阅读说明：本技术 稀土金属氧化物晶体的位错检测方法 (Dislocation detection method of rare earth metal oxide crystal ) 是由 李子阳 黄凯 骆文锋 张坤 朱刚 刘子莲 于 2021-07-26 设计创作，主要内容包括：本发明公开了一种稀土金属氧化物晶体的位错检测方法,包括以下步骤：利用质量分数为75％～95％的磷酸溶液在80℃～200℃下对所述稀土金属氧化物晶体刻蚀处理10分钟～60分钟,制备预处理样品；对所述预处理样品进行观察,获取所述稀土金属氧化物晶体的位错特征。通过对稀土金属氧化物晶体选择适当的刻蚀温度以及刻蚀液,使晶体结构中的位错易于在光学显微镜下以及扫描电子显微镜下进行观察,不仅可以判断稀土金属氧化物的晶体结构中位错的类型,还能进一步计算出晶体位错密度。上述测试方法成本低且周期短,避免传统透射电子显微镜对样品进行繁琐处理以及X射线衍射不能对晶体位错类型进行判断的缺陷。(The invention discloses a dislocation detection method of rare earth metal oxide crystals, which comprises the following steps: etching the rare earth metal oxide crystal by using a phosphoric acid solution with the mass fraction of 75-95% at the temperature of 80-200 ℃ for 10-60 minutes to prepare a pretreated sample; and observing the pretreated sample to obtain the dislocation characteristics of the rare earth metal oxide crystal. By selecting proper etching temperature and etching liquid for the rare earth metal oxide crystal, the dislocation in the crystal structure can be easily observed under an optical microscope and a scanning electron microscope, the type of the dislocation in the crystal structure of the rare earth metal oxide can be judged, and the crystal dislocation density can be further calculated. The testing method is low in cost and short in period, and the defects that a traditional transmission electron microscope carries out tedious processing on a sample and X-ray diffraction cannot judge the type of crystal dislocation are overcome.)

1. A dislocation detection method of a rare earth metal oxide crystal is characterized by comprising the following steps:

s1: etching the rare earth metal oxide crystal by using a phosphoric acid solution with the mass fraction of 75-95% at the temperature of 80-200 ℃ for 10-60 minutes to prepare a pretreated sample;

s2: and observing the pretreated sample to obtain the dislocation characteristics of the rare earth metal oxide crystal.

2. A dislocation detection method of a rare earth metal oxide crystal according to claim 1, wherein said dislocation characteristics include dislocation type and dislocation density.

3. A dislocation detection method of a rare earth metal oxide crystal as claimed in claim 1, wherein said rare earth metal oxide is lutetium oxide, and an image after observation shows:

the triangular pit is in a shape of a triangular pit, and a bottom recess in the middle of the pit is a triangular platform which is in a screw dislocation shape;

the triangular pit is in an inverted triangular cone shape and is edge dislocation;

the triangular pit is in a shape of a triangular pit, at least one triangular platform is arranged in the middle of the pit, and the center of the platform is an inverted triangular cone which is a mixed dislocation.

4. A dislocation detection method of a rare earth metal oxide crystal according to claim 3, wherein the observation is performed by a scanning electron microscope.

5. A dislocation detection method of a rare earth metal oxide crystal according to claim 1, wherein the temperature of the etching treatment is 80 to 130 ℃.

6. A dislocation detection method of a rare earth metal oxide crystal according to claim 1, characterized in that the etching treatment time is 30 minutes to 50 minutes.

7. A dislocation detection method of a rare earth metal oxide crystal according to claim 1, further comprising, before step S1, the steps of sequentially grinding, polishing, first cleaning and first drying the rare earth metal oxide crystal.

8. A dislocation detection method of rare earth metal oxide crystals as claimed in claim 7, characterized in that the step of grinding comprises: and polishing the rare earth metal oxide crystal by using sand paper.

9. A dislocation detection method of a rare earth metal oxide crystal according to claim 8, wherein the mesh number of the sand paper is 2000 to 4000.

