CN115575428A - Scanning electron microscope sample rapid sampling method for barium-based piezoelectric ceramic material for EBSD analysis - Google Patents
Scanning electron microscope sample rapid sampling method for barium-based piezoelectric ceramic material for EBSD analysis Download PDFInfo
- Publication number
- CN115575428A CN115575428A CN202210942688.XA CN202210942688A CN115575428A CN 115575428 A CN115575428 A CN 115575428A CN 202210942688 A CN202210942688 A CN 202210942688A CN 115575428 A CN115575428 A CN 115575428A
- Authority
- CN
- China
- Prior art keywords
- polishing
- sample
- piezoelectric ceramic
- barium
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- 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
- G01N23/2202—Preparing specimens therefor
-
- 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]
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The invention relates to the field of sample preparation of an electron back scattering research technology of barium-based piezoelectric ceramic, and discloses a method for quickly preparing a scanning electron microscope sample of barium-based piezoelectric ceramic material for EBSD analysis, which comprises the following steps: (1) Mechanically polishing the piezoelectric ceramic sample by using 3-micron diamond abrasive paper to obtain a smooth surface with higher quality; (2) polishing by adopting a soft velvet polishing cloth; (3) polishing by adopting double-sided polishing cotton; and (4) carrying out vibration polishing treatment on the sample. The method adopts a pure physical polishing technology, effectively controls the expansion of the holes of the ceramic sample, avoids the extrinsic influence of electrolysis and ion polishing on the domain structure and the microstructure of the piezoelectric ceramic, greatly shortens the preparation time of the sample relative to the ion polishing, reduces the preparation cost and improves the sample preparation efficiency.
Description
Technical Field
The invention relates to the technical field of electron back scattering research of barium-based piezoelectric ceramics, in particular to a scanning electron microscope sample rapid sampling method of barium-based piezoelectric ceramics for EBSD analysis.
Background
The piezoelectric material with the positive and negative piezoelectric effect can realize the interconversion of mechanical energy and electric energy, and is widely applied to the fields of driving, energy storage, transduction and the like. The dielectric and piezoelectric properties of piezoelectric ceramics are derived from intrinsic and extrinsic contributions, the former being closely related to lattice distortion and the latter being closely related to domain wall motion and even field-induced phase transition. Therefore, a reasonable and correct knowledge of the microstructure is considered to be one of the important ways to understand the change in properties. Electron backscatter diffraction (EBSD) is widely applied to microstructure and microtexture characterization of materials at present, and a series of analyses including local orientation difference, special crystal boundary identification, local stress difference and the like can be carried out by obtaining an electron backscatter diffraction pattern. The current common EBSD sample preparation methods include electrolytic polishing and ion polishing. However, for the barium-based piezoelectric ceramics, which are relatively soft, the following problems may exist in the electrolytic polishing and the ion polishing: (1) The electrolytic polishing needs to be provided with electrolyte, and the electrolyte is related to chemical components of the oxide ceramic, so that the use limitation is increased; (2) Because the sample is soft, the ion beam is easy to knock the sample surface out of a small pit in the ion polishing process, so that the smoothness is reduced, the orientation distribution analysis is not facilitated, the time consumption is long, and the time is generally more than 3 hours. (3) In the ion polishing process, high-energy ions bombard the surface of a sample, so that part of intrinsic defects can be released, and the real surface appearance is difficult to obtain.
Different from the two methods, the vibration polishing almost has no limitation on the sample, has the characteristics of high safety, high success rate, simple operation, rapid preparation and the like, and is very suitable for the barium-based piezoelectric ceramic material. The patent CN113514485A adopts a vibration polishing method to obtain a high-quality chrysanthemum pool pattern distribution diagram of neodymium iron boron, and the total time consumption is about 10 hours. CN113295724A adopts the vibration polishing technology to make the aluminum alloy sample after corrosion have higher structural calibration rate, and can clearly analyze the corrosion type, path and orientation of the sample. However, how to combine mechanical polishing and vibratory polishing to improve EBSD calibration rate and sample preparation efficiency for softer piezoelectric ceramics still remains to be improved.
