阅读说明：本技术 一种金刚石对顶压砧用精细样品的制备方法 (Preparation method of fine sample for diamond opposite-vertex anvil press ) 是由 廖益传 路超 侯琪玥 肖大武 张厚亮 何立峰 李守瑞 于 2019-11-05 设计创作，主要内容包括：本发明公开了金刚石对顶压砧用精细样品的制备方法,包括以下步骤：A、将初始样品、初始压标材料和封垫固定在预制样品台上,再将预制样品台转移至FIB-SEM双束系统中并抽真空；B、利用离子束对初始样品进行切割,得到预期大小和形状的待测样品；C、利用机械手将待测样品转移并固定在所述封垫的样品腔内壁上；D、利用离子束对初始压标材料进行切割,得到预期大小和形状的压标；E、利用机械手将压标转移并固定在所述封垫的样品腔内壁上；步骤B、步骤C、步骤D和步骤E的顺序可调,需实现先切割再转移固定并且最后得到所述金刚石对顶压砧用精细样品。本发明能较好地固定金刚石对顶压砧样品和压标,提高装金刚石对顶压砧样品的成功率。(The invention discloses a preparation method of a fine sample for a diamond anvil cell, which comprises the following steps: A. fixing an initial sample, an initial marking material and a sealing pad on a prefabricated sample table, transferring the prefabricated sample table to an FIB-SEM dual-beam system, and vacuumizing; B. cutting the initial sample by using an ion beam to obtain a sample to be detected with an expected size and shape; C. transferring and fixing a sample to be detected on the inner wall of the sample cavity of the sealing pad by using a manipulator; D. cutting the initial marking material by using an ion beam to obtain a marking with an expected size and shape; E. transferring and fixing the pressure mark on the inner wall of the sample cavity of the sealing pad by using a manipulator; the sequence of the step B, the step C, the step D and the step E can be adjusted, cutting is firstly carried out, then transferring and fixing are carried out, and finally the fine sample for the diamond anvil cell is obtained. The diamond anvil cell sample fixing device can better fix the diamond anvil cell sample and the pressure mark, and improve the success rate of diamond anvil cell sample installation.)

1. A preparation method of a fine sample for a diamond anvil cell is characterized by comprising the following steps:

A. fixing an initial sample, an initial marking material and a sealing pad on a prefabricated sample table, transferring the prefabricated sample table to an FIB-SEM dual-beam system, and vacuumizing;

B. cutting the initial sample by using an ion beam to obtain a sample to be detected with an expected size and shape;

C. transferring and fixing the sample to be detected on the inner wall of the sample cavity of the sealing pad by using a manipulator;

D. cutting the initial marking material by using an ion beam to obtain a marking with an expected size and shape;

E. transferring and fixing the pressure mark on the inner wall of the sample cavity of the sealing pad by using a manipulator;

and the sequence of the step B, the step C, the step D and the step E can be adjusted, cutting is firstly carried out, then transfer and fixation are carried out, and finally the fine sample for the diamond anvil cell is obtained.

2. The method for preparing a fine sample for a diamond anvil cell according to claim 1, wherein the inclination of the plane of the preliminary sample stage is 0 °, the FIB-SEM dual beam system is a focused ion beam electron beam microanalysis system and the angle α between the ion beam and the electron beam is 45 to 55 °.

3. The method for preparing a fine sample for a diamond anvil according to claim 2, wherein in the cutting by the ion beam in the steps B and D, the ion beam is made perpendicular to the surfaces of the initial sample and the initial marking material after rotating the sample stage by an angle α.

4. The method of preparing a fine sample for a diamond anvil according to claim 1, wherein the initial sample, the initial marking material and the seal are conductive materials.

5. The method for preparing a fine sample for a diamond anvil cell according to claim 4, wherein the initial sample, the initial stamp material and the seal are a metallic material or a semiconductor material.