10. A dislocation detection method of rare earth metal oxide crystals as claimed in claim 7, characterized in that the step of polishing comprises: polishing the ground rare earth metal oxide crystal by using at least one of diamond, cerium oxide, aluminum oxide, silicon oxide, iron oxide, zirconium oxide and chromium oxide.

11. A dislocation detection method of rare earth metal oxide crystals as claimed in claim 7, characterized in that the step of first cleaning includes: and respectively utilizing a first organic solvent and a first inorganic solvent to carry out primary cleaning on the polished rare earth metal oxide crystal.

12. A dislocation detection method of rare earth metal oxide crystals as claimed in claim 1, further comprising the steps of a second cleaning and a second drying treatment of said pre-treated sample before step S2 and after step S1.

13. A dislocation detection method for a rare earth metal oxide crystal according to claim 12, wherein the step of second cleaning includes: and respectively washing the pretreated sample for the second time by using a second organic solvent and a second inorganic solvent.

14. A dislocation detection method of a rare earth metal oxide crystal according to claim 11 or 13, characterized in that said first organic solvent and said second organic solvent are each independently selected from at least one of ethanol and acetone.

Technical Field

The invention relates to the field of crystal structure detection, in particular to a dislocation detection method of a rare earth metal oxide crystal.

Background

The atomic structure of the rare earth element may be represented by 4f^x5d16s²To indicate that x represents a number from 0 to 14. Among the valences of rare earth elements, there are many different valences, for example, in some compounds such as cerium and europium, the valences of which are three-valent or four-valent or two-valent or three-valent, and this kind of valence change phenomenon is receiving increasing attention. The rare earth ions have large radius and high valence, so the rare earth ions are very easy to be polarized, and the higher the polarization degree is, the higher the ion refractive index is, so the rare earth ions have excellent optical, electrical and magnetic properties. The rare earth material has excellent magnetic property, electrical and optical characteristics, plays a great role in improving product performance, improving production efficiency and producing multipurpose commodities, and plays an indispensable role in promoting various fields such as aerospace national defense, metallurgical industry, glass, petroleum, chemical industry, ceramics, even agriculture and the like. In the research field of new materials such as aerospace, color-changing glass, superconducting permanent magnetic materials and the like, rare earth materials are also gaining more and more attention, such as typical rare earth metal oxide lutetium oxide. The lutetium oxide crystal has the characteristics of lower phonon energy, wider emission spectrum, higher thermal conductivity and the like, and has become a laser crystal widely used on a high-power solid laser.

The properties of the lutetium oxide crystal depend on the structure, composition, defect distribution, etc. inside it. The preparation process of the lutetium oxide crystal is complex, and the quality of the crystal is determined to a great extent by the process parameters of crystal growth. In addition, lutetium oxide is a typical hard and brittle hard-to-machine material, and large surface defects and subsurface damage are generated in ultra-precise machining processes such as grinding and polishing, so that the quality and the service life of a laser are affected.

In recent years, crystal growth and microscopic characterization of lutetium oxide, both high quality and large size, have become one of the hot spots of research. Dislocations are typical crystal structure microscopic defects, and in optically transparent ceramic materials, dislocations are generally considered as scattering sources in laser crystals, which seriously affect the quality and the photoelectric characteristics of the crystals. Therefore, the detection method for dislocation in the lutetium oxide crystal can be researched, the evaluation method for the quality of the lutetium oxide crystal can be perfected, and the defects of the lutetium oxide preparation process can be found through the detection means, so that the crystal growth and the processing technology of lutetium oxide are promoted.

The conventional dislocation density detection method for crystals at present has three types: the first method is that firstly, focused ion beams are adopted to cut crystals to obtain samples in specific areas, and then a transmission electron microscope is adopted to observe dislocation; the second method is that X-ray diffraction is adopted to obtain an XRD (X-ray diffraction) pattern of a phase, then peak shape fitting is carried out on the diffraction pattern to obtain the positions and half-height widths of diffraction peaks of different diffraction surfaces, then multi-step fitting is carried out on the XRD pattern, and finally the crystal dislocation density is calculated through a mathematical formula; the third is a photo-assisted wet etching technique, in which a crystal is placed in an etching solution and a specific light source is introduced to increase the etching rate.

