CN111024534A - Mechanical characterization method for optical glass subsurface damage - Google Patents
Mechanical characterization method for optical glass subsurface damage Download PDFInfo
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- CN111024534A CN111024534A CN201911391458.3A CN201911391458A CN111024534A CN 111024534 A CN111024534 A CN 111024534A CN 201911391458 A CN201911391458 A CN 201911391458A CN 111024534 A CN111024534 A CN 111024534A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/40—Investigating hardness or rebound hardness
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
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- G01N2203/0078—Hardness, compressibility or resistance to crushing using indentation
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Abstract
The invention discloses a mechanical characterization method of optical glass subsurface damage, which comprises the steps of cutting a section vertical to the surface of an optical glass sample, and polishing the section; then etching the polished sample, ultrasonically cleaning and drying; carrying out nano indentation test on the dried sample section, wherein the included angle between the indentation direction and the surface is theta, measuring the indentation hardness and indentation elastic modulus of the section along the depth direction, and recording the depth information of each test point; and finally, determining the subsurface damage depth of the sample by analyzing the gradient change curve of mechanical indexes (hardness and elastic modulus) measured in the section along the depth direction. The invention provides a mechanical characterization method for optical glass subsurface damage, which utilizes a nanometer indentation instrument to test gradient change of mechanical parameters in a damaged layer, and obtains geometric indexes and mechanical indexes of the subsurface damage through one-time test.
Description
Technical Field
The invention relates to a mechanical characterization method for optical glass subsurface damage, in particular to a method for testing optical glass ultra-precision machining subsurface damage based on a nanometer indenter.
Background
The optical glass element is generally obtained by cutting a raw material thereof and then ultraprecision processing (grinding, lapping, polishing, etc.). Damage (cracks, pits, scratches, plastic deformation, residual stress, etc.) inevitably remains on the surface layer of the material during the processing. The damage layer will significantly affect the application properties (optical coefficient, laser damage threshold and frictional wear properties, etc.) of the optical element. Therefore, it is necessary to effectively characterize the sub-surface damage layer of the optical glass so as to optimize the ultra-precision processing technology and improve the processing quality of the optical glass surface.
The subsurface damage layer of the optical glass comprises a crack damage layer and a residual stress layer. At present, the damage degree of the crack is mainly represented by geometric indexes (crack depth and density), and the detection method comprises the following steps: nondestructive testing and damage testing methods. The main means of the nondestructive testing method comprises the following steps: laser confocal scanning microscope, total internal reflection microscope, optical coherence tomography, high frequency ultrasonic scanning and fluorescence microscope; the method for detecting the damage mainly comprises the following steps: angle polishing, cross-section microscopic method, chemical etching method. Aiming at the subsurface damage generated by ultra-precision machining, the detection method is analyzed, so that the detection method of the depth of the crack layer has more alternatives; the depth of the residual stress layer is generally detected by a chemical corrosion method, and the detection result of the method is greatly influenced by the environment. Therefore, the complete subsurface damage information is obtained by combining at least two methods, and the process is complicated and has low efficiency. In addition, the subsurface damage layer of the optical glass is generally characterized by geometric indexes at present, and certain limitations exist in the evaluation of the mechanical properties of the subsurface damage layer of the optical glass.
Disclosure of Invention
The invention aims to provide a mechanical characterization method for subsurface damage of optical glass, which utilizes a nanometer indentation instrument to test the gradient change of mechanical indexes in a damaged layer along with the depth, and obtains the geometric depth and the mechanical property of the subsurface damage through one-time test.
In order to achieve the above purpose, the invention is realized by the following technical scheme:
cutting a section perpendicular to the surface of an optical glass sample;
fixing a sample by using a special clamp and then polishing a section;
putting the polished sample into an acid solution for treatment, and drying after ultrasonic cleaning;
performing nano indentation test on the dried sample section, wherein the included angle between the indentation direction and the surface is theta, and measuring the indentation hardness H of the section along the depth directionITAnd modulus of elasticity for indentation EITRecording the depth information of each test point;
hardness H of indentation measured in analysis sectionITAnd modulus of elasticity for indentation EITAnd determining the subsurface damage depth of the sample along the gradient change curve in the depth direction.
The object of the present invention and the technical problems solved thereby can be further achieved by the following technical measures.
