample assembly parts, for next step substep corrosion is prepared;
(4) effect of plastics compressing tablet is to stop same sample surface two regions to be corroded simultaneously, above-mentioned two regions are made to carry out substep corrosion (same corrosion environment, etching time differs a time period), make in i+1 etching operation, 1st district (first having corroded a time period) the i-th+1 time corrosion depth and i-th time, 2nd district corrosion depth can be obtained, and i-th time, 2nd district, i-th time, corrosion depth in theory with 1 district corrosion depth is equal, and actual measured value differs greatly, this causes due to experimental implementation error;
(5) above-mentioned sample assembly parts are placed in the etching solution prepared, put into water bath with thermostatic control, make described processed sample to be detected and do not touched the region of covering by plastics compressing tablet in the matrix exemplar upper surface of fully corrosion to be emerging in corrosive liquid and to corrode, after corroding a time period, sample assembly parts are taken out, put into supersonic wave cleaning machine to clean and then take out, put into drying box and dry;
(6) measure processed sample to be detected on sample assembly parts and matrix exemplar respectively with step instrument to be corroded the erosion profile in region, draw the corrosion depth mean value of processed sample to be detected and matrix exemplar corrosion area respectively, calculate respective average corrosion rate;
(7) the plastics compressing tablet on sample assembly parts is removed, to processed sample to be detected with through the burn into cleaning of matrix exemplar upper surface also described in uncorroded region repetition (5), (6) step of abundant corrosion, dry, measurement; Draw the corrosion depth mean value in processed sample to be detected and matrix exemplar first district, the secondth district respectively, calculate respective average corrosion rate;
(8) correction factor is calculated.Introduce processed sample corrosion adjusted coefficient K i, i refers to i-th etching operation.K
1=1, K
2=P
a21/ P
a11, K
3=P
a22/ P
a12k
i=P
a2 (i-1)/ P
a1 (i-1), the actual corrosion depth of processing exemplar (A group) correspondence can use formula | P
a1i|=P
a1i× K
irepresent, P
a1ifor the corrosion depth that processed sample A1 region records at i-th etching operation, the correction principle of the corrosion depth in B1 district is the same, namely introduces matrix sample corrosion correction factor C
i, i refers to i-th etching operation.C
1=1, C
2=J
b21/ J
b11, C
3=J
b22/ J
b12c
i=J
b2 (i-1)/ J
b1 (i-1), the actual corrosion depth that matrix exemplar (B group) is corresponding can use formula | J
b1i|=J
b1i× C
irepresent, J
b1ifor the corrosion depth that matrix sample B1 region records at i-th etching operation.
(9) calculating of sub-surface damage layer thickness.When through i+1 etching operation, meet following condition: (1) simultaneously | P
ai| ≠ | J
ai|; (2) | P
ai+1|=| J
ai+1|, then processed sample sub-surface damage layer depth is
namely, within the i-th+1 time etching operation time, the actual corrosion depth in A1 region equals the actual corrosion depth (being equal to corrosion rate equal) in B1 region, then processed sample sub-surface damage layer depth is the accumulated value of front i corrosion depth.
In order to effectively reduce the experiment accumulated error caused because of experimental situation factor and multistep repetitive operation, introduce adjusted coefficient K i, Ki is the different surf zone (2nd district and 1st district) of same sample, at the ratio of 2 districts' corrosion (the i-th-1 time etching operation) degree of depth and 1 district's corrosion depth (i-th etching operation).The effect introducing adjusted coefficient K i is, while i-th etching operation is carried out to 1st district, i-1 etching operation is carried out to 2nd district, at this moment the corrosion environment in two regions is the same, while being equivalent to that current corrosion is carried out to the same area, be repeated the etching operation once going up a time period under identical experimental situation simultaneously, experimental situation (experimental temperature is drawn from the data of the corrosion depth recorded, etchant concentration, experimental implementation etc.) factor of influence to experimental data, i.e. Ki, decreases the impact of change on experimental result of environment.
