CN113008917A - Macro-micro comprehensive detection method for surface damage of hard and brittle optical crystal - Google Patents
Macro-micro comprehensive detection method for surface damage of hard and brittle optical crystal Download PDFInfo
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- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
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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
- G01B11/00—Measuring arrangements characterised by the use of optical techniques
- G01B11/22—Measuring arrangements characterised by the use of optical techniques for measuring depth
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20058—Measuring diffraction of electrons, e.g. low energy electron diffraction [LEED] method or reflection high energy electron diffraction [RHEED] method
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
- G01N23/2251—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
Abstract
The invention discloses a macro-micro comprehensive detection method for surface damage of a hard and brittle optical crystal, which comprises the following steps: carrying out precision grinding on the hard and brittle optical crystal sample; cleaning the ground sample and then carrying out gold spraying treatment; detecting the surface micro-morphology of the sample subjected to the gold spraying treatment by using a scanning electron microscope; preparing a sample in a typical characteristic position area on the surface of the sample by adopting a focused ion beam; detecting the prepared sample by using a transmission electron microscope to obtain the subsurface damage microscopic information of the hard and brittle optical crystal; carrying out deterministic spot polishing on the ground sample, then carrying out corrosion treatment, and cleaning the corroded sample; and detecting a crack region in the polishing spot to obtain the depth information of the macroscopic subsurface damage layer of the hard and brittle optical crystal. The method can comprehensively detect and research the macroscopic and microscopic damage of the ground subsurface, and provides a more reliable and comprehensive data basis for the low-damage processing technology of the hard and brittle optical crystal.
Description
Technical Field
The invention belongs to the technical field of hard and brittle optical crystal sub-surface damage detection, and particularly relates to a macro-micro comprehensive detection method for hard and brittle optical crystal surface damage based on magneto-rheological spot polishing and a projection electron microscope (TEM).
Background
The hard and brittle optical crystal is widely applied to the fields of aerospace, solid lasers and the like by virtue of excellent optical, mechanical and thermal stability properties. In order to achieve better performance indexes such as energy density and output efficiency, an optimized structure design method is required, and extremely high optical element manufacturing quality is also required. Generally, an optical element is manufactured by cutting, grinding and polishing a hard and brittle optical crystal, and due to the characteristics of high hardness, high brittleness, low toughness and the like, subsurface damage of different degrees is easy to occur in the processing process. Subsurface damage can reduce material strength and affect laser damage threshold, thereby affecting indexes such as service life, laser beam quality and energy transmission efficiency of optical components. Therefore, the control of the subsurface damage layer of the hard and brittle optical crystal element is an important index for improving the processability of the material, and the deterministic detection of the subsurface damage layer is an important prerequisite for realizing the high-precision processing of the material, especially for controlling the subsurface damage.
At present, researchers often use subsurface crack depth as an index for evaluating the depth of subsurface damage during grinding, and subsurface crack depth is usually present in a brittle removal area. For subsurface crack depth measurement, common destructive detection methods such as a section microscopic method, an angle polishing method, a magnetorheological polishing method (including a magnetorheological slope polishing method and a magnetorheological spot polishing method) and the like can be used for detecting damage depth in a larger range, and the accuracy is highest particularly by the magnetorheological polishing method. However, due to the non-uniformity of the shape and size of the abrasive grains in the grinding process and the characteristics of the grinding process, the brittle removal in the grinding process is usually accompanied by the plastic removal, and the sub-surface micro information under the surface characteristics left by the plastic removal contains numerous types of sub-surface damages except the sub-surface cracks, but is usually ignored, and the information has important significance for comprehensively knowing the sub-surface damages in the grinding process. There is therefore a need for a method that allows both macroscopic detection of subsurface crack depths and microscopic analysis of localized subsurface damage.
Disclosure of Invention
The invention provides a macro-micro comprehensive detection method for surface damage of a hard and brittle optical crystal based on magnetorheological spot polishing and a Transmission Electron Microscope (TEM), aiming at solving the problem that the existing detection method cannot comprehensively consider the sub-surface damage in the grinding process, thereby influencing the damage control precision and reliability. The method comprises the steps of precisely grinding the surface of a hard and brittle optical crystal material by using a Focused Ion Beam (FIB) to prepare a sample, and observing the sub-surface of the sample in a TEM (transverse electric field), so as to obtain detailed local sub-surface microscopic information of the sample; and integrally detecting the macroscopic subsurface damage depth by utilizing the characteristic that the magnetorheological polishing spots have no additional damage.
