CN103128657A - Clamp used for electron back scattering diffraction sample vibration polishing and use method thereof - Google Patents

Abstract

The invention relates to a fixture for vibratory polishing of an electron backscattered diffraction sample, which includes a sample, and is characterized in that: the sample is arranged at the bottom of a second cylinder, and the first cylinder is sequentially arranged above the second cylinder. The cylinder and the weight plate are provided with a first stud in the horizontal direction of the sample, and the first stud extends from a through hole in the side wall of the second cylinder into the inner side of the second cylinder, and in the sample A second stud is arranged vertically on the upper end, and the second stud extends into the second cylinder from the through holes of the second cylinder, the first cylinder and the weight plate. At the same time, the invention also provides a method for using a jig used for vibration polishing of electron backscattered diffraction samples. The fixture provided by the present invention can be used to effectively solve the problem of difficult sample preparation due to the small size of the electron backscattered diffraction sample, the problem of poor vibratory polishing effect due to the small weight of the sample, and the problem of being compatible with a specific crystal orientation. The processing problem of the surface of the sample of a certain relationship.

Description

A fixture for vibrating polishing of electron backscattered diffraction samples and its application method

technical field

The invention relates to a fixture and a using method thereof, in particular to a fixture for vibration polishing of an electron backscattered diffraction sample and a using method thereof.

Background technique

Electron Backscattered Diffraction (EBSD, that is, Electron BackScattered Diffraction), that is, a fixed electron beam hits an inclined crystal sample to form a diffraction pattern on the fluorescent screen, which shows the crystal structure of the sample. It is mainly used to quickly obtain crystallographic information of crystalline materials. It can analyze the texture and orientation difference between grains, the analysis of grain size and shape distribution, the analysis of grain boundaries, sub-grains and twins, and the analysis of strain and recrystallization. , as well as phase identification and phase content calculation, etc., to solve problems in the process of crystallization, thin film preparation, semiconductor devices, deformation, recrystallization, phase change, fracture, corrosion, etc.

With the development of electron backscatter diffraction analysis technology, there are more and more experimental requirements for electron backscatter diffraction analysis in daily scientific research and production work. Since electron backscatter diffraction analysis has high requirements for samples, the preparation of electron backscatter diffraction analysis samples has become an important research direction. The limitation of the electron backscatter diffraction analysis on the sample mainly comes from two aspects: one is that the sample size should not be too large because the electron backscatter diffraction analysis needs to tilt the sample at a certain angle; Scattering diffraction analysis has high requirements on the thickness of the strain residual layer on the surface of the sample. Once the strain residual layer is thick, it will have a serious impact on the quality of the diffraction pattern, and may even cause the pattern to fail to be produced.

The above-mentioned restrictive requirements for samples make the following difficulties in preparing samples:

First, the small sample size itself increases the difficulty of sample preparation. The small size of the sample will inevitably make it difficult to hold the sample during the grinding and polishing stage, thus increasing the difficulty of grinding and polishing, and even the situation that the sample cannot be held and the sample will fly out, which will affect the sample preparation personnel. pose a threat to personal safety and easily destroy the sample;

Secondly, the electron backscatter diffraction analysis has high requirements on the surface stress state of the sample, so in general, multiple polishing methods are mainly used to reduce the surface stress, that is, the initial polishing is carried out under high-speed, coarse polishing particle polishing liquid, and then at low Fine polishing is carried out under the rotating speed and fine polishing particle polishing liquid. For some special samples, 3-4 times of polishing are even required, which greatly reduces the efficiency of sample preparation and cannot meet the needs of scientific research and production; another method is to use vibration polishing technology to remove the surface of the sample. stress layer. The principle of vibration polishing is to use the vibration and self-weight of the sample to reduce the surface strain layer, which is mainly used for polishing of soft materials. However, the requirements of the electron backscatter diffraction analysis sample itself on the sample size make its own weight unable to meet the weight requirements of vibration polishing. Moreover, the existing sample fixtures cannot meet the requirements of flexible counterweighting for different polished samples, and only a single counterweight can be used, that is, the optimal counterweight is performed according to the requirements of the sample.

Thirdly, the original sample preparation method has high requirements on the parallelism of the sample before polishing. It is required that the upper and lower surfaces of the sample must be parallel before the sample is prepared, because the parallelism of the upper and lower surfaces of the sample cannot be adjusted during the sample preparation process. In addition, if it is necessary to observe the orientation of the special plane of the sample, it cannot be achieved in the traditional sample preparation process.

