CN108534732B - Method for detecting thickness of subsurface damage layer of silicate glass - Google Patents
Method for detecting thickness of subsurface damage layer of silicate glass Download PDFInfo
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- CN108534732B CN108534732B CN201810259422.9A CN201810259422A CN108534732B CN 108534732 B CN108534732 B CN 108534732B CN 201810259422 A CN201810259422 A CN 201810259422A CN 108534732 B CN108534732 B CN 108534732B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B21/00—Measuring arrangements or details thereof, where the measuring technique is not covered by the other groups of this subclass, unspecified or not relevant
- G01B21/02—Measuring arrangements or details thereof, where the measuring technique is not covered by the other groups of this subclass, unspecified or not relevant for measuring length, width, or thickness
- G01B21/08—Measuring arrangements or details thereof, where the measuring technique is not covered by the other groups of this subclass, unspecified or not relevant for measuring length, width, or thickness for measuring thickness
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B1/00—Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes
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Abstract
The invention relates to a method for detecting the thickness of a damaged layer on the subsurface of silicate glass, which comprises the following steps: cutting an inclined plane of a silicate glass sample, wherein the inclination angle alpha is an included angle between the inclined plane and a plane, and cleaning and ultrasonically treating; polishing, cleaning and ultrasonically treating the inclined plane; performing acid-alkali-acid treatment on the polished inclined plane, cleaning, performing ultrasonic dehydration, and drying; reducing the dried sample at high temperature, cooling, measuring the length L of the damaged area on the inclined plane, and calculating the thickness D of the damaged layer as L multiplied by sin alpha by taking the boundary line of the plane and the inclined plane as a starting point and the boundary line of the crack area and the crack-free area on the inclined plane as an end point. The method is suitable for detecting the thickness of the sub-surface damage layer of the silicate glass, has high detection precision and can realize engineering application.
Description
Technical Field
The invention relates to a method for detecting the thickness of a subsurface damaged layer of an optical element, in particular to a method for detecting the thickness of a subsurface damaged layer of silicate glass.
Background
Generally, due to the properties of glass, a certain degree of damage is caused to a subsurface by traditional processing processes such as cutting, grinding, polishing and the like, and the existence of a damaged layer can cause the performance and the service life of the glass to be reduced in subsequent use. As another example, in laser driver design, the laser damage threshold of optical elements including optical materials and optical films is one of the key design criteria, and the laser damage threshold is not only related to optical films and material defects, but also affected by subsurface damage introduced by the optical manufacturing process, and is likely to be the source of laser damage to the elements. Therefore, it is necessary to detect the subsurface damage layer, optimize the processing parameters and the process route by taking the detection as a reference, and improve the quality of the processed surface. The sub-surface damage layer includes cracks, residual stress and the like, and the detection technology of the sub-surface damage layer can be divided into destructive detection and non-destructive detection according to whether the sample is damaged or not. The destructive detection method can partially or completely destroy the sample in the detection process so as to display the detected damage on the surface, and then a required damage detection result is obtained through a proper microscopic observation technology. In the prior art, the subsurface cracks are exposed and amplified based on chemical etching, the appearance of the cracks at different positions on a section is measured by using a roughness measuring tool or a profile gauge, and the thickness of the subsurface damage layer of a sample is calculated. The problem with this approach is that the microscopic cracks and residual stresses are not amplified during processing and cannot be detected with roughness measuring tools or profilometers.
The principle of nondestructive detection is to detect the abnormality and defect in the material or structure by using the reaction change of the material to heat, sound, light, electricity, magnetism and the like caused by the defect in the material, and the method has the advantages of rapidness, convenient operation and the like, and particularly has the advantages in the aspect of detection of plastic damage such as dislocation, a phase change layer, residual stress and the like. However, the research on the response mechanism of the detection medium such as sound wave, optical field, magnetic field, ray and the like to the micron-scale defect is still incomplete, and the detection of the shape and position of the micron-scale crack is difficult.