According to the method for observing the crystal through the transmission electron microscope sample, the sample needs to be cut in a selected area by utilizing the focused ion beam under the scanning electron microscope, the lutetium oxide material has hard and brittle properties, the sample preparation process is complex, the observable area is generally only a few microns, the cost is high, the period is long, and the method is not suitable for conventional detection; the X-ray diffraction method cannot directly observe the dislocation in the crystal, and cannot characterize the type, form, distribution and the like of the dislocation; in addition, the photo-assisted wet etching technique requires a specific light source for irradiation during the test and cannot rapidly analyze the dislocation type.

Disclosure of Invention

Based on this, it is necessary to provide a dislocation detection method for a rare earth metal oxide crystal which is low in cost, short in cycle time, and capable of directly observing dislocations in the crystal.

The invention provides a dislocation detection method of rare earth metal oxide crystals, which comprises the following steps:

s1: etching the rare earth metal oxide crystal by using a phosphoric acid solution with the mass fraction of 75-95% at the temperature of 80-200 ℃ for 10-60 minutes to prepare a pretreated sample;

s2: and observing the pretreated sample to obtain the dislocation characteristics of the rare earth metal oxide crystal.

In one embodiment, the dislocation characteristics include dislocation type and dislocation density.

In one embodiment, the rare earth metal oxide is lutetium oxide and the observed image shows:

the triangular pit is in a shape of a triangular pit, and a bottom recess in the middle of the pit is a triangular platform which is in a screw dislocation shape;

the triangular pit is in an inverted triangular cone shape and is edge dislocation;

the triangular pit is in a shape of a triangular pit, at least one triangular platform is arranged in the middle of the pit, and the center of the platform is an inverted triangular cone which is a mixed dislocation.

In one embodiment, the observation is performed using a scanning electron microscope.

In one embodiment, the temperature of the etching process is 80 ℃ to 130 ℃.

In one embodiment, the etching process is performed for 30 minutes to 50 minutes.

In one embodiment, before step S1, the method further includes, sequentially grinding, polishing, first cleaning, and first drying the rare earth oxide crystal.

In one embodiment, the step of grinding comprises: and polishing the rare earth metal oxide crystal by using sand paper.

In one embodiment, the mesh number of the sand paper is 2000-4000.

In one embodiment, the step of polishing comprises: polishing the ground rare earth metal oxide crystal by using at least one of diamond, cerium oxide, aluminum oxide, silicon oxide, iron oxide, zirconium oxide and chromium oxide.

In one embodiment, the first washing step comprises: and respectively utilizing a first organic solvent and a first inorganic solvent to carry out primary cleaning on the polished rare earth metal oxide crystal.

In one embodiment, the method further comprises a step of performing a second washing and a second drying process on the pretreated sample before the step S2 and after the step S1.

In one embodiment, the second cleaning step comprises: and respectively washing the pretreated sample for the second time by using a second organic solvent and a second inorganic solvent.

In one embodiment, the first organic solvent and the second organic solvent are each independently selected from at least one of ethanol and acetone.

By selecting proper etching temperature and etching liquid for etching treatment, the dislocation in the crystal structure can be easily observed under instruments such as an optical microscope and a scanning electron microscope, the type of the dislocation in the crystal structure of the rare earth metal oxide can be judged, and the crystal dislocation density can be further calculated. The testing method is low in cost and short in period, and the defects that a traditional transmission electron microscope carries out tedious processing on a sample and X-ray diffraction cannot judge the type of crystal dislocation are overcome.