Using HF acid-etching solution as chemical corrosion liquid, the invention will be further described below.As shown in Figure 1, configuration body HF etching solution HF(40%wt) and NH4F (40%wt) ratio be 1:20, the beaker holding HF etching solution is placed in water bath with thermostatic control, and to set bath temperature be 25 DEG C.By matrix exemplar under isoperibol, be placed in corrosive liquid 2 hours, guarantee that its sub-surface damage layer is removed completely.Supersonic wave cleaning machine cleaning 5 minutes is put into by processed sample with through the matrix exemplar (length and width are measure-alike) of fully corrosion, then take out, put into drying box and dry test specimen, Vltrasonic device is the Gen2500W of CREST company, frequency of operation is 68KHz, has scanning ultrasound functions.Prepare sample assembly parts as shown in Figure 2 and Figure 3.First, first one piece of 60mm × 120mm × 10mm plastic base plate is prepared; And calibration measurements datum line and reference point thereon; Plastic base plate sticks processing exemplar A(and is divided into A1 and A2 two regions) and matrix exemplar B, be divided into B1 and B2 two regions equally; Be attached on A2, B2 region with one piece of 100mm × 100mm × 25mm plastics compressing tablet, cover A2, B2 region completely.Be placed in by processed sample with through the matrix exemplar of fully corrosion the corrosive liquid prepared, put into water bath with thermostatic control, temperature 25 DEG C.Corroding a time period (can be 5,10,15 or 20 minutes, but once after determining a time period, the identical time period must be used than in matrix exemplar B and processed sample A corrosion measurement process to same, so that analytical calculation) after, take out, put into supersonic wave cleaning machine cleaning 5 minutes, then take out, put into drying box and dry test specimen.With step instrument (vertical precision 0.1nm) according to the datum line demarcated in abovementioned steps, processed sample A1 region and the matrix exemplar B1 region erosion profile on datum line is measured respectively with step instrument scanning datum line, draw corrosion depth mean value respectively, calculate respective average corrosion rate.Removing plastics compressing tablet, repeat aforesaid corrosion step, measure processed sample A1, A2 region and matrix exemplar B1, B2 region erosion profile on datum line respectively with step instrument scanning datum line, draw corrosion depth mean value respectively, calculate respective average corrosion rate.
The measurement of corrosion depth (step) is carried out on NanoMap-500LS type three-dimensional surface topography instrument.After having demarcated measurement " zero point ", use three-dimensional surface topography instrument directly to measure the difference in height of etch planes and measuring basis, the corrosion depth of each experimental implementation can have been obtained.In order to reduce to measure the error with the degree of depth zero point, choose the mean value of etch planes and reference plane height to calculate corrosion depth.
Repeat corrosion and measure processed sample A1, A2 region and matrix exemplar B1, B2 region, record measurement data, according to shown in Fig. 4 and the front data correction computing formula chatted, 1. 2. 3. 4. 5. represent corrosion step in Fig. 4, draw actual corrosion depth and the corrosion rate of processed sample A1 region and each etching time section of matrix sample B1 region.Sub-surface damage layer thickness is calculated according to aforesaid sub-surface damage layer thickness equations.
As shown in Figure 6, before correction, the time dependent rule of B1 corrosion rate not obviously (Fig. 7), after revising, reduces measuring error, and the actual corrosion rate change of B1 is mild.Comparison diagram 6 and Fig. 7, can assert, A1 sample and the corrosion rate of B1 sample etches after 20 minutes basically identical, illustrate: corrode after 20 minutes, the corrosion of A1 sample enters body portion, and now, total corrosion depth is sub-surface damage layer depth.
The part that the present invention does not relate to prior art that maybe can adopt all same as the prior art is realized.