Disclosure of Invention
The invention mainly aims to provide a novel method for detecting the thickness of a subsurface damaged layer of silicate glass, and the technical problem to be solved is to ensure that the detection precision is high, so that the method is more practical.
The purpose of the invention and the technical problem to be solved are realized by adopting the following technical scheme. The invention provides a method for detecting the thickness of a damaged layer on the subsurface of silicate glass, which comprises the following steps:
cutting an inclined plane of a silicate glass sample, wherein the inclination angle alpha is an included angle between the inclined plane and a plane, and cleaning and ultrasonically treating;
polishing, cleaning and ultrasonically treating the inclined plane;
performing acid-alkali-acid treatment on the polished inclined plane, cleaning, performing ultrasonic dehydration, and drying;
reducing the dried sample at high temperature, cooling, measuring the length L of the damaged area on the inclined plane, and calculating the thickness D of the damaged layer as L multiplied by sin alpha by taking the boundary line of the plane and the inclined plane as a starting point and the boundary line of the crack area and the crack-free area on the inclined plane as an end point.
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 detecting the thickness of the sub-surface damage layer of silicate glass, the tilt angle α is 160-175 °.
Preferably, the method for detecting the thickness of the damaged layer on the subsurface of the silicate glass is implemented, wherein the frequency of the ultrasonic wave is 40-80 Hz.
Preferably, in the method for detecting the thickness of the damaged layer on the sub-surface of the silicate glass, the polishing solution is CeO2Or Fe2O3The suspension liquid has a suspension liquid concentration of 200-400g/L, the grain diameter of the polishing grains is less than or equal to 1 μm, and the polishing removal amount is more than 50 μm.
Preferably, the method for detecting the thickness of the subsurface damaged layer of the silicate glass comprises the following steps: the sample is stirred in hydrofluoric acid solution, cleaned, sonicated in sodium hydroxide solution, cleaned, and stirred in hydrofluoric acid solution.
Preferably, in the method for detecting the thickness of the damaged layer on the sub-surface of the silicate glass, the concentration of the hydrofluoric acid solution is 2 to 10 wt%.
Preferably, the method for detecting the thickness of the damaged layer on the subsurface of the silicate glass is characterized in that the concentration of the sodium hydroxide solution is 0.5-2 wt%, and the temperature of the sodium hydroxide solution is 40-60 ℃.
Preferably, in the method for detecting the thickness of the damaged layer on the subsurface of the silicate glass, the drying temperature is 90-100 ℃, and the drying time is 5-15 min.
Preferably, in the method for detecting the thickness of the subsurface damaged layer of silicate glass, the temperature of the high-temperature reduction is 350-.
By the technical scheme, the method for detecting the thickness of the subsurface damage layer of the silicate glass at least has the following advantages:
according to the invention, an angle polishing method is adopted to amplify the damaged layer, so that the measurement error is smaller; polishing by adopting polishing solution with a small particle size so as to facilitate observation of the inclined plane of the sample without adding a new damage layer; the method of acid-alkali-acid repeated etching is adopted to ensure that the sample and the corrosive liquid fully react and most cracks are exposed; the superfine microcracks and residual stress areas of the damaged layer are shown in a high-temperature reduction mode in a reducing atmosphere; the surface damage can be obviously exposed after treatment, and the observation and the measurement can be carried out by using a common optical microscope. The method is suitable for detecting the thickness of the sub-surface damage layer of the silicate glass, has high detection precision and can realize engineering application.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to implement them in accordance with the contents of the description, the following detailed description is given with reference to the preferred embodiments of the present invention and the accompanying drawings.
Drawings
FIG. 1 is a schematic diagram of the bevel of a silicate glass sample.