Therefore, the method for rapidly preparing the scanning electron microscope sample of the barium-based piezoelectric ceramic material for EBSD analysis has the advantages of safety, high success rate, simplicity in operation, rapidness in preparation and the like, and has important significance for improving EBSD calibration accuracy and reducing zero resolution rate so as to further explore the relationship between local orientation difference, special grain boundary identification, local stress difference and other results and performances.
Disclosure of Invention
The invention aims to provide a rapid sample preparation method for a scanning electron microscope sample of a barium-based piezoelectric ceramic material for EBSD analysis. The method can greatly avoid the expansion of intrinsic holes by a pretreatment mode of the soft flannelette and the polishing cotton. Based on a pure physical polishing mode, the method avoids the influence of chemistry and ions on the intrinsic microstructure of the surface of the barium-based piezoelectric ceramic, has the characteristics of safety, high success rate, simple operation, rapid preparation and the like, and can obtain nearly 100 percent of electron back scattering diffraction resolution rate.
In order to realize the purpose, the technical scheme adopted by the invention comprises the following steps:
step one, mechanically polishing a sample to obtain a smooth surface;
polishing the sample by using a velveteen polishing cloth;
polishing the sample by adopting double-sided polishing cotton;
step four, placing the sample in a vibration polishing machine for vibration polishing;
and step five, after the treatment is finished, carrying out electron back scattering diffraction analysis.
Preferably, the step one test sample is obtained by a diamond cutter, and the surface of the test sample is polished by using 3 μm diamond abrasive paper until the surface has slight and uniform-direction scratches.
Preferably, in the first step, the size of the sample obtained by the diamond cutter is 2.5 × 2.5 × 2mm.
Preferably, in the second step, the sample is polished by a soft flannelette at a rotating speed of 60-80 r/min.
Preferably, in the second step, the sample is polished for 5min by using a soft flannel.
Preferably, in the third step, the water-wetted and lubricated surface is polished by double-sided polishing cotton, and the polishing direction is fixed.
Preferably, in the third step, the double-sided polishing cotton is 8000 meshes.
Preferably, in the fourth step, the vibration polishing is performed on the sample at 20% power for about 15-20 min.
Preferably, in the fourth step, the vibration polishing is performed on the sample at 20% power for about 18min.
Preferably, in the fourth step, the vibration polishing is performed on the sample at 20% power for about 18min.
Preferably, in the fifth step, the sample is fixed on a sample stage by silver paste, and electron back scattering diffraction observation is performed.
By adopting the technical scheme, the invention has the following beneficial technical effects:
(1) Safety: the preparation process of the sample does not involve any volatile or harmful chemical substances, and the pure physical polishing mode can reduce the damage of the sample preparation to the surface to the maximum extent and reduce the real surface morphology and diffraction information of the sample.
(2) The success rate is high: the polishing process only needs to keep the polishing direction consistent, and the artificial influence is small.
(3) The operation is simple: the preparation process adopts a pure physical mode, and compared with the conventional common polishing modes, namely electrolytic polishing and ion polishing, the preparation of electrolyte and the regulation and control of ion beam current are avoided.
(4) The sample preparation time is short: polishing with 3 μm abrasive paper for 10min, polishing with velveteen polishing cloth for 5min, polishing with double-sided polishing cotton for 5min, and vibration polishing for 15-20 min, wherein the total time is only 35-40 min.
Drawings
Fig. 1 is a schematic flow chart of a scanning electron microscope sample rapid sampling method of a barium-based piezoelectric ceramic material for EBSD analysis provided by the present application.
Fig. 2 is an IPF image obtained after EBSD.
Figure 3 is the percentage content of the phase obtained after EBSD.
Fig. 4 is an IPF image obtained by ion polishing.