Claims (3)
1. measure a method for thickness of subsurface damaged layer of bucky optical material, in its feature, it comprises the following steps:
(1) preparation of matrix exemplar: the container holding chemical corrosion liquid is placed in isoperibol, is placed in chemical corrosion liquid by matrix exemplar and is no less than 2 hours, guarantees that its sub-surface damage layer is removed completely, obtains matrix exemplar B for comparison;
(2) matrix exemplar B and processed sample A is cleaned and dried: the to be detected processed sample A measure-alike with matrix exemplar B length and width and matrix exemplar B is put into supersonic wave cleaning machine at the same time or separately and cleans, take out, put into drying box and dry;
(3) assembly parts of matrix exemplar B and processed sample A are prepared respectively; By the processed sample A to be detected upper surface being attached to plastic base plate parallel with the lower surface of matrix exemplar B through cleaning-drying, the upper surface of plastic base plate is as the reference field measuring corrosion depth; Meanwhile, divide formation two symmetrical region A1 and A2, B1 and B2 respectively at processed sample A to be detected and matrix exemplar B upper surface, respectively touch one of them region with plastics compressing tablet, obtain sample assembly parts, for next step substep corrosion is prepared; The effect of plastics compressing tablet is to stop same sample surface two regions to be corroded simultaneously, above-mentioned two regions are made to carry out substep corrosion, corrosion environment is each time identical, but etching time total separately differs a time period, make in i+1 etching operation, the i-th+1 time, the firstth district corrosion depth and i-th time, the secondth district corrosion depth of a time period first can be corroded, and i-th time, the secondth district, i-th time, corrosion depth in theory with the first district corrosion depth is equal, and actual measured value differs greatly, this causes due to experimental implementation error;
(4) above-mentioned matrix exemplar B and processed sample A assembly parts are placed in the etching solution prepared simultaneously, put into water bath with thermostatic control, make described processed sample A and do not touched the region of covering by plastics compressing tablet in matrix exemplar B upper surface to be emerging in etching solution and to corrode, after corroding a time period, matrix exemplar B and processed sample A assembly parts are taken out, put into supersonic wave cleaning machine to clean and then take out, put into drying box and dry;
(5) measure processed sample A on matrix exemplar B and processed sample A assembly parts and matrix exemplar B respectively with step instrument to be corroded the erosion profile in region, draw the corrosion depth mean value of processed sample A and matrix exemplar B corrosion area respectively, calculate respective average corrosion rate;
(6) remove the plastics compressing tablet on matrix exemplar B and processed sample A assembly parts, they are put into chemical corrosion liquid repetition (4), the burn into cleaning described in (5) step, dry, measurement; Draw the corrosion depth mean value in processed sample A first district, the secondth district and matrix exemplar B first district, the secondth district respectively, calculate respective average corrosion rate;
(7) correction factor is calculated; Introduce the corrosion adjusted coefficient K of processed sample A
i, i refers to i-th etching operation; K
1=1, K
2=P
a21/ P
a11, K
3=P
a22/ P
a12k
i=P
a2 (i-1)/ P
a1 (i-1), the actual corrosion depth that processed sample A is corresponding can use formula | P
a1i|=P
a1i× K
irepresent, P
a1ifor the corrosion depth that processed sample A1 region records at i-th etching operation; The correction principle of the corrosion depth in B1 region is the same, namely introduces matrix sample corrosion correction factor C
i, i refers to i-th etching operation, C
1=1, C
2=J
b21/ J
b11, C
3=J
b22/ J
b12c
i=J
b2 (i-1)/ J
b1 (i-1), the actual corrosion depth that matrix exemplar B is corresponding can use formula | J
b1i|=J
b1i× C
irepresent, J
b1ifor the corrosion depth that matrix sample B1 region records at i-th etching operation;
(8) calculating of sub-surface damage layer thickness; When through i+1 etching operation, meet following condition: (1) simultaneously | P
ai| ≠ | J
ai|; (2) | P
ai+1|=| J
ai+1|, then processed sample sub-surface damage layer depth is
namely, within the i-th+1 time etching operation time, the actual corrosion depth in A1 region equals the actual corrosion depth in B1 region, then processed sample sub-surface damage layer depth is the accumulated value of front i corrosion depth.
2. the method for measurement thickness of subsurface damaged layer of bucky optical material according to claim 1, it is characterized in that described chemical corrosion liquid be HF acid or other can to optical material carry out lose separate corrosive liquid.
3. the method for measurement thickness of subsurface damaged layer of bucky optical material according to claim 1, it is characterized in that in step (4) identical with the time period that processed sample A corrodes to matrix exemplar B, for convenience of calculation, etching time section is unified is set as 5,10,15 or 20 minutes.
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| CN104132944B (en) * | 2014-07-11 | 2017-02-15 | 西安交通大学 | Method for detecting subsurface damage degree characterization parameters of spherical optical element |
| CN104792291A (en) * | 2015-04-27 | 2015-07-22 | 中国工程物理研究院化工材料研究所 | Method for precisely measuring thickness of thin macromolecular coating layer |
| CN107907086B (en) * | 2017-11-15 | 2019-07-23 | 西安交通大学 | Chemical etching measurement method, auxiliary experiment device and the test method of optical element sub-surface damage |
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| CN108534732B (en) * | 2018-03-27 | 2020-01-17 | 中国建筑材料科学研究总院有限公司 | Method for detecting thickness of subsurface damage layer of silicate glass |
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| CN110793986A (en) * | 2019-10-14 | 2020-02-14 | 中国电子科技集团公司第十一研究所 | Method for testing depth of damage layer of InSb wafer |
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