Detailed Description
To further illustrate the technical means and effects of the present invention for achieving the predetermined objects, the following detailed description will be given to the specific implementation, structure, features and effects of the method for detecting the thickness of the damaged layer on the sub-surface of silicate glass according to the present invention with reference to the accompanying drawings and preferred embodiments. In the following description, different "one embodiment" or "an embodiment" refers to not necessarily the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
The invention provides a method for detecting the thickness of a damaged layer on the subsurface of silicate glass, which comprises the following steps:
cutting an inclined plane on a silicate glass sample by using a cutting machine, wherein the inclined angle alpha is an included angle between the inclined plane and a plane, washing cutting oil and cutting particles on the surface of the sample by using deionized water, and then placing the sample in absolute ethyl alcohol for ultrasonic cleaning for 10-20min at the ultrasonic frequency of 40-80 Hz;
polishing the inclined plane by using a polishing machine, wherein a polishing medium is fluid polishing liquid, a damage layer with a removal amount larger than that of the inclined plane is removed by polishing, the polishing liquid and polishing particles on the surface of the sample are washed clean by using deionized water, and then the sample is placed in absolute ethyl alcohol for ultrasonic cleaning, wherein the ultrasonic frequency is 40-80Hz, and the cleaning time is 10-20 min;
and (3) performing acid-alkali-acid treatment on the polished inclined plane: placing the sample on a polytetrafluoroethylene fixture, immersing the sample and the polytetrafluoroethylene fixture together in 2-10 wt% hydrofluoric acid solution, placing a container containing the sample and hydrofluoric acid on a stirrer, and stirring for 10-60 min. Washing with deionized water after etching to remove residual acid liquor; then putting the sample and the clamp into 0.5-2 wt% NaOH solution, wherein the solution temperature is 40-60 ℃, and cleaning with ultrasonic wave, the ultrasonic frequency is 40-80Hz, and the cleaning time is 5-15min, so as to remove the reaction product of HF acid and the sample, and facilitate the reaction to continue; after cleaning, the stirring process is repeated in HF acid again, and the parameters are the same as those of the former process, so that the damaged part and the HF acid can fully react. And after etching, cleaning the surface and the interior of the sample with deionized water, and then putting the sample into isopropanol for ultrasonic cleaning at the ultrasonic frequency of 40-80Hz for 5-15min to dehydrate the sample. Drying in a drying oven at 90-100 deg.C for 5-15min after dehydration. After the treatment, the HF acid reacts with the sample, the damaged area presents cracks due to high reaction speed, and most of cracks in the sample processing damaged layer are shown after the acid-alkali-acid repeated treatment.
And (3) placing the dried sample in an atmosphere reduction furnace, raising the temperature in the furnace to 350-500 ℃, introducing a reduction atmosphere, and reacting gas with network gap ions in the glass body, wherein stress exists in the damage area due to non-uniform reaction speed, and the damage area is shown in a form of microcracks under the action of the stress. After reduction for 2-5h, stopping ventilation to cool the furnace, preferably adopting gradient cooling during cooling, slowly cooling to about 300 ℃ and then naturally cooling. After the high-temperature treatment in the reducing atmosphere, the superfine microcracks and residual stress areas of the sample processing damage layer are also shown. The length L of the damaged area on the bevel, where the bevel is divided into a cracked area 1 and a crack-free area 2 as shown in fig. 1, was measured, and the thickness D of the damaged layer was calculated as L × sin α, starting from the boundary line between the plane and the bevel and ending at the boundary line between the cracked area and the crack-free area on the bevel.
Preferably, the tilt angle α is 160-175 °.
Preferably, the polishing solution is selected for polishing, and the polishing solution is CeO2Or Fe2O3The suspension liquid has a suspension liquid concentration of 200-400g/L, the grain diameter of the polishing grains is less than or equal to 1 μm, and the polishing removal amount is more than 50 μm.
Preferably, the reducing atmosphere is hydrogen, the flow rate of the hydrogen is 0.01-0.1L/min, and the pressure of the hydrogen is 0.01-0.2 MPa.