For the preparation and processing of samples, there are mainly the following patent documents in China at present:

Application number: 200520126668.7, utility model name: multi-function grinding fixture for spectroscopic analysis samples. Its main feature is that the front end of the handle is fixed on the adjustable looper, four symmetrical concave sockets are set on the edge of the adjustable looper, and adjusting screws are provided on the arc-shaped pieces between adjacent concave sockets. , Fix non-magnetic materials and samples of different shapes and thicknesses through concave sockets and adjusting screws. However, the fixture provided by this utility model cannot ensure the fixation of the sample with a special orientation, that is, the surface of the sample that has a certain relationship with the specific crystal orientation cannot be prepared, and the weight cannot be flexibly balanced.

Application number: 200620047017.3, utility model name: a sample polishing jig. The fixture provided by the utility model places the sample by setting two concave cavities, and the fastening screw extends from the side section of the body into the concave cavity of the body to clamp and fix the sample, and a magnetic body is set in the body cavity to absorb the sample. Sample. However, this type of fixture cannot prepare non-magnetic specimens, has no flexible weighting, and cannot prepare specimen surfaces that have a certain relationship with specific crystal orientations.

Contents of the invention

In order to solve the above existing problems, the object of the present invention is to provide a fixture for vibration polishing of electron backscattered diffraction samples, which is used to effectively solve the problem of difficult sample preparation due to the small size of electron backscattered diffraction samples, The problem of poor vibration polishing effect due to the small weight of the sample and the processing of the surface of the sample that has a certain relationship with the specific crystal orientation. At the same time, the present invention also provides the use method of the jig for vibration polishing of electron backscattered diffraction samples.

To achieve the above object, the present invention takes the following technical solutions:

A fixture for vibratory polishing of electron backscattered diffraction samples, the fixture is used to hold the sample, and is characterized in that:

The sample is arranged at the bottom of the second cylinder,

A first cylinder and a weight plate are sequentially arranged above the second cylinder,

A first stud is arranged in the horizontal direction of the sample, and the first stud extends from a through hole in the side wall of the second cylinder into the inside of the second cylinder,

A second stud is arranged vertically on the upper end of the sample, and the second stud extends into the second cylinder from the through holes of the second cylinder, the first cylinder and the weight plate.

According to a jig for vibration polishing of electron backscattered diffraction samples provided by the present invention, the number of the first studs is 4, the number of the second studs is 4, and the The four first studs are arranged in a cross shape, and the four second studs are arranged in a square shape.

According to a jig for vibratory polishing of electron backscattered diffraction samples provided by the present invention, the second stud is provided with a nut at one end of the weight plate, and the through hole is a threaded through hole.

According to a jig for vibration polishing of electron backscattered diffraction samples provided by the present invention, the diameter of the first cylinder is 25-35 mm, and the diameter of the second cylinder is 15-25 mm.

According to a jig for vibration polishing of electron backscattered diffraction samples provided by the present invention, the second cylinder is a hollow cylinder with an opening at the bottom.

According to a jig for vibratory polishing of electron backscattered diffraction samples provided by the present invention, the first stud, the second stud, the first cylinder and the second cylinder are selected from one or two Made of more than one low-density metal, the low-density metal includes aluminum, titanium, and magnesium.

According to a jig for vibration polishing of electron backscattered diffraction samples provided by the present invention, the weight plate is processed by mixing several metals, and the metals include aluminum, iron and molybdenum.

In addition, the present invention also provides a method for using a jig for vibratory polishing of electron backscattered diffraction samples, and the technical scheme is as follows:

The sample is placed horizontally, and the face to be processed is placed downward, and it is characterized in that it also includes the following steps:

(a) Place the fixture vertically above the sample;

(b) Adjust the first stud so that the first stud fixes the sample from the side;

(c), adjust the second stud so that the second stud fixes the sample from above;

(d), grinding and polishing the sample;

(e), adjust the overall total amount of the sample and the fixture through the weight plate;

(f), the sample is subjected to vibration polishing treatment;

(g) Prepare the required sample.