Preferably, in the method for mechanical characterization of subsurface damage of optical glass, the sample profile polishing solutions are Al2O3And CeO 210 wt% of suspension, the grain diameters of the polishing grains are respectively 10 mu m and 1 mu m-3 mu m, and the polishing removal amount is more than 50 mu m.
Preferably, in the mechanical characterization method for the subsurface damage of the optical glass, the acid solution is a mixed solution of hydrofluoric acid and ammonium fluoride, and the ratio of the mixed solution is HF (40 wt%): NH (NH)4F (40 wt%,) -1: 20, etch time 5 min.
Preferably, in the method for mechanical characterization of the subsurface damage of the optical glass, the indentation depth of the nanoindentation test is 250nm to 500nm, and the included angle θ between the indentation direction and the surface is determined by the number of indentations in the damaged layer and the indentation depth, so that the indentation distance is ensured to be greater than 20 times of the indentation depth.
By adopting the technical scheme, the invention has the beneficial effects that: mechanical index (indentation hardness H) in section of sample detected by nanometer indentation instrumentITAnd modulus of elasticity for indentation EIT) Along the gradient change curve in the depth direction, the geometric depth and the mechanical property of the optical glass subsurface damage layer can be measured by one-time test, the measurement efficiency is improved, and meanwhile, a reference basis is provided for the optimization of the processing technology.
The method can be used for characterizing the subsurface damage of the optical glass, can also be applied to the subsurface damage characterization of other brittle materials, and has strong engineering applicability.
Drawings
The invention is further described with reference to the following figures and specific embodiments:
FIG. 1 is a schematic flow chart of the preparation of an optical glass mechanical test sample in the embodiment of the invention;
FIG. 2 is a schematic cross-sectional view of an indentation according to an embodiment of the invention;
FIG. 3 is a graph of indentation hardness as measured by indentation along a depth for an embodiment of the invention;
FIG. 4 is a graph of indentation modulus of elasticity measured by indentation as a function of depth in an embodiment of the invention.
Detailed Description
The above-described scheme is further illustrated below with reference to specific examples.
The mechanical action of the optical glass in abrasive machining generates sub-surface damage mainly comprising cracks. The subsurface damage changes the microstructure of the surface layer of the material, and further changes the mechanical property of the surface layer of the sample. Therefore, the characterizing parameters of the damage layer should include geometric and mechanical indicators. The invention utilizes a nanometer indentation instrument to measure the high resolution of mechanical indexes in a material micro/nanometer scale range, detects the gradient change of the mechanical indexes along the depth in a damaged layer section, further determines the subsurface damage depth through a change curve, and the preparation flow of a test sample is shown in figure 1.
In this embodiment, the mechanical characterization method for the subsurface damage of the optical glass disclosed by the invention is used for characterizing the subsurface damage layer of the K9 glass after being ground by No. 360 carborundum. The method comprises the following steps:
horizontally fixing an optical glass sample on a working platform of a diamond wire cutting machine, and cutting a section vertical to the surface of the sample;
selecting K9 glass with the same size as a polishing accompanying sheet, adhering and fixing the polishing accompanying sheet to the processing surface of a sample to avoid the edge collapse of the processing surface in the polishing process, then fixing the polishing accompanying sheet by using a special fixture, and grinding and polishing the section, wherein the processing medium and the processing time are 10 mu mAl2O33 μm and 1 μm CeO2Polishing for 30min respectively;
after polishingThe sample of (2) was put into HF (40 wt%): NH (NH)4F (40 wt%,) (1: 20) is corroded for 5min in the solution, the chemical corrosion deposition layer is removed, then ultrasonic cleaning is carried out for 10min, the ultrasonic frequency is 50-100 Hz, and the cleaned product is placed into a vacuum drying oven to be dried;
and (3) carrying out nano indentation test on the section of the dried sample, selecting a glass pressure head, adopting a displacement driving mode, measuring one point at intervals of 1 mu m of indentation depth of 250nm and indentation strain rate of 0.05, and ensuring that the indentation distance is more than 20 times of the indentation depth in order to avoid the influence of interference between indentations on the measurement result, wherein theta is set to be 10 degrees. Measuring indentation hardness H of profile along depth directionITAnd modulus of elasticity for indentation EITRecording the depth information of each test point, wherein the indentation schematic diagram is shown in figure 2; obtaining the indentation hardness H measured in the section planeITAnd modulus of elasticity for indentation EITThe gradient profile in the depth direction is shown in fig. 3 and 4. As can be seen from the figure, the hardness HITAnd modulus of elasticity for indentation EITThe subsurface damage depths at which the stabilized values were reached were all 20 μm, and it was thus found that the subsurface damage had substantially the same tendency to affect the hardness and elastic modulus in the damaged layer, and the subsurface damage depth of the available samples was about 20 μm. In order to verify the accuracy of the subsurface damage depth obtained by the characterization method, the subsurface damage depth of the sample is directly measured to be 20.7 microns by an angle method, and the subsurface damage depth are basically the same.