Drawings

FIG. 1 is a 200-fold optical microscope photograph of a crystal to be tested in example 1 after treatment;

FIG. 2 is a 500-fold optical microscope photograph of the crystal to be tested in example 1 after treatment;

FIG. 3 is a scanning electron microscope photograph of dislocations of the crystal to be tested of example 1, (a) screw dislocations (b) edge dislocations (c) mixed dislocations;

FIG. 4 is a 200-fold optical microscope photograph of the crystals to be tested in example 2 after treatment;

FIG. 5 is a graph showing the dislocation density of the crystal to be tested as a function of processing time in example 3.

Detailed Description

To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.

Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the invention, "a plurality" means at least two, e.g., two, three, etc., unless explicitly specified otherwise. In the description of the present invention, "a plurality" means at least one, e.g., one, two, etc., unless specifically limited otherwise.

The words "preferably," "more preferably," and the like in this disclosure mean embodiments of the invention that may, in some instances, provide certain benefits. However, other embodiments may be preferred, under the same or other circumstances. Furthermore, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention.

When a range of values is disclosed herein, the range is considered to be continuous and includes both the minimum and maximum values of the range, as well as each value between such minimum and maximum values. Further, when a range refers to an integer, each integer between the minimum and maximum values of the range is included. Further, when multiple range-describing features or characteristics are provided, the ranges may be combined. In other words, unless otherwise indicated, all ranges disclosed herein are to be understood to encompass any and all subranges subsumed therein.

Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.

The invention provides a dislocation detection method of rare earth metal oxide crystals, which comprises the following steps:

step S1: etching the rare earth metal oxide crystal by using a phosphoric acid solution with the mass fraction of 75-95% at the temperature of 80-200 ℃ for 10-60 minutes to prepare a pretreated sample;

step S2: and observing the pretreated sample, and detecting the dislocation characteristics of the rare earth metal oxide crystal.

Preferably, the phosphoric acid solution has a mass fraction of 80% to 90%, and specifically, the mass fraction may be, but not limited to, 80%, 81%, 82%, 83%, 84%, 85%, 86%, 87%, 88%, 89%, or 90%.

Further, the above observation manner may be, but is not limited to, using at least one of a scanning electron microscope and an optical microscope.

It will be appreciated that the dislocation characteristics described above include the type of dislocation and the dislocation density.

Specifically, the etching temperature may be 80 ℃ to 130 ℃, and preferably, the etching temperature may also be, but is not limited to, 80 ℃, 85 ℃, 90 ℃, 95 ℃, 100 ℃, 105 ℃, 110 ℃, 115 ℃, 120 ℃, 125 ℃ or 130 ℃.

Specifically, the etching time may be 30 minutes to 50 minutes, and preferably, the etching time may also be 10 minutes, 20 minutes, 30 minutes, 40 minutes, 50 minutes, or 60 minutes.

In one specific example, the rare earth metal oxide is lutetium oxide and the observed image shows:

the triangular pit is in a shape of a triangular pit, and a bottom recess in the middle of the pit is a triangular platform which is in a screw dislocation shape;

the triangular pit is in an inverted triangular cone shape and is edge dislocation;

the triangular pit is in a shape of a triangular pit, at least one triangular platform is arranged in the middle of the pit, and the center of the platform is an inverted triangular cone which is a mixed dislocation.

It will be appreciated that the observation of the dislocation types described above is by scanning electron microscopy.

Dislocations are the boundary between slipped and non-slipped parts in a crystal, and the crystal slips differently under different stress conditions. Dislocations are classified into edge dislocations, screw dislocations, and mixed dislocations, according to the geometrical characteristics of the slip direction and dislocation line orientation of atoms.

Mixed dislocations, i.e., any point on a dislocation line, can be decomposed into blade dislocations and screw dislocation components after vector decomposition. The shape of the dislocation lines in the crystal can be arbitrary, but the bernoulli vectors at each point on the dislocation lines are the same, only the knife-shaped and spiral-shaped components at each point are different.

In one embodiment, before step S1, the method further includes, sequentially grinding, polishing, first cleaning, and first drying the rare earth oxide crystal.