According to a method for using a jig for vibration polishing of an electron backscattered diffraction sample provided by the present invention, when the sample is an irregular small sample, the following steps are also included:

(1), adjust the second stud described in the step (c), so that the second stud is attached to the upper surface of the sample;

(2), adjust the first stud according to the steps, so that the first stud fixes the sample from the side;

(3), according to the steps, the sample is ground and polished, so that the lower surface of the sample is flush with the lower surface of the first cylinder;

(4), take out the treated sample in step (3), invert the sample and fix the sample according to step (1) and step (2);

(5), according to the step (d), the sample in the step is ground and polished, so that the lower surface of the sample is flush with the upper surface;

(6), according to said step (e) and step (f), the sample obtained after step (5) is processed is processed;

(7) Prepare the required samples.

According to a jig for vibratory polishing of electron backscattered diffraction samples provided by the present invention, when the sample is a sample with a special orientation, the following steps are also included:

(A), determine the angle of the sample surface and special crystal orientation prepared in the step (g) by X-ray diffractometer;

(B), adjust the second stud described in the step (c), so that the sample made in the step (f) forms the angle determined in the step (A);

(C), repeat step (3) to step (6) to obtain the required sample.

The beneficial effects of a jig for vibratory polishing of electron backscattered diffraction samples and its use method provided by the present invention are as follows:

(1) By setting the first cylinder and the second cylinder, the size of the sample is expanded, thereby reducing the difficulty of sample preparation and improving the efficiency of sample preparation;

(2) Through the cooperation of the weight plate and the fixture, the overall weight of the sample and the fixture can be flexibly adjusted to meet the requirements of different metals and sample surface conditions on the weight of the polished surface during vibration polishing, thereby improving the vibration polishing of the sample. Surface quality, improve work efficiency;

(3) By setting the first stud and the second stud, the stability and easy clamping of the sample can be ensured during processing, so the irregular small sample that is not easy to cut can be processed into a small sample whose upper and lower surfaces are parallel. sample;

(4) By setting the first stud and the second stud, the stability and easy clamping of the sample can be ensured during processing, so it is possible to prepare a sample with a certain angle to the special crystal orientation (that is, the special orientation test Sample).

Description of drawings

FIG. 1 is a schematic structural view of a jig for vibratory polishing of electron backscattered diffraction samples provided by the present invention.

FIG. 2 is a top view of FIG. 1 .

Fig. 3 is a schematic structural view of a jig for vibrating polishing of electron backscattered diffraction samples provided by the present invention when processing small irregular samples.

Fig. 4 is a schematic structural view of the lower surface of the small irregular sample in Fig. 3 after processing.

Fig. 5 is a schematic diagram of the structure of the irregular small sample in Fig. 4 after being turned upside down.

Fig. 6 is a schematic structural view of the lower surface of the small irregular sample in Fig. 5 after processing.

Fig. 7 is a schematic diagram of the structure of a sample prepared with a special orientation.

In the figure, 1, the first cylinder 2, the first stud 3, the weight plate 4, the sample 5, the nut 6, the second cylinder 7, the second stud 8, the through hole.

Detailed ways

A jig for vibratory polishing of electron backscattered diffraction samples provided by the present invention and its usage method will be further explained below in conjunction with the accompanying drawings.

First, the structure of the fixture used for vibration polishing of electron backscattered diffraction samples is as follows:

As shown in Figure 1, the sample 4 is arranged at the bottom of the second cylinder 6, the second cylinder 6 is a hollow cylinder with an open lower end, and the upper end of the second cylinder 6 is sequentially provided with the first cylinder 1 and the counterweight The sheet 3 is provided with a first stud 2 in the horizontal direction of the sample 4, and the first stud 2 extends into the inside of the second cylinder 6 from the through hole 8 on the side wall of the second cylinder 6, and in the The upper end of the sample 4 is provided with a second stud 7 in the vertical direction, and the second stud 7 extends into the second cylinder 6 from the through hole 8 of the second cylinder 6, the first cylinder 1 and the weight plate 3 , the second stud 7 is provided with a nut 5 at one end of the weight plate 3 for fixing the weight plate 3 .