The invention is realized by the following technical scheme:
a macro-micro comprehensive detection method for surface damage of a hard and brittle optical crystal comprises the following steps:
step S1, precisely grinding the hard and brittle optical crystal sample;
step S2, cleaning the ground sample and then carrying out metal spraying treatment;
step S3, detecting the micro-topography of the sample surface after the gold spraying treatment by using a scanning electron microscope, and distinguishing the typical characteristic position area of the sample surface;
step S4, preparing a sample in a typical characteristic position area on the surface of the sample by adopting a focused ion beam; detecting a sample prepared in a typical characteristic position area of the surface of the sample by using a transmission electron microscope, and analyzing the subsurface damage of the typical characteristic of the surface to obtain the microscopic information of the subsurface damage of the hard and brittle optical crystal;
step S5, performing deterministic spot polishing on the ground sample, performing corrosion treatment on the polished sample, and cleaning and drying the corroded sample;
and step S6, detecting crack areas in the polished spots of the cleaned and dried sample to obtain the depth information of the macroscopic subsurface damage layer of the hard and brittle optical crystal.
Preferably, the characteristic feature location areas of the sample surface distinguished in step S3 of the present invention include: a brittle removal zone and a plastic removal zone.
Preferably, step S4 of the present invention specifically includes:
step S41, preparing a sample in the brittleness removal area by using focused ion beams;
step S42, detecting the sample prepared in the step S41 by using a transmission electron microscope, and analyzing the sub-surface damage characteristic information of the sample, wherein the sub-surface damage characteristic information comprises phase change, amorphous, dislocation, slippage and polycrystal characteristic information in the sample;
step S43, preparing a sample in the plastic removal area by using a focused ion beam;
and step S44, detecting the sample prepared in the step S43 by using a transmission electron microscope, and analyzing the sub-surface damage characteristic information of the sample, wherein the sub-surface damage characteristic information comprises phase change, amorphous, dislocation, slippage and polycrystal characteristic information in the sample.
Preferably, the samples prepared in step S41 and step S43 of the present invention are required to be as follows:
(1) the size is 10 multiplied by 6 multiplied by 0.1 um;
(2) the section to be detected has no additional damage;
(3) the section to be detected is perpendicular to the grinding direction.
Preferably, the deterministic spot polishing of step S5 of the present invention uses an alumina polishing solution, and the requirements for polishing spots are as follows:
(1) the depth of the spot is greater than the depth of the subsurface crack;
(2) 1/2 where the area of the spot on the grinding surface is greater than the area of the sample grinding surface;
(3) the spots are all on the grinding surface and must not touch the edge.
Preferably, the etching treatment of step S5 of the present invention is specifically to etch the sample in a 20% HF solution for 3 min.
Preferably, step S6 of the present invention specifically includes:
step S61, measuring by using a super-depth-of-field microscope, moving the platform along the direction of the grinding direction by taking the tip of the left part of the spot as a measuring reference, and recording the distance of each movement until the crack cannot be observed, wherein the total distance of the platform movement is the length L of the subsurface crack region;
step S62, measuring the spot profile by using a linear profiler, wherein the measuring path passes through the centers of the left tip and the right edge of the spot to obtain the profile appearance of the spot and obtain the inclination angle alpha of the spot profile;
in step S63, the subsurface crack depth SSD ═ L tan α is calculated.
Preferably, step S1 of the present invention is grinding with a diamond grinding head, and the grinding surface is a plane of 15 × 9 mm.
Preferably, the hard brittle optical crystal sample of the present invention is a neodymium-doped yttrium aluminum garnet (Nd: YAG) sample with dimensions of 15X 9X 7 mm.
The invention has the following advantages and beneficial effects:
according to the invention, the microscopic region of the sub-surface damage with local typical characteristics after grinding is analyzed through the TEM, and the macroscopic depth information is accurately obtained by utilizing the magnetorheological polishing spot method, so that the sub-surface damage after grinding is comprehensively detected and researched, and a foundation is laid for guiding the low-damage processing technology of the hard and brittle optical crystal.
Drawings
The accompanying drawings, which are included to provide a further understanding of the embodiments of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the principles of the invention. In the drawings:
FIG. 1 is a schematic flow chart of the method of the present invention.
FIG. 2 is a schematic diagram of the local subsurface damage detection of the present invention.
FIG. 3 is a schematic view of a magnetorheological spot according to the present invention.
FIG. 4 is a schematic view of measuring the sub-surface crack zone width with ultra depth of field according to the present invention.
FIG. 5 is a schematic view of the line profiler measuring spot profile according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples and accompanying drawings, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not meant to limit the present invention.
Example 1
The embodiment provides a macro and micro comprehensive detection method for surface damage of a hard and brittle optical crystal based on magnetorheological spot polishing and a Transmission Electron Microscope (TEM), and the method can be used for comprehensively researching macro and micro information of sub-surface damage of the hard and brittle optical crystal, so that a more reliable data base can be provided for a low-damage processing technology of the brittle optical crystal.