Example 1
The invention provides a method for detecting the thickness of a damaged layer on the subsurface of silicate glass, which comprises the following steps:
cutting an inclined plane on a silicate glass sample by using a cutting machine, wherein the inclination angle alpha is 175 degrees, washing cutting oil and cutting particles on the surface of the sample by using deionized water, and then placing the sample in absolute ethyl alcohol for ultrasonic cleaning for 15min, wherein the ultrasonic frequency is 40 Hz;
polishing the inclined plane by a polishing machine, wherein the polishing medium is fluid polishing solution, and the polishing solution is CeO2Suspension with a suspension concentration of 200g/L, CeO2The grain size of the grains is not more than 1 mu m, the removal amount of polishing is 100 mu m, the polishing solution and the polishing grains on the surface of the sample are washed clean by deionized water, and then the sample is placed in absolute ethyl alcohol for ultrasonic cleaning, the ultrasonic frequency is 40Hz, and the cleaning time is 10 min;
and (3) performing acid-alkali-acid treatment on the polished inclined plane: the sample was placed on a teflon holder and immersed together in a 5 wt% hydrofluoric acid solution, and the container holding the sample and hydrofluoric acid was placed on a stirrer and stirred for 40 min. Washing with deionized water after etching to remove residual acid liquor; then putting the sample and the clamp into 1 wt% NaOH solution, wherein the solution temperature is 40 ℃, and cleaning with ultrasonic wave, the ultrasonic frequency is 40Hz, and the cleaning time is 10min, so as to remove the reaction product of HF acid and the sample, and facilitate the reaction to continue; after cleaning, the stirring process is repeated in HF acid again, and the parameters are the same as those of the former process, so that the damaged part and the HF acid can fully react. And after etching, cleaning the surface and the interior of the sample with deionized water, and then putting the sample into isopropanol for ultrasonic cleaning at an ultrasonic frequency of 40Hz for 10min to dehydrate the sample. Drying in a drying oven at 95 deg.C for 15min after dehydration.
And (3) placing the dried sample in an atmosphere reduction furnace, raising the temperature in the furnace to 450 ℃, and then introducing hydrogen, wherein the hydrogen flow rate is 0.01L/min, the hydrogen pressure is 0.05MPa, and the reaction time is 3 h. And after the reaction is finished, stopping introducing air to cool the furnace, and naturally cooling after the temperature is reduced to about 300 ℃ for 1 h. After the high-temperature treatment in the reducing atmosphere, the superfine microcracks and residual stress areas of the sample processing damage layer are also shown. And measuring the length L of the damaged area on the inclined plane, wherein the length L takes the boundary line of the plane and the inclined plane as a starting point, and the boundary line of the crack area and the crack-free area on the inclined plane as an end point, and calculating the thickness D of the damaged layer to be L multiplied by sin alpha.
Example 2
The invention provides a method for detecting the thickness of a damaged layer on the subsurface of silicate glass, which comprises the following steps:
cutting an inclined plane on a silicate glass sample by using a cutting machine, wherein the inclination angle alpha is 165 degrees, washing cutting oil and cutting particles on the surface of the sample by using deionized water, and then placing the sample in absolute ethyl alcohol for ultrasonic cleaning for 10min, wherein the ultrasonic frequency is 40 Hz;
polishing the inclined plane by a polishing machine, wherein the polishing medium is fluid polishing liquid, and the polishing liquid is Fe2O3Suspension with a suspension concentration of 400g/L and Fe2O3The grain size of the grains is not more than 1 mu m, the removal amount of polishing is 80 mu m, the polishing solution and the polishing grains on the surface of the sample are washed clean by deionized water, and then the sample is placed in absolute ethyl alcohol for ultrasonic cleaning, the ultrasonic frequency is 80Hz, and the cleaning time is 15 min;
and (3) performing acid-alkali-acid treatment on the polished inclined plane: the sample was placed on a teflon holder and immersed in a 10 wt% hydrofluoric acid solution together, and the container holding the sample and hydrofluoric acid was placed on a stirrer and stirred for 20 min. Washing with deionized water after etching to remove residual acid liquor; then putting the sample and the clamp into 0.5 wt% NaOH solution, wherein the solution temperature is 60 ℃, and cleaning by ultrasonic waves with the ultrasonic frequency of 80Hz for 15min to remove products generated by reaction of HF acid and the sample, so that the reaction is convenient to continue; after cleaning, the stirring process is repeated in HF acid again, and the parameters are the same as those of the former process, so that the damaged part and the HF acid can fully react. And after etching, using deionized water to clean the surface and the residual corrosive liquid inside the sample, and then placing the sample into isopropanol to carry out ultrasonic cleaning, wherein the ultrasonic frequency is 80Hz, and the cleaning time is 8min, so that the sample is dehydrated. Drying in a drying oven at 100 deg.C for 10 min.