6. The method for preparing a fine sample for a diamond anvil cell according to claim 1, wherein the length, width, height and size of the sample cavity of the seal are several micrometers to several hundred micrometers, the length, width, height and size of the sample to be tested and the stamp are several micrometers to several hundred micrometers, and the length, width, height and size of the sample to be tested and the stamp are smaller than the length, width, height and size of the sample cavity.

7. The method for preparing a fine sample for a diamond anvil cell according to claim 1 or 6, wherein the distribution positions of the sample to be measured and the stamp in the sample chamber can be arbitrarily set.

8. The method for preparing a fine sample for a diamond anvil cell according to claim 7, wherein the sample to be measured and the stamp are symmetrically placed in the sample chamber, and the sample to be measured and the stamp do not protrude from the upper and lower surfaces of the sample chamber.

Technical Field

The invention belongs to the field of preparation of diamond opposite-vertex anvil cell samples, relates to a preparation method of a fine sample for a diamond opposite-vertex anvil cell, and particularly relates to a preparation method of a dozen-micron regular fine sample for the diamond opposite-vertex anvil cell.

Background

The Diamond Anvil Cell (DAC) consists of one pair of diamond anvil cells and sealing pad. The sample and the pressure measuring ruby are simultaneously placed in the diamond anvil sealing pad, and the anvil is screwed tightly to obtain high pressure of hundreds of GPa. The ultra-high pressure condition generated by the method enables people to more deeply know the physical and chemical properties of the substance under high pressure.

The existing diamond anvil cell sample preparation mainly adopts a scalpel to cut a large sample material into a size suitable for a sample cavity of a standby press, selects a small sample with a size suitable for the sample cavity of the standby press, and adopts a metal fine needle to pick the small sample into the diamond anvil cell sample cavity. The sample obtained by the method is irregular in shape and size, and is not beneficial to measuring deformation in the later period.

Because the sample cavity of the diamond anvil is very small, generally in the order of tens of microns to hundreds of microns, the sample is smaller than the size of the sample cavity. After the sample and the pressure mark are picked into the sample cavity, a pressure transmission medium such as liquid argon or liquid nitrogen or liquid helium needs to be injected. In the process of injecting the pressure transmission medium, because the sample and the pressure mark are both small, the flow of the fluid can cause the movement of the placed sample or the pressure mark, and the sample or the pressure mark can move to an unexpected position, thereby causing sample loading failure and low sample loading success rate. Because the sample is loaded by the traditional method, the sample is not firmly fixed, and the sample is easy to overflow during the pressurizing process.

Therefore, it is necessary to develop a method for fixing the sample and pressing the label better, so as to improve the success rate of sample loading.

Disclosure of Invention

The invention aims to overcome the problems in the prior art and provide a method for preparing a fine sample for a diamond anvil cell, which can better fix a diamond anvil cell sample and a label, so that the success rate of loading the diamond anvil cell sample is improved.

The invention provides a preparation method of a fine sample for a diamond anvil cell, which comprises the following steps:

A. fixing an initial sample, an initial marking material and a sealing pad on a prefabricated sample table, transferring the prefabricated sample table to an FIB-SEM dual-beam system, and vacuumizing;

B. cutting the initial sample by using an ion beam to obtain a sample to be detected with an expected size and shape;

C. transferring and fixing the sample to be detected on the inner wall of the sample cavity of the sealing pad by using a manipulator;

D. cutting the initial marking material by using an ion beam to obtain a marking with an expected size and shape;

E. transferring and fixing the pressure mark on the inner wall of the sample cavity of the sealing pad by using a manipulator;

and the sequence of the step B, the step C, the step D and the step E can be adjusted, cutting is firstly carried out, then transfer and fixation are carried out, and finally the fine sample for the diamond anvil cell is obtained.

According to one embodiment of the method for preparing the fine sample for the diamond anvil cell, the inclination angle of the plane of the prefabricated sample stage is 0 °, the FIB-SEM dual-beam system is a focused ion beam and electron beam microanalysis system, and the included angle alpha between the ion beam and the electron beam is 45-55 °.