This example further illustrates the embodiments of the present invention by taking a sample of neodymium-doped yttrium aluminum garnet (Nd: YAG) with dimensions of 15X 9X 7mm as the object of the test. As shown in fig. 1, the specific implementation steps of this embodiment are as follows:
step S1, precisely grinding the hard and brittle optical crystal sample: in this example, a sample which was polished without damage was clamped on a precision grinding machine, ground with a diamond grinding head having a grinding surface of 15 × 9mm, and then removed and the workpiece was cleaned with an ultrasonic cleaner.
Step S2, cleaning the ground sample and then carrying out metal spraying treatment; this example was gold-blasted so that the sample could be imaged clearly in the SEM, but the surface features were not masked by the gold film.
Step S3, detecting the micro-topography of the sample surface after the gold spraying treatment by using a scanning electron microscope, and distinguishing the typical characteristic position area of the sample surface; in this embodiment, a sample after being sprayed with gold is placed in an SEM chamber for observation, and a brittle removal region and a plastic removal region are distinguished, as shown in a schematic diagram of common surface characteristics after YAG grinding (mainly including the brittle removal region and the plastic removal region) in fig. 2.
Step S4, preparing a sample in a typical characteristic position area on the surface of the sample by adopting a focused ion beam; detecting a sample prepared in a typical characteristic position area of the surface of the sample by using a transmission electron microscope, and analyzing the subsurface damage of the typical characteristic of the surface to obtain the microscopic information of the subsurface damage of the hard and brittle optical crystal; step S4 of this embodiment specifically includes:
step S41, positioning the brittle removal area, and preparing a sample in the brittle removal area by adopting a focused ion beam;
step S42, detecting the sample prepared in the step S41 by using a transmission electron microscope, and then analyzing the sub-surface damage characteristic information of the sample by using transmission electron microscope analysis software Digital Micrograth, wherein the sub-surface damage characteristic information comprises sub-surface damage characteristic information of phase change, amorphousness, dislocation, slippage, polycrystal and the like in the sample;
step S43, preparing a sample in the plastic removal area by using a focused ion beam;
and step S44, detecting the sample prepared in the step S43 by using a transmission electron microscope, and analyzing the sub-surface damage characteristic information of the sample, wherein the sub-surface damage characteristic information comprises sub-surface damage characteristic information of phase change, amorphousness, dislocation, slippage, polycrystal and the like in the sample.
The samples prepared in step S41 and step S43 in this example were required to be as follows:
(1) the dimension is 10 multiplied by 6 multiplied by 0.1um, (2) the section to be detected has no additional damage, (3) the section to be detected is perpendicular to the grinding direction shown in fig. 2.
And step S5, performing deterministic spot polishing on the ground sample, performing corrosion treatment on the polished sample, and cleaning and drying the corroded sample.
The spot polishing process of this embodiment is specifically: the method comprises the following steps of (1) enabling the grinding surface of a sample to face upwards, adhering the sample to a workpiece platform of a magnetorheological polishing machine tool, setting polishing parameters to polish magnetorheological spots, wherein an alumina polishing solution is used as the polishing solution, and the requirements for polishing the spots are as follows: (1) the depth of the spot is greater than the subsurface crack depth, (2) the area of the spot in the grinding plane is greater than 1/2 for the area of the sample grinding surface, (3) the spot should be guaranteed to be completely on the grinding surface and not to contact the edge, and the schematic view of the polishing spot is shown in fig. 3.
The etching treatment in this embodiment is specifically: and (3) putting the sample into a 20% HF solution for corrosion for 3min, and carrying out ultrasonic cleaning and drying treatment after corrosion.
And step S6, detecting crack areas in the polished spots of the cleaned and dried sample to obtain the depth information of the macroscopic subsurface damage layer of the hard and brittle optical crystal.