In one particular example, the step of grinding comprises: and (4) polishing the rare earth metal oxide crystal by using sand paper.

Furthermore, the mesh number of the sand paper is 2000-4000.

Preferably, the sandpaper has a mesh size of 2000, 2500, 3000 or 4000.

It will be appreciated that the sandpaper may be, but is not limited to, silicon carbide sandpaper.

In one specific example, the step of polishing comprises: polishing the grinded rare earth metal oxide crystal by using at least one of diamond, cerium oxide, aluminum oxide, silicon oxide, iron oxide, zirconium oxide and chromium oxide.

Preferably, the polishing treatment is preferably alumina.

The particle size of the alumina is 0.5 to 2 μm, and specifically, the particle size of the alumina may be, but not limited to, 0.5, 1, 1.5 or 2.5 μm.

The particle size of the alumina is preferably 1 μm.

In one specific example, the rare earth metal oxide crystal after the polishing treatment is subjected to a first cleaning treatment with a first organic solvent and a first inorganic solvent, respectively.

In one specific example, steps of a second washing and a second drying process of the pre-processed sample are further included before step S2 and after step S1.

In one specific example, the step of second cleaning comprises: and (3) carrying out secondary cleaning treatment on the pretreated sample by using a second organic solvent and a second inorganic solvent respectively.

In a specific example, the first organic solvent and the second organic solvent are each independently selected from at least one of ethanol and acetone.

The first inorganic solvent and the second inorganic solvent are deionized water.

The dislocation detection method of the rare earth metal oxide crystal provided by the invention comprises the following specific steps:

sequentially grinding, polishing, cleaning for the first time and drying for the first time on the rare earth metal oxide crystal; treating the rare earth metal oxide crystal by using a phosphoric acid solution with the mass fraction of 75-95% at the temperature of 80-200 ℃ for 10-60 minutes to prepare a pretreated sample; second washing and second drying of the pretreated sample; and respectively characterizing the pretreated sample by using an optical microscope and a scanning electron microscope, detecting the dislocation type of the rare earth metal oxide crystal and calculating the dislocation density.

By etching the rare earth metal oxide crystal, the dislocation in the crystal structure can be easily observed under an optical microscope and a scanning electron microscope, the type of the dislocation in the crystal structure of the rare earth metal oxide can be judged, and the crystal dislocation density can be further calculated. The test method has low cost and short period.

The dislocation detection method of the rare earth metal oxide crystal can be used for rapidly detecting the dislocation in the rare earth metal oxide crystal, accurately researching the dislocation type and dislocation distribution on the surface of the rare earth metal oxide crystal and determining the dislocation density. The method has a great application prospect in the aspects of quality evaluation, reliability evaluation, failure analysis and the like of the rare earth metal oxide crystal.

The dislocation detection method of the rare earth metal oxide crystal of the present invention will be described in further detail below with reference to specific examples, but in the following specific examples, all raw materials can be commercially available unless otherwise specified.

Example 1

The present embodiment provides a dislocation detection method for a rare earth metal oxide crystal, where the rare earth metal oxide crystal to be detected is a lutetium oxide crystal.

Grinding lutetium oxide crystals by using 2000-mesh silicon carbide abrasive paper, polishing the surfaces of the lutetium oxide crystals by using aluminum oxide polishing powder with the particle size of 1 mu m, sequentially cleaning the lutetium oxide crystals by using alcohol and deionized water, and finally drying the lutetium oxide crystals by using a blower;

50ml of phosphoric acid solution with the mass fraction of 85 percent is poured into a 200ml glass beaker, the beaker is placed in a constant-temperature heating stirrer, the treated lutetium oxide crystals are placed in the stirrer, and the temperature is raised to 100 ℃ for corrosion for 20 min;

taking out a pretreated sample, washing the surface by using deionized water, washing by using acetone, alcohol and deionized water in sequence, and finally drying by using a blower;

characterizing the surface appearance of the corroded sample by using an optical microscope and a scanning electron microscope;

the optical microscope images of the lutetium oxide crystal of this example at 200 times are shown in fig. 1 and 500 times are shown in fig. 2, and the specific morphologies of threading dislocations, edge dislocations, and mixed dislocations are shown in fig. 3 (a), (b), and (c), respectively, under a scanning electron microscope;

calculating the number of dislocations in the unit area of the lutetium oxide crystal to obtain the dislocation density, wherein the dislocation density of the lutetium oxide crystal is 11823 dislocations/cm²。