Wherein, the through hole 8 is a threaded through hole; the diameter of the first cylinder 1 is 25-35mm, and the diameter of the second cylinder 6 is 15-25mm; the first stud 2, the second The stud 7, the first cylinder 1 and the second cylinder 6 are made of one or more than two low-density metals, the low-density metals include aluminum, titanium, magnesium, and the density is lower than Fe7.86 Defined as low density. Its material can be a single metal, or two or more, that is, an alloy; the weight plate 3 is processed by mixing several metals, and the metals include aluminum, iron and molybdenum, and the purpose of mixing light and heavy metals It is to change the weight of the weight plate without changing the size of the weight plate. The weight of the weight plate can be flexibly changed through the change of the weight plate of different densities, so as to achieve the weight requirements of different styles of polishing. The function of the first stud 2 is to fix the sample 4, so that the sample 4 moves together with the fixture; the function of the second stud 7 is to prevent the sample 4 from moving up and down, and at the same time, it is used to load the weight plate 3. It can cooperate with the first cylinder 1 to complete the processing of plane samples with different angles.

As shown in FIG. 2 , the number of the first studs 2 is 4, and they are arranged symmetrically in pairs in a cross shape; the number of the second studs 7 is 4, and they are arranged symmetrically in a square.

Secondly, the method of using the fixture for vibration polishing of electron backscattered diffraction samples is as follows:

1. Preparation of common samples

As shown in Figure 1, the sample 4 in the figure is a common sample, and the operation steps of the fixture are as follows:

(a), place the sample 4 horizontally, place the analysis surface to be processed and polished downward, place the fixture vertically above the sample 4, adjust the first stud 2 and the second stud 7, so that the first stud 2 2 and the space formed by the second stud 7 is sufficient to accommodate the sample 4;

(b), adjust the first stud 2 through the through hole 8, so that the first stud 2 fixes the sample 4 from the side;

(c), adjust the second stud 7 through the through hole 8, so that the second stud 7 fixes the sample 4 from above;

(d), sample 4 is polished and polished;

(e), adjust the overall total amount of the sample 4 and the fixture through the counterweight plate 3, so that it meets the requirements of vibration polishing;

(f), sample 4 is subjected to vibration polishing treatment, so that it reaches the surface state of the sample that meets the requirements of electron backscatter diffraction analysis;

(g) Prepare the required sample.

2. Preparation of irregular small samples

As shown in Figure 3, sample 4 in the figure is an irregular small sample, and the operation steps of the fixture are as follows:

(1) Place the sample 4 horizontally, place the analysis surface to be processed and polished downward, place the fixture vertically above the sample 4, adjust the first stud 2 and the second stud 7, so that the first stud 2 2 and the space formed by the second stud 7 is sufficient to accommodate the sample 4;

(2), adjust the first stud 2 through the through hole 8, so that the first stud 2 fixes the sample 4 from the side;

(3), adjust the second stud 7 through the through hole 8, so that the second stud 7 fixes the sample 4 from above. The upper surface of , as shown in Figure 3;

(4), the sample 4 in the step (3) is polished and polished, so that the lower surface of the sample 4 is flush with the lower surface of the second cylinder 6, as shown in Figure 4;

(5) Take out the treated sample 4 in step (4), invert the sample 4 and fix the sample 4 according to step (2) and step (3), as shown in FIG. 5 .

(6), the sample 4 in the step (5) is polished and polished, so that the upper surface of the lower surface of the sample 4 is even, as shown in Figure 6;

(7), adjust the overall total amount of the sample 4 and the fixture through the counterweight plate 3, so that it meets the requirements of vibration polishing;

(8), the sample 4 described in the step (6) is carried out vibration polishing treatment, makes it reach the sample surface state that meets the electronic backscatter diffraction analysis requirement;

(9) Prepare the required samples.

3. Preparation of Specimen with Special Orientation

(A), determine the angle of the sample surface and special crystal orientation prepared in the step (g) by X-ray diffractometer;

(B), adjust the second stud described in step (c), so that the sample made in step (g) forms the angle determined in step (A), as shown in Figure 7;

(C), repeat steps (4) to (8) in the preparation steps of the irregular small sample, so as to obtain the required sample.

The following table is a comparison between samples processed by using a jig for vibration polishing of electron backscattered diffraction samples provided by the present invention and samples processed by the prior art.

preparation time   Sample Surface Quality Backscattered Diffraction Pattern this invention 30 minutes good clear comparative example 1-2 working days Poor more vague

Adopting a jig for vibration polishing of electron backscatter diffraction samples provided by the present invention can effectively solve the problem of difficult sample preparation and poor vibration polishing effect caused by the small size of backscatter diffraction samples and the problem of insufficient weight problems as well as the preparation of orientation-specific specimens.