According to one embodiment of the method for preparing a fine sample for a diamond anvil according to the present invention, in the cutting using the ion beam in the steps B and D, the ion beam is perpendicular to the surfaces of the initial sample and the initial marking material after rotating the sample stage by an angle α.

According to one embodiment of the method for preparing a fine sample for a diamond anvil according to the present invention, the initial sample, the initial marking material and the seal are conductive materials.

According to one embodiment of the method for preparing a fine sample for a diamond anvil according to the present invention, the initial sample, the initial marking material and the seal are metallic materials or semiconductor materials.

According to one embodiment of the method for preparing the fine sample for the diamond anvil, the length, width and height of the sample cavity of the sealing pad are several micrometers to hundreds of micrometers, the length, width and height of the sample to be tested and the stamp are several micrometers to hundreds of micrometers, and the length, width and height of the sample to be tested and the stamp are smaller than the length, width and height of the sample cavity.

According to one embodiment of the preparation method of the fine sample for the diamond anvil, the distribution positions of the sample to be measured and the stamps in the sample cavity can be set at will.

According to one embodiment of the preparation method of the fine sample for the diamond anvil cell, the sample to be tested and the pressing mark are symmetrically arranged in the sample cavity, and the sample to be tested and the pressing mark do not exceed the upper surface and the lower surface of the sample cavity.

Compared with the prior art, the method utilizes an FIB-SEM double-beam system to carry out the preparation process of the in-situ diamond opposite-vertex anvil sample, realizes the fixation of the sample to be detected and the stamp in the seal pad sample cavity, and can customize the shape, size and position of the sample to be detected and the stamp as required; the randomness of the traditional sample preparation method is avoided, and the process of selecting samples is omitted; random movement of the sample and the pressure mark in the DAC sample loading process is reduced, and overflow of the sample in the pressurizing process is also reduced; the method is favorable for improving the success rate of DAC sample loading, reduces the labor intensity and saves the time and material consumption.

Drawings

Fig. 1 shows a flowchart of a method for preparing a fine sample for a diamond-to-anvil according to an exemplary embodiment of the present invention.

FIG. 2 shows a schematic of the location of the initial sample, initial marking material and seal on the pre-prepared sample stage.

Fig. 3a shows a schematic position diagram of the electron beam, the ion beam and the initial sample, the initial marking material and the sealing pad when the sample stage is at the 0 ° position, and fig. 3b shows a schematic position diagram of the electron beam, the ion beam and the initial sample, the initial marking material and the sealing pad when the sample stage is rotated by an angle α.

FIG. 4 is a schematic diagram showing the use of a robot to transfer and fix the cut sample to be tested to the inner wall of the sample chamber of the seal.

FIG. 5 shows a schematic view of the completed fixing of the sample to be tested and the stamp to the inner wall of the sample chamber of the seal.

Fig. 6a and 6b show electron beam imaging photographs of the sample to be measured cut in example 1.

FIG. 7a is an electron beam image of the sample to be tested extracted by the manipulator in example 1, FIG. 7b is an electron beam image of the sample to be tested transferred to the inner wall of the sample cavity of the seal pad by the manipulator in example 1, FIG. 7c is an electron beam image of the sample to be tested fixed to the inner wall of the sample cavity of the seal pad and the connection between the manipulator and the sample in example 1, and FIG. 7d and FIG. 7e are electron beam images of the sample to be tested fixed to the inner wall of the sample cavity of the seal pad after the manipulator is withdrawn in example 1.

Fig. 8a and 8b show electron beam imaging photographs of cutting a sample to be measured in example 2.

Fig. 9a shows an electron beam image of the sample to be tested transferred to the inner wall of the sample cavity of the seal pad by using the manipulator in example 2, fig. 9b shows an ion beam image of the sample to be tested transferred to the inner wall of the sample cavity of the seal pad by using the manipulator in example 2, fig. 9c shows an electron beam image of the sample to be tested fixed to the inner wall of the sample cavity of the seal pad in example 2, and fig. 9d shows an electron beam image of the sample to be tested fixed to the inner wall of the sample cavity of the seal pad after exiting the manipulator in example 2.