Example 2

The present embodiment provides a dislocation detection method for a rare earth metal oxide crystal, where the rare earth metal oxide crystal to be detected is a lutetium oxide crystal.

Grinding lutetium oxide crystals by adopting 2500-mesh silicon carbide abrasive paper, then using aluminum oxide polishing powder with the granularity of 1 mu m to perform surface polishing, firstly washing the surface by using deionized water, then sequentially using alcohol and deionized water to clean, and finally drying the surfaces of the crystals by using an air gun;

50ml of phosphoric acid solution with the mass fraction of 85 percent is poured into a 200ml glass beaker, the beaker is placed in a constant-temperature heating stirrer, the treated lutetium oxide crystals are placed in the stirrer, and the temperature is raised to 90 ℃ for corrosion for 20 min;

taking out a pretreated sample, washing the surface by using deionized water, then sequentially cleaning by using acetone, alcohol and deionized water, and finally drying by using a blower;

characterizing the surface appearance of the corroded sample by using an optical microscope;

an optical microscope photograph of the lutetium oxide crystal of this example is shown in fig. 4, in which the number of dislocations in the unit area of the lutetium oxide crystal is calculated to obtain a dislocation density, and the dislocation density of the lutetium oxide crystal of this example is 9064 dislocations/cm²。

Example 3

The present embodiment provides a dislocation detection method for a rare earth metal oxide crystal, where the rare earth metal oxide crystal to be detected is a lutetium oxide crystal.

Grinding lutetium oxide crystals by using 2000-mesh silicon carbide abrasive paper, polishing the surfaces of the lutetium oxide crystals by using aluminum oxide polishing powder with the particle size of 1 mu m, sequentially cleaning the lutetium oxide crystals by using alcohol and deionized water, and finally drying the lutetium oxide crystals by using a blower;

pouring 50ml of 85 mass percent phosphoric acid solution into a 200ml glass beaker, placing the beaker into a constant-temperature heating stirrer, placing the treated lutetium oxide crystal, heating to 100 ℃, taking out the lutetium oxide crystal every 10min, cleaning and drying the lutetium oxide crystal, and observing and calculating the dislocation density by adopting an optical microscope;

and (3) drawing a curve of the dislocation density of the crystal to be measured along with the etching time, counting the relation between the dislocation density and the processing time, and drawing the curve as shown in figure 5.

Comparative example 1

The comparative example provides a dislocation detection method for a rare earth metal oxide crystal, wherein the rare earth metal oxide crystal to be detected is a lutetium oxide crystal.

Grinding lutetium oxide crystals by using 2000-mesh silicon carbide abrasive paper, polishing the surfaces of the lutetium oxide crystals by using aluminum oxide polishing powder with the particle size of 1 mu m, sequentially cleaning the lutetium oxide crystals by using alcohol and deionized water, and finally drying the lutetium oxide crystals by using a blower;

50ml of phosphoric acid solution with the mass fraction of 85 percent is poured into a 200ml glass beaker, the beaker is placed in a constant-temperature heating stirrer, the treated lutetium oxide crystals are placed in the stirrer, and the temperature is raised to 50 ℃ for corrosion for 60 min;

taking out a pretreated sample, washing the surface by using deionized water, washing by using acetone, alcohol and deionized water in sequence, and finally drying by using a blower;

characterizing the surface appearance of the corroded sample by using an optical microscope and a scanning electron microscope;

calculating the number of dislocation in unit area to obtain dislocation density, wherein the dislocation density of the lutetium oxide crystal of the comparative example is 2560/cm²。

Comparative example 2

The comparative example provides a dislocation detection method for a rare earth metal oxide crystal, wherein the rare earth metal oxide crystal to be detected is a lutetium oxide crystal.