Detailed Description
Example 1:
the invention will be described in further detail below with reference to specific embodiments and the attached drawings:
a scanning electron microscope sample rapid sampling method of a barium-based piezoelectric ceramic material for EBSD analysis is disclosed, and is shown in figure 1, and comprises the following steps:
the method comprises the following steps: taking out the sample, and then mechanically polishing the sample; the samples were mechanically polished to obtain a smooth surface.
The sample is cut into 2.5 multiplied by 2mm blocks by a diamond cutting machine, the surface of the sample is polished by using 3 mu m diamond abrasive paper and using clear water as a medium, 100g of balancing weight is added in the polishing process to accelerate the polishing process, and the polishing speed is 30r/min until the surface has slight scratches with the same direction.
Step two: and polishing the sample by using a soft velvet polishing cloth.
And polishing the sample on a velveteen polishing cloth by using clean water as a medium, wherein the polishing rotating speed is increased to 60 r/min-80 r/min, and the polishing time is about 5min so as to reduce the scratch depth. It should be noted that the diamond suspension is not used as the polishing medium, and since the barium-based ceramic contains some pores, the diamond particles are easily stuck in the pores to cause the cracks around the pores, thereby increasing the pore area.
Step three: and polishing the sample by adopting double-sided polishing cotton.
The sample is polished on 8000-mesh double-sided polishing cotton by wetting and lubricating the surface, and the polishing cotton needs to be polished along the same direction without back-and-forth friction.
Step four: and (3) placing the sample in a vibration polishing machine for vibration polishing.
The sample is placed in a vibration polishing machine, 10ml of polishing solution is added to soak polishing cloth, the polishing power is 20%, and the polishing time is about 15-20 min, preferably 18min. And after finishing, washing the polished surface by deionized water and alcohol alternately, and drying.
The pretreatment of the soft flannelette and the polishing cotton can avoid the expansion of intrinsic holes to a great extent, reduce the time of single-use vibration polishing, and the 20 percent vibration power can not influence the pressure-sensitive barium-based piezoelectric ceramic material.
Step five: the sample is placed on a sample stage special for electron back scattering diffraction, silver paste is used as an adhesive, the sample is fixed on the sample stage, electron back scattering diffraction observation and analysis are carried out on a target area, and the result is shown in fig. 2 and fig. 3.
The inventor of the present application finds out in the research process that the method needs to pay attention to the following points:
(1) When the 3-micron diamond abrasive paper is used in the first step, if a sample has sharp edges, the sample needs to be smoothed by using low-mesh-number abrasive paper, otherwise, the diamond abrasive paper is easily scratched, and free diamond chips are generated to scratch the surface.
(2) In the first step, the polishing rotation speed is not too high, which is easy to cause steps on the surface of the sample, and is not beneficial to the overall smoothness.
(3) And in the second step, the soft velvet polishing cloth is required to be thoroughly cleaned before being used, so that fine particles possibly remaining in the soft velvet polishing cloth are removed.
(4) And in the third step, when 8000-mesh double-sided polishing cotton is adopted, clear water is used as a medium to reduce resistance, and when the surface of the polishing cotton is changed from white to other colors, the polishing cotton needs to be replaced.
(5) And in the fourth step, the surface of the sample needs to be cleaned immediately after the vibration polishing so as to remove the potential influence of the polishing solution on the sample.
The electron back scattering diffraction results show that the orientation information and the phase information of the barium-based piezoelectric ceramic material can be effectively obtained by the method, as shown in fig. 2 and 3. The surface is almost free from any scratch, and the local stress caused by the interface can be further analyzed. And by the statistics of phase percentage, the zero solution is only 3.06 percent and is all derived from intrinsic holes of the target region. The results show that the method can quickly obtain the barium-based piezoelectric ceramic material applied to electron back scattering diffraction analysis.