Step S6 of this embodiment specifically includes:
step S61, measuring by using a super-depth-of-field microscope, as shown in FIG. 4, moving the platform along the direction of the grinding direction by using 400X multiplying power and taking the tip of the left part of the spot as a measuring reference, and recording the distance of each movement until the crack cannot be observed, wherein the total distance of the platform movement is the length L of the sub-surface crack region;
step S62, measuring the spot profile by using a linear profiler, wherein the measuring path passes through the centers of the left tip and the right edge of the spot to obtain the profile appearance of the spot, and obtaining the inclination angle alpha of the spot profile, as shown in FIG. 5;
in step S63, the subsurface crack depth SSD ═ L tan α is calculated based on the measured sub-planar crack region length L and the spot profile inclination angle α, that is, the macroscopic subsurface damage layer depth information can be obtained.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (9)
1. A macro-micro comprehensive detection method for surface damage of a hard and brittle optical crystal is characterized by comprising the following steps:
step S1, precisely grinding the hard and brittle optical crystal sample;
step S2, cleaning the ground sample and then carrying out metal spraying treatment;
step S3, detecting the micro-topography of the sample surface after the gold spraying treatment by using a scanning electron microscope, and distinguishing the typical characteristic position area of the sample surface;
step S4, preparing a sample in a typical characteristic position area on the surface of the sample by adopting a focused ion beam; detecting a sample prepared in a typical characteristic position area of the surface of the sample by using a transmission electron microscope, and analyzing the subsurface damage of the typical characteristic of the surface to obtain the microscopic information of the subsurface damage of the hard and brittle optical crystal;
step S5, performing deterministic spot polishing on the ground sample, performing corrosion treatment on the polished sample, and cleaning and drying the corroded sample;
and step S6, detecting crack areas in the polished spots of the cleaned and dried sample to obtain the depth information of the macroscopic subsurface damage layer of the hard and brittle optical crystal.
2. The method for comprehensively detecting the macro and micro damage on the surface of the hard and brittle optical crystal according to claim 1, wherein the sample surface typical characteristic position areas distinguished in the step S3 comprise: a brittle removal zone and a plastic removal zone.
3. The method for comprehensively detecting the surface damage of the hard and brittle optical crystal according to claim 2, wherein the step S4 specifically comprises:
step S41, preparing a sample in the brittleness removal area by using focused ion beams;
step S42, detecting the sample prepared in the step S41 by using a transmission electron microscope, and analyzing the sub-surface damage characteristic information of the sample, wherein the sub-surface damage characteristic information comprises phase change, amorphous, dislocation, slippage and polycrystal characteristic information in the sample;
step S43, preparing a sample in the plastic removal area by using a focused ion beam;
and step S44, detecting the sample prepared in the step S43 by using a transmission electron microscope, and analyzing the sub-surface damage characteristic information of the sample, wherein the sub-surface damage characteristic information comprises phase change, amorphous, dislocation, slippage and polycrystal characteristic information in the sample. .
4. The method for comprehensively detecting the surface damage of the hard and brittle optical crystal according to claim 3, wherein the samples prepared in the steps S41 and S43 are required to be as follows:
(1) the size is 10 multiplied by 6 multiplied by 0.1 um;
(2) the section to be detected has no additional damage;
(3) the section to be detected is perpendicular to the grinding direction.
5. The method for comprehensively detecting the macro and micro damage on the surface of the hard and brittle optical crystal according to claim 1, wherein the deterministic spot polishing of step S5 is performed with an alumina polishing solution, and the requirements for polishing spots are as follows:
(1) the depth of the spot is greater than the depth of the subsurface crack;
(2) 1/2 where the area of the spot on the grinding surface is greater than the area of the sample grinding surface;
(3) the spots are all on the grinding surface and must not touch the edge.
6. The method for comprehensively detecting the surface damage of the hard and brittle optical crystal according to claim 1, wherein the corrosion treatment of step S5 is specifically to put the sample into a 20% HF solution for corrosion for 3 min.
7. The method for comprehensively detecting the surface damage of the hard and brittle optical crystal according to claim 1, wherein the step S6 specifically comprises:
step S61, measuring by using a super-depth-of-field microscope, moving the platform along the direction of the grinding direction by taking the tip of the left part of the spot as a measuring reference, and recording the distance of each movement until the crack cannot be observed, wherein the total distance of the platform movement is the length L of the subsurface crack region;
step S62, measuring the spot profile by using a linear profiler, wherein the measuring path passes through the centers of the left tip and the right edge of the spot to obtain the profile appearance of the spot and obtain the inclination angle alpha of the spot profile;
in step S63, the subsurface crack depth SSD ═ Ltan α is calculated.
8. The method for comprehensively detecting the macro and micro damage on the surface of the hard and brittle optical crystal according to claim 1, wherein the step S1 is implemented by grinding with a diamond grinding head, and the grinding surface is a plane of 15 x 9 mm.
9. The method for comprehensively detecting the surface damage of the hard and brittle optical crystal according to claim 1, wherein the hard and brittle optical crystal sample is a neodymium-doped yttrium aluminum garnet (Nd: YAG) sample, and the size of the sample is 15 x 9 x 7 mm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115343301A (en) * | 2022-10-20 | 2022-11-15 | 盛吉盛(宁波)半导体科技有限公司 | Characterization method for subsurface damage depth of non-metallic material |
| CN115372090A (en) * | 2022-07-29 | 2022-11-22 | 中国船舶重工集团公司第七0七研究所 | Method for manufacturing and detecting quartz glass subsurface damage depth sample |
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