Claims (10)

1. one kind is used for the fixture that the EBSD sample shakes polishing, and described fixture is used for clamping sample (4), it is characterized in that:

Described sample (4) is arranged at bottom the second cylinder (6),

Described the second cylinder (6) top is disposed with the first cylinder (1) and weight stack (3),

Be provided with the first double-screw bolt (2) in described sample (4) horizontal direction, described the first double-screw bolt (2) stretches into the second cylinder (6) inboard from the through hole (8) of the second cylinder (6) sidewall,

Be provided with the second double-screw bolt (7) in described sample (4) upper end vertical direction, described the second double-screw bolt (7) stretches into the second cylinder (6) inside from the through hole (8) of the second cylinder (6), the first cylinder (1) and weight stack (3).

2. a kind of fixture for EBSD sample vibrations polishing according to claim 1, it is characterized in that: the quantity of described the first double-screw bolt (2) is 4, the quantity of described the second double-screw bolt (7) is 4, described 4 the first double-screw bolts (2) are the cross setting, described 4 the second double-screw bolts (7) setting that is square.

3. a kind of fixture for EBSD sample vibrations polishing according to claim 1, it is characterized in that: described the second double-screw bolt (7) is provided with nut (5) at weight stack (3) one ends, and described through hole (8) is tapped through hole.

4. a kind of fixture for EBSD sample vibrations polishing according to claim 1, it is characterized in that: the diameter of described the first cylinder (1) is 25～35mm, the diameter of described the second cylinder (6) is 15～25mm.

5. according to claim 1 or 4 described a kind of fixtures for EBSD sample vibrations polishing, it is characterized in that: described the second cylinder (6) is hollow cylinder, and bottom opening.

6. a kind of fixture for EBSD sample vibrations polishing according to claim 1, it is characterized in that: described the first double-screw bolt (2), the second double-screw bolt (7), the first cylinder (1) and the second cylinder (6) select one or more low density metals to make, and described low density metals comprises aluminium, titanium, magnesium.

7. a kind of fixture for EBSD sample vibrations polishing according to claim 1, it is characterized in that: described weight stack (3) is processed by several metal mixed, and described metal comprises aluminium, iron and molybdenum.

8. the using method of the fixture for EBSD sample vibrations polishing as claimed in claim 1, with sample (4) horizontal positioned, the placed face down with needs processing is characterized in that, also comprises the steps:

(a), clip vertical is positioned over the top of sample (4);

(b), adjust the first double-screw bolt (2), make the first double-screw bolt (2) from the side that sample (4) is fixing;

(c), adjust the second double-screw bolt (7), make the second double-screw bolt (7) from the top, that sample (4) is fixing;

(d), sample (4) is polished and polishing;

(e), adjust the whole total amount of sample (4) and fixture by weight stack (3);

(f), sample (4) is shaken polishing;

(g), make required sample.

9. a kind of using method that shakes the fixture of polishing for the EBSD sample according to claim 8, is characterized in that, when sample (4) is irregular small sample, also comprises the steps:

(1), adjust the second double-screw bolt (7) described in described step (c), the second double-screw bolt (7) and sample (4) upper surface are fitted;

(2), adjust the first double-screw bolt (2) according to described step (b), make the first double-screw bolt (2) from the side that sample (4) is fixing;

(3), according to described step (d), sample (4) is polished and polishing, make sample (4) lower surface concordant with the first cylinder (1) lower surface;

(4), after treatment sample (4) in step (three) is taken out, be inverted sample (4) and according to the fixing sample (4) of step () and step (two);

(5), according to described step (d), the sample (4) in step (four) is polished and polishing, make sample (4) lower surface concordant with upper surface;

(6), according to described step (e) and step (f), the sample (4) that obtains after processing through step (five) is processed processing;

(7), make required sample.

10. according to claim 8 or 9 described a kind of usings method that shake the fixture of polishing for the EBSD sample, is characterized in that, when sample (4) is the particular orientation sample, also comprises the steps:

(A), determine the angle of the specimen surface that makes in described step (g) and crystal orientation by X-ray diffractometer;

(B), the second double-screw bolt (7) described in set-up procedure (c), make that in step (g), prepared sample forms determined angle in step (A);

(C), repeating step (three) is to step (six), makes required sample.

Images