CN113008917B - 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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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 take the subsurface crack depth as an index for evaluating the subsurface damage depth in the grinding process, and the subsurface crack depth usually exists 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 particles in the grinding process and the characteristics of the grinding process, the brittle removal in the grinding process is usually accompanied by plastic removal, and the subsurface micro information under the surface characteristics left by the plastic removal contains numerous types of subsurface damage except subsurface cracks, but is usually ignored, and the information has important significance for comprehensively recognizing the subsurface damage 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 subsurface damage in the grinding process, so that the damage control precision and reliability are influenced. 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 a hard and brittle optical crystal sample;
s2, cleaning the ground sample and then carrying out gold spraying treatment;
s3, detecting the surface micro-morphology of the sample subjected to the gold spraying treatment by using a scanning electron microscope, and distinguishing typical characteristic position areas of the surface of the sample;
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 S6, detecting a crack region in the polished spot of the sample after cleaning and drying treatment to obtain the depth information of the macroscopic subsurface damage layer of the hard and brittle optical crystal.
Preferably, the characteristic feature location area on the sample surface distinguished in step S3 of the present invention includes: a brittle removal zone and a plastic removal zone.
Preferably, step S4 of the present invention specifically includes:
s41, preparing a sample in a brittle removal area by adopting a focused ion beam;
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;
s43, preparing a sample in a plastic removal area by using a focused ion beam;
and 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 0.1um;
(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 in 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) The area of the spot on the grinding surface is larger than 1/2 of the area of the grinding surface of the sample;
(3) The spots are all on the grinding surface and must not contact 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 3min.
Preferably, step S6 of the present invention specifically includes:
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 moving distance of each time until the crack cannot be observed, wherein the total moving distance of the platform is the length L of the sub-surface crack region;
s62, measuring the spot profile by using a linear profiler, wherein a 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;
step S63, calculating the subsurface crack depth SSD = L tan α.
Preferably, step S1 of the present invention is grinding with a diamond grinding head, wherein the grinding surface is a plane of 15 × 9 mm.
Preferably, the samples of the hard and brittle optical crystal of the present invention are neodymium-doped yttrium aluminum garnet (Nd: YAG) samples with dimensions of 15X 9X 7mm.
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 using 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 magnetorheological speckles 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 the accompanying drawings, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not used as limiting the present invention.
Example 1
The embodiment 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), and the method can comprehensively research 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 practice of the present invention with a sample of neodymium-doped yttrium aluminum garnet (Nd: YAG) having dimensions of 15X 9X 7mm as the target of the test. As shown in fig. 1, the specific implementation steps of this embodiment are as follows:
step S1, precisely grinding a 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.
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.
S3, detecting the surface micro-morphology of the sample subjected to the gold spraying treatment by using a scanning electron microscope, and distinguishing typical characteristic position areas of the surface of the sample; 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.
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:
s41, positioning to a 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;
s43, preparing a sample in a plasticity removal area by using a focused ion beam;
and 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 are required to be as follows:
the size of (1) is 10 multiplied by 6 multiplied by 0.1um, (2) the section to be detected has no additional damage, and (3) the section to be detected is perpendicular to the grinding direction shown in fig. 2.
And 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 in 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: the depth of the spot is (1) larger than the depth of the subsurface crack, (2) the area of the spot on the grinding plane is larger than 1/2 of the area of the grinding surface of the sample, and (3) the spot is ensured to be completely on the grinding surface and not to be contacted with the edge, and a schematic diagram 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 S6, detecting a crack region in the polished spot of the sample after cleaning and drying treatment 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 movement of the platform is the length L of the sub-surface crack region;
step S62, measuring the spot profile by using a linear profiler, wherein a 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;
and S63, calculating the sub-surface crack depth SSD = L tan alpha based on the measured sub-plane crack region length L and the spot profile inclination angle alpha, and obtaining the macroscopic sub-surface damage layer depth information.
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 (8)
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 a hard and brittle optical crystal sample;
s2, cleaning the ground sample and then carrying out gold spraying treatment;
s3, detecting the surface micro-morphology of the sample subjected to the gold spraying treatment by using a scanning electron microscope, and distinguishing typical characteristic position areas of the surface of the sample;
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 on 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 subsurface damage microscopic information 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;
s6, detecting a crack area in the polished spot of the sample after cleaning and drying treatment to obtain depth information of a macroscopic subsurface damage layer of the hard and brittle optical crystal; the sample surface characteristic feature position areas distinguished in the step S3 comprise: a brittle removal zone and a plastic removal zone.
2. The macro-micro comprehensive detection method for the surface damage of the hard and brittle optical crystal according to claim 1, wherein the step S4 specifically comprises:
s41, preparing a sample in a brittle removal area by adopting a focused ion beam;
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;
s43, preparing a sample in a plasticity removal area by using a focused ion beam;
and 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.
3. The method for comprehensively detecting the surface damage of the hard and brittle optical crystal according to claim 2, wherein the samples prepared in the steps S41 and S43 are required to be as follows:
(1) Has a size of
；
(2) The section to be detected has no additional damage;
(3) The section to be detected is perpendicular to the grinding direction.
4. The method for comprehensively detecting the surface damage of the hard and brittle optical crystal by the macro and micro method according to claim 1, wherein the deterministic spot polishing in the step S5 is performed by using 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) The area of the spot on the grinding surface is more than 1/2 of the area of the grinding surface of the sample;
(3) The spots are all on the grinding surface and must not touch the edge.
5. The method for comprehensively detecting the surface damage of the hard and brittle optical crystal according to claim 1, wherein the corrosion treatment in step S5 is specifically to put the sample into a 20% HF solution for corrosion for 3min.
6. The macro and micro comprehensive detection method for surface damage of a hard and brittle optical crystal according to claim 1, wherein the step S6 specifically comprises:
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 moving distance of each time until no crack can be observed, wherein the total moving distance of the platform 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 obtaining the inclination angle of the spot profile
；
Step S63, calculating to obtain the depth of the subsurface crack
。
7. The macro and micro comprehensive detection method for surface damage of hard and brittle optical crystals as claimed in claim 1, wherein step S1 is carried out by grinding with a diamond grinding head having a grinding surface
Of the plane of (a).
8. The macro-micro comprehensive detection method for surface damage of hard and brittle optical crystal according to claim 1, characterized in that the hard and brittle optical crystal sample is a neodymium-doped yttrium aluminum garnet sample, and the size of the sample is neodymium-doped yttrium aluminum garnet
。
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| 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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