Comparative example 1:
and obtaining an ion polishing pretreatment sample according to the first step to the third step, and carrying out ion polishing treatment on the sample, wherein the specific parameters are 4 kV-30 min, 3 kV-30 min, 2 kV-40 min and 1 kV-40 min. The subsequent topography and EBSD results are shown in figure 3. Although higher resolution is obtained by ion polishing, the ion etching, which is more complex in operation, takes about 7 times as long as vibration polishing and lacks the attenuation of fine scratches, expanding intrinsic pores topographically.
In conclusion, the scanning electron microscope sample rapid sampling method for the barium-based piezoelectric ceramic material for EBSD analysis provided by the application can greatly avoid the expansion of intrinsic pores through the pretreatment mode of the soft flannelette and the polishing cotton. Based on a pure physical polishing mode, the method avoids the influence of chemistry and ions on the intrinsic microstructure of the surface of the barium-based piezoelectric ceramic, has the characteristics of safety, high success rate, simple operation, rapid preparation and the like, and can obtain nearly 100 percent of electron back scattering diffraction resolution rate.
Particularly, no volatile or harmful chemical substances are involved in the sample preparation process, and the pure physical polishing mode can reduce the damage of sample preparation to the surface to the maximum extent and reduce the real surface appearance and diffraction information of the sample; the safety performance is extremely high. And the polishing process only needs to keep the same polishing direction, and the artificial influence is small, so the success rate is high. Compared with the common polishing modes of electrolytic polishing and ion polishing, the preparation process adopts a pure physical mode, avoids the preparation of electrolyte and the regulation and control of ion beam current, so the operation is simple, and the operation process is simplified greatly compared with the prior art. Polishing with 3 μm abrasive paper for 10min, polishing with velveteen polishing cloth for 5min, polishing with double-sided polishing cotton for 5min, and vibration polishing for 15-20 min, wherein the total time is only 35-40 min. Therefore, the sample preparation time is short, the preparation efficiency is high, compared with ion polishing, the sample preparation time is greatly shortened, the preparation cost is reduced, and the sample preparation efficiency is improved.
In addition, the method for preparing the scanning sample for electron back scattering diffraction observation is not limited to the barium-based piezoelectric ceramic material, and the piezoelectric ceramic material with similar hardness also meets the application range of the method.
The above description is only an embodiment of the present invention, and it should be noted that, for those skilled in the art, many variations and modifications can be made without departing from the structure of the present invention, and these should also be considered as the protection scope of the present invention, which will not affect the effect of the implementation of the present invention and the practicability of the patent. The scope of the claims of the present application shall be determined by the contents of the claims, and the description of the embodiments and the like in the specification shall be used to explain the contents of the claims.
Claims (10)
1. A scanning electron microscope sample rapid sample preparation method of a barium-based piezoelectric ceramic material for EBSD analysis is characterized by comprising the following steps:
step one, mechanically polishing a sample to obtain a smooth surface;
polishing the sample by using a velveteen polishing cloth;
polishing the sample by adopting double-sided polishing cotton;
step four, placing the sample in a vibration polishing machine for vibration polishing;
and step five, after the treatment is finished, carrying out electron back scattering diffraction analysis.
2. The method according to claim 1, wherein the sample in the first step is obtained by a diamond cutting machine, and the surface of the sample is polished by using 3 μm diamond sandpaper until the surface has slight and uniform scratches.
3. The production method according to claim 2, wherein in the first step, the size of the sample obtained by the diamond cutter is 2.5 x 2mm.
4. The method according to claim 1, wherein in the second step, the sample is polished with a lint at a rotation speed of 60 to 80 r/min.
5. The method according to claim 4, wherein in the second step, the sample is polished with a lint for 5min.
6. The method as claimed in claim 1, wherein in the third step, the polishing is performed by using double-sided polishing cotton to wet the lubricated surface, and the polishing direction is fixed.