Fig. 10 shows an electron beam image of a Cu stamper cut using an ion beam in example 2.

FIG. 11a shows an electron beam image of the cut stamp transferred by the robot in example 2, FIG. 11b shows an ion beam image of the stamp fixed to the inner wall of the seal sample chamber after the robot is withdrawn in example 2, and FIG. 11c shows an electron beam image of the stamp fixed to the inner wall of the seal sample chamber after the robot is withdrawn in example 2.

FIG. 12a shows the image of the electron beam of the embodiment 3 in which the pressing mark is fixed on the inner wall of the cavity of the seal after the robot is withdrawn, and FIG. 12b shows the image of the ion beam of the embodiment 3 in which the pressing mark is fixed on the inner wall of the sample cavity of the seal after the robot is withdrawn.

FIG. 13a shows an electron beam image of a sample cut by the transfer robot in example 3, and FIG. 13b shows an electron beam image of a sample fixed on the inner wall of the sample cavity of the seal pad after exiting the robot in example 3.

FIG. 14a shows an electron beam image of the sample to be tested cut in example 4, FIG. 14b shows an electron beam image of the sample to be tested transferred to the inner wall of the sample cavity of the seal pad by using the manipulator in example 4, and FIG. 14c shows an electron beam image of the sample to be tested fixed on the inner wall of the sample cavity of the seal pad after the manipulator is withdrawn in example 4.

FIG. 15a shows the electron beam image of the Cu stamp cut by ion beam in example 4, FIG. 15b shows the electron beam image of the stamp fixed on the inner wall of the sample chamber by the robot in example 4, and FIG. 15c shows the electron beam image of the stamp and the sample on the inner wall of the sealed sample chamber after the robot is withdrawn in example 4.

Description of reference numerals:

1-initial sample, 2-initial labeling material, 3-sealing pad, 4-sample cavity, 5-prefabricated sample stage, 6-electron beam, 7-ion beam, 8-mechanical arm, 9-sample to be detected, 10-sample cavity side wall and 11-labeling.

Detailed Description

All of the features disclosed in this specification, or all of the steps in any method or process so disclosed, may be combined in any combination, except combinations of features and/or steps that are mutually exclusive.

Any feature disclosed in this specification may be replaced by alternative features serving equivalent or similar purposes, unless expressly stated otherwise. That is, unless expressly stated otherwise, each feature is only an example of a generic series of equivalent or similar features.

The method for preparing a fine sample for a diamond anvil according to the present invention will be described in detail with reference to the accompanying drawings. The method is carried out based on the existing FIB-SEM double-beam system with an included angle beta of 45-55 degrees between an ion beam and an electron beam, the fixing of a sample to be detected and a pressing mark in a sealing pad is realized, the shape, the size and the position of the sample to be detected and the pressing mark can be customized according to requirements, wherein the beta is usually 52 degrees.

Fig. 1 shows a flowchart of a method for preparing a fine sample for a diamond-to-anvil according to an exemplary embodiment of the present invention. As shown in fig. 1, the method for preparing a fine sample for a diamond anvil according to an exemplary embodiment of the present invention mainly includes the following steps.

Step A:

FIG. 2 shows a schematic of the location of the initial sample, initial marking material and seal on the pre-prepared sample stage. As shown in fig. 2, the initial sample 1, the initial stamp material 2 and the seal 3 are fixed on a preliminary sample stage 5, and the preliminary sample stage 5 is transferred to a FIB-SEM dual beam system and evacuated. Wherein the seal 3 has a sample chamber 4 therein.

And B:

the initial sample 1 is cut by the ion beam 6 to obtain a sample 9 to be measured of a desired size and shape.

And C:

the sample 9 to be measured is transferred and fixed on the inner wall 10 of the sample chamber of the seal 3 by the manipulator 8.

Step D:

the initial marking material 2 is cut by the ion beam 6 to obtain a marking 11 of a desired size and shape.

Step E:

the stamp 11 is transferred and fixed to the inner wall 10 of the sample chamber of the seal 3 by means of the robot arm 8.