Claims (4)
1. A mechanical characterization method for subsurface damage of optical glass is characterized by comprising the following steps:
cutting a section perpendicular to the surface of an optical glass sample;
fixing a sample by using a special clamp and then polishing a section;
putting the polished sample into an acid solution for treatment, and drying after ultrasonic cleaning;
performing nano indentation test on the dried sample section, wherein the included angle between the indentation direction and the surface is theta, and measuring the indentation hardness H of the section along the depth directionITAnd modulus of elasticity for indentation EITRecording the depth information of each test point;
hardness H of indentation measured in analysis sectionITAnd modulus of elasticity for indentation EITAnd determining the subsurface damage depth of the sample along the gradient change curve in the depth direction.
2. A mechanical characterization method for optical glass sub-surface damage according to claim 1, wherein the sample profile polishing solutions are each Al2O3And CeO210 wt% of suspension, the grain diameters of the polishing grains are respectively 10 mu m and 1 mu m-3 mu m, and the polishing removal amount is more than 50 mu m.
3. The method for mechanical characterization of subsurface damage of optical glass according to claim 1, wherein said acid solution is a mixture of hydrofluoric acid and ammonium fluoride in the ratio of HF (40 wt%): NH4F (40 wt%,) -1: 20, etch time 5 min.
4. The mechanical characterization method for optical glass subsurface damage according to claim 1, wherein the indentation depth of the nano indentation test is 250nm to 500nm, the included angle θ between the indentation direction and the surface is determined by the indentation number and the indentation depth in the damage layer, and the indentation distance is ensured to be greater than 20 times of the indentation depth.
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| CN112414876A (en) * | 2020-11-27 | 2021-02-26 | 郑州磨料磨具磨削研究所有限公司 | Method for rapidly detecting depth of damaged layer of substrate material |
| CN113008917A (en) * | 2021-03-19 | 2021-06-22 | 中国工程物理研究院机械制造工艺研究所 | Macro-micro comprehensive detection method for surface damage of hard and brittle optical crystal |
| CN113640079A (en) * | 2021-07-28 | 2021-11-12 | 昆明理工大学 | Brittle material subsurface damage depth rapid evaluation method based on fracture strength |
| CN113776912A (en) * | 2021-09-16 | 2021-12-10 | 齐鲁工业大学 | Method for rapidly determining chemical stability of medicinal glass |
| CN114002043A (en) * | 2021-09-16 | 2022-02-01 | 西南科技大学 | Method for testing chemical stability of glass based on nano scratches |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112414876A (en) * | 2020-11-27 | 2021-02-26 | 郑州磨料磨具磨削研究所有限公司 | Method for rapidly detecting depth of damaged layer of substrate material |
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| CN113008917A (en) * | 2021-03-19 | 2021-06-22 | 中国工程物理研究院机械制造工艺研究所 | Macro-micro comprehensive detection method for surface damage of hard and brittle optical crystal |
| CN113008917B (en) * | 2021-03-19 | 2022-12-06 | 中国工程物理研究院机械制造工艺研究所 | Macro-micro comprehensive detection method for surface damage of hard and brittle optical crystal |
| CN113640079A (en) * | 2021-07-28 | 2021-11-12 | 昆明理工大学 | Brittle material subsurface damage depth rapid evaluation method based on fracture strength |
| CN113776912A (en) * | 2021-09-16 | 2021-12-10 | 齐鲁工业大学 | Method for rapidly determining chemical stability of medicinal glass |
| CN114002043A (en) * | 2021-09-16 | 2022-02-01 | 西南科技大学 | Method for testing chemical stability of glass based on nano scratches |
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Application publication date: 20200417 |