And (3) placing the dried sample in an atmosphere reduction furnace, raising the temperature in the furnace to 500 ℃, and then introducing hydrogen, wherein the hydrogen flow rate is 0.1L/min, the hydrogen pressure is 0.1MPa, and the reaction time is 2 h. And after the reaction is finished, stopping introducing air to cool the furnace, and naturally cooling after cooling to about 300 ℃ for 2 h. After the high-temperature treatment in the reducing atmosphere, the superfine microcracks and residual stress areas of the sample processing damage layer are also shown. And measuring the length L of the damaged area on the inclined plane, wherein the length L takes the boundary line of the plane and the inclined plane as a starting point, and the boundary line of the crack area and the crack-free area on the inclined plane as an end point, and calculating the thickness D of the damaged layer to be L multiplied by sin alpha.
Example 3
The invention provides a method for detecting the thickness of a damaged layer on the subsurface of silicate glass, which comprises the following steps:
cutting an inclined plane on a silicate glass sample by using a cutting machine, wherein the inclination angle alpha is 160 degrees, washing cutting oil and cutting particles on the surface of the sample by using deionized water, and then placing the sample in absolute ethyl alcohol for ultrasonic cleaning for 15min, wherein the ultrasonic frequency is 80 Hz;
polishing the inclined plane by a polishing machine, wherein the polishing medium is fluid polishing liquid, and the polishing liquid is Fe2O3Suspension with a suspension concentration of 300g/L and Fe2O3The grain size of the grains is not more than 1 mu m, the removal amount of polishing is 80 mu m, the polishing solution and the polishing grains on the surface of the sample are washed clean by deionized water, and then the sample is placed in absolute ethyl alcohol for ultrasonic cleaning, the ultrasonic frequency is 80Hz, and the cleaning time is 15 min;
and (3) performing acid-alkali-acid treatment on the polished inclined plane: the sample was placed on a teflon holder and immersed together in a 5 wt% hydrofluoric acid solution, and the container holding the sample and hydrofluoric acid was placed on a stirrer and stirred for 50 min. Washing with deionized water after etching to remove residual acid liquor; then putting the sample and the clamp into 1 wt% NaOH solution, wherein the solution temperature is 50 ℃, and cleaning with ultrasonic wave, the ultrasonic frequency is 80Hz, and the cleaning time is 10min, so as to remove the reaction product of HF acid and the sample, and facilitate the reaction to continue; after cleaning, the stirring process is repeated in HF acid again, and the parameters are the same as those of the former process, so that the damaged part and the HF acid can fully react. And after etching, using deionized water to clean the surface and the residual corrosive liquid inside the sample, and then placing the sample into isopropanol to carry out ultrasonic cleaning, wherein the ultrasonic frequency is 80Hz, and the cleaning time is 8min, so that the sample is dehydrated. Drying at 90 deg.C for 10 min.