And C, the sequence of the step B, the step C, the step D and the step E is adjustable, cutting is firstly carried out, then transfer and fixation are carried out, and finally the fine sample for the diamond anvil cell is obtained.

That is, the step B, C, D, E is not required to be performed in strict sequence, and may be performed in the sequence of B, C, D, E, or may be performed in the sequence of D, E, B, C, B, D, C, E, D, B, E, C, or the like, as long as the sample to be tested or the pressure mark can be fixed on the inner wall of the sample cavity of the seal pad.

Fig. 3a shows a schematic diagram of the positions of the electron beam, the ion beam and the initial sample, the initial marking material and the seal pad when the sample stage is at the 0 ° position, fig. 3b shows a schematic diagram of the positions of the electron beam, the ion beam and the initial sample, the initial marking material and the seal pad when the sample stage rotates by an angle α, fig. 4 shows a schematic diagram of transferring and fixing the cut sample to be tested to the inner wall of the seal pad sample cavity by using a manipulator, and fig. 5 shows a schematic diagram of completing the fixing of the sample to be tested and the marking to the inner wall of the seal pad sample cavity.

As shown in fig. 3a to 5, the inclination of the plane of the pre-fabricated sample stage 5 is 0 °, the FIB-SEM dual beam system is a focused ion beam electron beam microanalysis system, and the angle α between the ion beam 7 and the electron beam 6 is 45 to 55 °. When the ion beam is used for cutting, the ion beam is perpendicular to the surfaces of the initial sample and the initial marking material after the sample table is rotated by an angle alpha. After cutting, respectively transferring and fixing the cut sample to be measured and the pressing mark on the inner wall of the sample cavity of the sealing pad by utilizing a manipulator, thus obtaining the fine sample for the diamond opposite-vertex pressing anvil.

The initial sample 1, the initial stamp material 2 and the sealing pad 3 should Be conductive materials, preferably metal materials or semiconductor materials, for example, the stamp may Be Cu, ruby, piezoelectric ceramic, etc., the sample may Be, Al, Fe, W, alumina, Ag, zirconium hydride, lanthanum hydride, silicon dioxide, etc., and the sealing pad may Be Re, stainless steel, tungsten, tantalum, etc. The length, width and height of the sample cavity 4 of the sealing pad 3 are several micrometers to hundreds of micrometers, the length, width and height of the sample 9 to be tested and the pressure mark 11 are several micrometers to hundreds of micrometers, and the length, width and height of the sample 9 to be tested and the pressure mark 11 are smaller than the length, width and height of the sample cavity 4.

The distribution positions of the sample 9 to be measured and the pressure marks 11 in the sample cavity 4 can be arbitrarily set, and are preferably symmetrically arranged, and the sample to be measured and the pressure marks do not exceed the upper surface and the lower surface of the sample cavity.

Wherein, the transfer and fixation of the sample to be tested or the stamp can be prepared by the following method: depositing Pt between a sample to be detected and a manipulator to connect the sample to be detected with the manipulator, and then cutting off the connection between the sample to be detected and an initial main body sample; moving the manipulator to enable the sample or the pressure mark to be detected to be close to the inner wall of the sample cavity of the sealing pad and be positioned between the upper surface and the lower surface of the sealing pad; depositing Pt between the sample or the pressure mark to be detected and the inner wall of the seal pad sample cavity to connect the sample or the pressure mark to be detected and the inner wall of the seal pad sample cavity, and connecting the sample or the pressure mark to be detected and the manipulator to obtain the sample or the pressure mark to be detected fixed on the inner wall of the seal pad sample cavity.

Through the adjustment of the method, the fixing of the sample to be detected and the pressure mark in the seal pad sample cavity is realized, the shape, the size and the position of the sample to be detected and the pressure mark can be customized according to the requirement, the randomness of the traditional sample preparation method is avoided, and the process of selecting the sample is omitted.

The present invention will be further described with reference to specific examples, but the scope of the present invention is not limited to the examples of the present invention.