Grinding lutetium oxide crystals by using 2000-mesh silicon carbide abrasive paper, polishing the surfaces of the lutetium oxide crystals by using aluminum oxide polishing powder with the particle size of 1 mu m, sequentially cleaning the lutetium oxide crystals by using alcohol and deionized water, and finally drying the lutetium oxide crystals by using a blower;

pouring 50ml of phosphoric acid solution into a 200ml glass beaker, placing the beaker in a constant-temperature heating stirrer, adding the treated lutetium oxide crystals, and heating to 210 ℃ to corrode the lutetium oxide crystals for 10 min;

taking out a pretreated sample, washing the surface by using deionized water, washing by using acetone, alcohol and deionized water in sequence, and finally drying by using a blower;

characterizing the surface appearance of the corroded sample by using an optical microscope and a scanning electron microscope;

calculating the number of dislocation in unit area to obtain the dislocation density, wherein the dislocation density of the lutetium oxide crystal of the comparative example is 5069/cm²。

Comparative example 3

The comparative example provides a dislocation detection method for a rare earth metal oxide crystal, wherein the rare earth metal oxide crystal to be detected is a lutetium oxide crystal.

Grinding lutetium oxide crystals by using 2000-mesh silicon carbide abrasive paper, polishing the surfaces of the lutetium oxide crystals by using aluminum oxide polishing powder with the particle size of 1 mu m, sequentially cleaning the lutetium oxide crystals by using alcohol and deionized water, and finally drying the lutetium oxide crystals by using a blower;

pouring 50ml of sulfuric acid solution into a 200ml glass beaker, placing the beaker in a constant-temperature heating stirrer, adding the treated lutetium oxide crystals, and heating to 100 ℃ to corrode the lutetium oxide crystals for 20 min;

taking out a pretreated sample, washing the surface by using deionized water, washing by using acetone, alcohol and deionized water in sequence, and finally drying by using a blower;

and (5) characterizing the surface appearance of the corroded sample by using an optical microscope and a scanning electron microscope, and observing the appearance that the dislocation exists on the surface of the crystal.

Comparative example 4

The comparative example provides a dislocation detection method for a rare earth metal oxide crystal, wherein the rare earth metal oxide crystal to be detected is a lutetium oxide crystal.

Grinding lutetium oxide crystals by using 2000-mesh silicon carbide abrasive paper, polishing the surfaces of the lutetium oxide crystals by using aluminum oxide polishing powder with the particle size of 1 mu m, sequentially cleaning the lutetium oxide crystals by using alcohol and deionized water, and finally drying the lutetium oxide crystals by using a blower;

pouring 50ml of nitric acid solution into a 200ml glass beaker, placing the beaker in a constant-temperature heating stirrer, adding the treated lutetium oxide crystals, and heating to 100 ℃ to corrode the lutetium oxide crystals for 20 min;

taking out a pretreated sample, washing the surface by using deionized water, washing by using acetone, alcohol and deionized water in sequence, and finally drying by using a blower;

and (5) characterizing the surface appearance of the corroded sample by using an optical microscope and a scanning electron microscope, and observing the appearance that the dislocation exists on the surface of the crystal.

The invention also provides the influence of the acid solution on the dislocation density of the sample to be detected along with the increase of the corrosion treatment time in the sample corrosion treatment process, and proves that the dislocation density only has the tendency of increasing and then decreasing along with the treatment time.

The dislocation detection method of the rare earth metal oxide crystal can be used for rapidly detecting the dislocation in the rare earth metal oxide crystal, accurately researching the dislocation type and dislocation distribution on the surface of the rare earth metal oxide crystal and determining the dislocation density. The method has a great application prospect in the aspects of quality evaluation, reliability evaluation, failure analysis and the like of the rare earth metal oxide crystal.

The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.

The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.