And (3) placing the dried sample in an atmosphere reduction furnace, raising the temperature in the furnace to 400 ℃, and then introducing hydrogen, wherein the hydrogen flow rate is 0.05L/min, the hydrogen pressure is 0.1MPa, and the reaction time is 4 h. And after the reaction is finished, stopping introducing air to cool the furnace, and naturally cooling after cooling to about 300 ℃ within 1.5 h. After the high-temperature treatment in the reducing atmosphere, the superfine microcracks and residual stress areas of the sample processing damage layer are also shown. And measuring the length L of the damaged area on the inclined plane, wherein the length L takes the boundary line of the plane and the inclined plane as a starting point, and the boundary line of the crack area and the crack-free area on the inclined plane as an end point, and calculating the thickness D of the damaged layer to be L multiplied by sin alpha.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiment according to the technical spirit of the present invention are still within the scope of the technical solution of the present invention.
Claims (5)
1. A method for detecting the thickness of a damaged layer on the sub-surface of silicate glass is characterized by comprising the following steps:
cutting an inclined plane of a silicate glass sample, wherein the inclination angle alpha is an included angle between the inclined plane and a plane, and cleaning and ultrasonically treating;
polishing, cleaning and ultrasonically treating the inclined plane;
performing acid-alkali-acid treatment on the polished inclined plane, cleaning, performing ultrasonic dehydration, and drying; the acid-base-acid treatment comprises the following steps: stirring and cleaning a sample in a hydrofluoric acid solution, performing ultrasonic treatment in a sodium hydroxide solution, cleaning, and stirring in the hydrofluoric acid solution; the concentration of the hydrofluoric acid solution is 2-10 wt%, the concentration of the sodium hydroxide solution is 0.5-2 wt%, and the temperature of the sodium hydroxide solution is 40-60 ℃;
reducing the dried sample at high temperature, cooling, measuring the length L of a damaged area on the inclined plane, and calculating the thickness D of the damaged layer as L multiplied by sin alpha by taking the boundary line of a plane and the inclined plane as a starting point and the boundary line of a crack area and a crack-free area on the inclined plane as an end point; the temperature of the high-temperature reduction is 350-500 ℃, the reduction time is 2-5h, the reduction atmosphere is hydrogen, the flow rate of the hydrogen is 0.01-0.1L/min, and the pressure of the hydrogen is 0.01-0.2 MPa.
2. The method as claimed in claim 1, wherein the tilt angle α is 175 ° and 160 °.
3. The method for detecting the thickness of the damaged layer on the subsurface of the silicate glass according to claim 1, wherein the frequency of the ultrasonic wave is 40-80 Hz.
4. The method for detecting the thickness of the damaged layer on the sub-surface of the silicate glass as claimed in claim 1, wherein the polishing solution is CeO2Or Fe2O3The suspension liquid has a suspension liquid concentration of 200-400g/L, the grain diameter of the polishing grains is less than or equal to 1 μm, and the polishing removal amount is more than 50 μm.
5. The method for detecting the thickness of the damaged layer on the subsurface of the silicate glass according to claim 1, wherein the drying temperature is 90-100 ℃ and the drying time is 5-15 min.
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| CN110220923B (en) * | 2019-06-24 | 2021-03-26 | 大连理工大学 | Optical glass abrasive particle processing sub-surface crack damage distribution characteristic detection method |
| CN110333251A (en) * | 2019-08-01 | 2019-10-15 | 西安奕斯伟硅片技术有限公司 | A kind of calculation method and device of edge damage depth |
| CN110561200A (en) * | 2019-08-02 | 2019-12-13 | 菲特晶(南京)电子有限公司 | quartz wafer processing technology |
| CN111024534A (en) * | 2019-12-30 | 2020-04-17 | 浙江师范大学 | Mechanical characterization method for optical glass subsurface damage |
| CN112834304B (en) * | 2021-01-20 | 2024-01-23 | 中国工程物理研究院机械制造工艺研究所 | Subsurface damage detection method based on metallographic mosaic |
| CN115116881A (en) * | 2022-08-25 | 2022-09-27 | 西安奕斯伟材料科技有限公司 | Method and system for measuring depth of damaged layer on surface of wafer |
| CN115343301B (en) * | 2022-10-20 | 2023-05-23 | 盛吉盛(宁波)半导体科技有限公司 | Characterization method of subsurface damage depth of nonmetallic material |
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