7. The method according to claim 1, wherein the double-sided polishing cotton is 8000 mesh.
8. The method of claim 1, wherein in the fourth step, the sample is vibro-polished at 20% power for about 15-20 min.
9. The method of claim 1, wherein in the fourth step, the vibration polishing is performed on the sample at 20% power for about 18min.
10. The preparation method according to claim 1, wherein in the fifth step, the sample is fixed on a sample stage by silver paste, and electron back scattering diffraction observation is performed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210942688.XA CN115575428A (en) | 2022-08-08 | 2022-08-08 | Scanning electron microscope sample rapid sampling method for barium-based piezoelectric ceramic material for EBSD analysis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210942688.XA CN115575428A (en) | 2022-08-08 | 2022-08-08 | Scanning electron microscope sample rapid sampling method for barium-based piezoelectric ceramic material for EBSD analysis |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115575428A true CN115575428A (en) | 2023-01-06 |
Family
ID=84580044
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210942688.XA Pending CN115575428A (en) | 2022-08-08 | 2022-08-08 | Scanning electron microscope sample rapid sampling method for barium-based piezoelectric ceramic material for EBSD analysis |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115575428A (en) |
-
2022
- 2022-08-08 CN CN202210942688.XA patent/CN115575428A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109470728A (en) | A kind of titanium alloy pendulum grinds the preparation method of part metallographic specimen | |
| CN111982642B (en) | EBSD sample preparation method of fracture sample section | |
| CN101738340A (en) | Method for preparing sample showing metallurgical structure of tantalum-tungsten alloy | |
| CN107976459A (en) | The analyzing detecting method of two-phase proportion in a kind of two phase stainless steel as-cast structure | |
| CN111693736B (en) | Section sample of lithium ion battery electrode plate for atomic force microscope characterization and preparation method thereof | |
| CN109211645A (en) | The metallographic etching agent of chromium tantalum-titanium alloy and its display methods of metallographic structure | |
| Chen et al. | Electrochemical jet-assisted precision grinding of single-crystal SiC using soft abrasive wheel | |
| CN110596163B (en) | Preparation method of EBSD sample of titanium alloy fracture section | |
| CN109540947B (en) | Method for preparing nose tip sample for FIB three-dimensional reconstruction | |
| CN109283204A (en) | A method of preparing near atomic ratio Co-Ni-Al magnetic control shape memory alloy electron backscatter diffraction sample | |
| CN115575428A (en) | Scanning electron microscope sample rapid sampling method for barium-based piezoelectric ceramic material for EBSD analysis | |
| CN110618153A (en) | Preparation method of electropolished titanium alloy large-size rod-shaped or plate-shaped sample | |
| CN104006994A (en) | Method for displaying color metallographic tissues of pure aluminum | |
| CN107764620A (en) | A kind of Pb-Ca-Sn-Al alloy metallographic preparation method | |
| CN110954388A (en) | Metallographic corrosive agent for laser cladding layer of titanium alloy containing rare earth and tissue display method | |
| CN115711899A (en) | Preparation method of EBSD (Electron Back-scattered diffraction) section sample with corrosion product film sample | |
| CN113533398B (en) | Method for representing multi-phase oxide layer of steel plate section by adopting EBSD technology | |
| Navitski et al. | Surface analyses and optimization of centrifugal barrel polishing of Nb cavities | |
| CN112441846A (en) | Treatment method and application of boron carbide ceramic | |
| CN107063786A (en) | A kind of preparation method of nanometer gradient structural material top layer EBSD samples | |
| CN110954571A (en) | Experimental method for rapidly improving hardness of titanium alloy at normal temperature | |
| CN112945676B (en) | Method for preparing pure aluminum metallographic sample by dielectric barrier discharge technology | |
| CN115753854A (en) | Method for preparing titanium alloy EBSD sample by additive manufacturing through chemical polishing | |
| CN114235864B (en) | Preparation method of bismuth alloy sample for EBSD test | |
| CN113960082A (en) | Sample preparation method for hot-rolled strip steel iron scale EBSD analysis |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |