CN104807840A - Sample fixing device for superconducting strip XRD texture measurement - Google Patents

Abstract

The invention discloses a sample fixing device for superconducting strip XRD texture measurement. The sample fixing device comprises a vacuum chuck, a vacuum pump, and a vacuum pipeline enabling the vacuum chuck and the vacuum pump to be communicated with each other, wherein the vacuum chuck includes a vacuum chamber of which the upper surface is used as a sample mounting surface, a plurality of capillary pores with openings formed in the upper surface of the vacuum chamber, and a vacuumizing connecting opening formed in the side wall of the vacuum chamber and used for communicating the vacuum pipeline with the vacuum chamber; the capillary pores are communicated with the interior of the vacuum chamber; the vacuum chamber is fixed on an XRD sample platform through a fixing device. The sample fixing device provided by the invention has the advantages as follows: as a separate component, the sample fixing device can be directly used on the existing XRD texture measuring instrument, so that the functions of the existing XRD texture measuring instrument are extended, and the XRD texture measuring instrument can measure thin superconducting strip samples which are liable to deformation; the accuracy and repeatability of the superconducting strip XRD texture measurement are improved, the working difficulty is greatly reduced, the measurement efficiency is improved, and the test sample can be recycled in a non-destructive manner.

Description

Sample fixture for XRD texture measurement of superconducting tape

technical field

The invention relates to the technical field of testing equipment, in particular to a sample fixing device for XRD texture measurement of superconducting strips.

Background technique

High-temperature superconducting materials have broad application prospects in fields such as electric power, new energy, medical equipment, and national defense equipment. Many companies at home and abroad are committed to the industrial development and application display of high-temperature superconducting strips, and high-temperature superconducting strips are forming a new industry. The main performance of the high-temperature superconducting tape - the current-carrying capacity depends on the orderliness of the grain arrangement of the superconducting film, that is, the crystal texture characteristics, so how to accurately detect the crystal properties of each film layer of the superconducting tape A key issue of materials. However, since the second-generation high-temperature superconducting strip uses a thin metal strip with a thickness between 30 and 100 μm, the slight stress in the strip can easily deform the strip, so the strip usually bends in the middle. As shown in Figure 1, the XRD texture measurement has high requirements on the flatness of the sample, which leads to incorrect or impossible measurement results.

In the XRD texture measurement of the above-mentioned second-generation high-temperature superconducting tape samples, the usual method is to glue the superconducting tape and the XRD sample stage together with double-sided adhesive. Double-sided tape, paste it on the XRD sample stage, and then paste the sample on the double-sided tape, no matter sticking the double-sided tape on the XRD sample stage or pasting the sample on the double-sided tape requires a high Skill, it needs to be operated very carefully to ensure that the double-sided adhesive tape is flat on the sample stage, without wrinkles and air bubbles. The usual practice is to put one end of the double-sided tape in contact with the XRD sample stage, apply an appropriate pressure on this end, and then move the pressure gradually and evenly, so that the double-sided tape is evenly stressed and gradually contacts the XRD sample stage in one direction. , making sure that no air bubbles are trapped under the double-sided tape. The same is true for sticking samples on double-sided tape. The disadvantage of this method is that the repeatability cannot be guaranteed, so the same sample, different people, and measurements at different times sometimes have different results. If the sample is not bonded successfully (bubbles, center line misalignment, etc.), the sample cannot be rebonded because tearing the sample off the double-sided tape essentially destroys the sample. Moreover, pressing the surface of the superconducting strip will cause some damage to the surface of the superconducting strip, which will affect the test results. After the test, the superconducting strip cannot be recycled for further other tests or to deposit other films.

We also try other methods to improve. Method 1: We stick the ends of the superconducting tape with adhesive tape to fix it on the sample stage. This method is easy to operate and does not touch the surface of the sample (unless the two ends of the measurement ) But in practice, it is found that the disadvantage is that there will still be some bulges in the middle of the superconducting strip, resulting in a decrease in the accuracy of the test data. Method 2, use adhesive tape along both sides of the superconducting tape for 2 to 4 mm, and stick the superconducting tape on the sample stage. Compared with method 1, the protrusion of the superconducting tape has been improved a lot, but there are still protrusions , while reducing the measurable area, which introduces errors in the Phi scan. At the same time, the measurement efficiency of these methods is low, and the time of sticking the sample occupies a considerable part of the total measurement time. In addition, the angle of sample placement is generally required to coincide with the zero degree of the XRD texture measuring instrument or have an accurate angle, and the center of the sample is also required to coincide with the instrument center of the XRD texture measuring instrument. method is difficult to achieve precise alignment.

Contents of the invention

The purpose of the present invention is to provide a sample fixing device for XRD texture measurement of superconducting tape, which uses vacuum adsorption method to fix the superconducting tape sample on the existing XRD texture measuring instrument, and expands the existing XRD texture The function of the structure measuring instrument enables it to measure very thin and easily deformed superconducting strip samples, and at the same time can improve the accuracy and repeatability of the XRD texture measurement of superconducting strips, improve the measurement efficiency simply and quickly, and test the samples Can be recycled without damage.

The technical solution of the present invention is: a sample fixing device for XRD texture measurement of superconducting strips, including a vacuum chuck, a vacuum pump, and a vacuum pipeline connecting the vacuum chuck and the vacuum pump, and the vacuum chuck includes an upper The surface of the vacuum chamber is used as the sample mounting surface, several openings are arranged on the upper surface of the vacuum chamber and communicate with the inside of the vacuum chamber, and are arranged on the side wall of the vacuum chamber and are used to communicate with the vacuum chamber. The vacuum line and the vacuum interface of the vacuum cavity, the vacuum cavity is fixed on the XRD sample stage by a fixing device.

As a preferred technical solution, the openings of the capillary pores on the upper surface of the vacuum cavity are arranged in a hexagonal close-packed structure.

As a preferred technical solution, both the diameter of the capillary pores and the spacing between adjacent capillary pores are less than 1mm.

As a more preferred technical solution, both the diameter of the capillary pores and the spacing between adjacent capillary pores are less than 0.5 mm.

As a preferred technical solution, in order to adapt to superconducting tape samples with different strengths and different stresses, the sample fixing device also includes a suction regulator, and the suction regulator includes a needle valve arranged on the vacuum pipeline, and can also be It is selected from the flow resistance focusing valve or the deflation valve, and the suction is adjusted according to different superconducting tape samples, so that the superconducting tape is smoothly adsorbed on the sample installation surface, and at the same time, the superconducting tape will not be caused by local uneven suction. The material deforms at the capillary.

As a preferred technical solution, the vacuum pump is placed outside the XRD texture measuring instrument and communicated with the vacuum chamber through the vacuum pipeline, because the vacuum pump usually has a strong vibration, and the XRD texture measuring instrument is a It is a precision instrument, so it must be placed away from the XRD texture measuring instrument and must be silenced to eliminate the impact of the vacuum pump vibration on the XRD texture measuring instrument; at the same time, the vacuum pump is connected to the vacuum chamber fixed on the XRD sample stage through the vacuum pipeline body, the requirement for the vacuum pipeline is that it should be soft enough that no vibration can be felt by hand at the end of the XRD texture measuring instrument, and there will be no vibration when doing 0-360-degree Phi scans and 0-90-degree Kai scans on the XRD sample stage. It has an influence on the XRD texture measuring instrument.

As a preferred technical solution, the vacuum pump is an oil-free micro-diaphragm vacuum pump.

As a preferred technical solution, the vacuum pipeline is a rubber tube or a soft plastic tube, which is highly flexible and can withstand vacuum pressure without deformation. The rubber tube is soft, but it can withstand pressure differences. Hard, so soft plastic tubes are more suitable for use here; at the same time, the thickness requirements for the vacuum chamber are as follows. Since the adjustment range of the sample height on the XRD texture measuring instrument is limited, a vacuum chamber that is too thick is not suitable for different XRD textures. The adaptability of the measuring instrument is poor, and the thickness is usually controlled within 10mm, preferably within 6mm, and the diameter of the vacuum pipeline is also affected by the vacuum chamber, and its diameter ranges from 3 to 6mm.

As a preferred technical solution, the vacuum pump is connected with a foot-operated vacuum switch, which is convenient for the user to turn on the vacuum pump immediately after aligning the superconducting strip sample to absorb the superconducting strip sample, reducing the time from aligning the sample to going Possible sample movement during switching on the vacuum pump.

As a preferred technical solution, coordinate lines are provided on the sample mounting surface to help the superconducting tape sample be installed on the measurement position accurately and repeatedly, so as to ensure the installation angle of the sample, and the center of the coordinate line is consistent with the XRD The zero position of the texture measuring instrument coincides with the center of the XRD texture measuring instrument.

The advantages of the present invention are:

1. The invention is used for the sample fixing device of XRD texture measurement of superconducting tape, expands the function of existing XRD texture measuring instrument so that it can measure very thin and easily deformed superconducting tape samples, and can improve the accuracy of superconducting tape The accuracy and repeatability of XRD texture measurement greatly reduces the difficulty of the work, improves the measurement efficiency, and the test samples can be recovered without damage;

2. The sample fixing device used for XRD texture measurement of superconducting strips of the present invention can be directly used on existing XRD texture measurement instruments as a separate component, and is easy to install, low in cost and easy to maintain, thereby improving its use value, And it does not affect the operation of the existing XRD texture measuring instrument and the rotation of each measuring arm;

3. The sample fixing device for measuring the XRD texture of superconducting strips in the present invention utilizes the size of capillary pores, the distance between adjacent capillary pores and the arrangement to make superconducting strip samples be reliably and smoothly adsorbed on the vacuum cavity surface (that is, the sample mounting surface), and at the same time, the superconducting tape will not be deformed at the capillary due to local uneven suction.

Description of drawings

The present invention will be further described below in conjunction with accompanying drawing and embodiment:

Figure 1 is a schematic diagram of the XRD texture measurement state of the existing superconducting tape;

Fig. 2 is the structural schematic diagram of the sample fixing device used for the XRD texture measurement of superconducting tape according to the present invention;

Among them: 1 vacuum pump, 2 vacuum pipeline, 3 vacuum suction cup, 3-1 vacuum cavity, 3-2 capillary hole, 3-3 vacuum interface, 4 fixture, 5XRD sample stage, 6 suction regulator, 7 pedal vacuum switch, 8 superconducting strips.

Detailed ways

Embodiment: With reference to Fig. 1, shown in Fig. 2, a kind of sample fixing device for XRD texture measurement of superconducting tape comprises vacuum chuck 3, vacuum pump 1 (this vacuum pump 1 is oil-free miniature diaphragm vacuum pump), and connects vacuum The suction cup 3 and the vacuum pipeline 2 of the vacuum pump 1. The vacuum suction cup 3 includes a vacuum chamber 3-1 whose upper surface is used as a sample mounting surface. Connected capillary holes 3-2, and a vacuum interface 3-3 arranged on the side wall of the vacuum chamber 3-1 and used to communicate with the vacuum pipeline 2 and the vacuum chamber 3-1, the vacuum chamber 3-1 passes through the fixing device 4 is fixed on the XRD sample stage 5, and the vacuum pump 1 is also connected with a foot-operated vacuum switch 7, which is convenient for the user to turn on the vacuum pump 1 immediately after aligning the sample of the superconducting strip 8 to absorb the sample of the superconducting strip 8, reducing Possible sample movement during the period from aligning the sample to turning on the switch of the vacuum pump 1. At the same time, there are coordinate lines on the sample mounting surface to help the superconducting strip 8 sample to be installed on the measurement position accurately and repeatedly to ensure that the sample The center of the coordinate line coincides with the zero position of the XRD texture measuring instrument and the center of the XRD texture measuring instrument.

The openings of the capillary holes 3-2 on the upper surface of the vacuum cavity 3-1 of the present invention are arranged in a hexagonal close-packed structure, and at the same time, the diameter of the capillary holes 3-2 and the spacing between the adjacent capillary holes 3-2 are less than 0.5mm. The superconducting tape 8 sample is reliably and smoothly adsorbed on the upper surface of the vacuum chamber 3-1 (i.e., the sample mounting surface) by using the size of the capillary 3-2 pore size, the distance between adjacent capillary holes 3-2 and the arrangement. , and at the same time, the superconducting strip 8 will not be deformed at the capillary 3-2 due to local uneven suction.

In order to adapt to samples of superconducting strips 8 with different strengths and different stresses, the sample fixing device also includes a suction regulator 6. The suction regulator 6 includes a needle valve arranged on the vacuum pipeline 2, and can also be selected from the Focusing valve or deflation valve, and adjust the suction according to different samples of superconducting strip 8, so that the superconducting strip 8 can be smoothly adsorbed on the sample installation surface, and at the same time, the superconducting strip will not be caused by local uneven suction. 8 is deformed at capillary 3-2.

The vacuum pump 1 of the present invention is placed outside the XRD texture measuring instrument, and communicates with the vacuum cavity 3-1 through the vacuum pipeline 2. Since the vacuum pump 1 usually has a strong vibration, and the XRD texture measuring instrument is a precision instrument, Therefore, it must be placed away from the XRD texture measuring instrument and must be silenced to eliminate the impact of the vibration of the vacuum pump 1 on the XRD texture measuring instrument; at the same time, the vacuum pump 1 is connected to the vacuum chamber fixed on the XRD sample stage through the vacuum pipeline 2 Body 3-1, the requirement for the vacuum line 2 is that it should be soft enough that no vibration can be felt by hand at the end of the XRD texture measuring instrument, and a 0-360-degree Phi scan and a 0-90-degree Kai should be performed on the XRD sample stage Scanning will not affect the XRD texture measuring instrument.

The vacuum pipeline 2 of the present invention is a soft plastic tube, which is highly flexible and can withstand vacuum pressure without deformation. The rubber tube is soft, but it is resistant to pressure difference, and the hard plastic tube is good in pressure resistance, but relatively hard, so the soft plastic tube is It is more appropriate to use here; at the same time, the thickness requirements of the vacuum chamber 3-1 are as follows. Since the adjustment range of the sample height on the XRD texture measuring instrument is limited, a vacuum chamber 3-1 that is too thick can measure different XRD textures. The adaptability of the instrument is poor, and the thickness is usually controlled within 10 mm, preferably within 6 mm. The diameter of the vacuum pipeline 2 is also affected by the vacuum chamber 3-1, and its diameter ranges from 3 to 6 mm.

In the present invention, the superconducting tape 8 is adsorbed and fixed on the upper surface of the vacuum cavity 3-1 to cover all capillary pores 3-2. If a special small superconducting tape sample is measured, all capillary pores 3-2 cannot be covered. , You can also use adhesive tape or other methods to seal the excess pores.

The above explanations are used to illustrate the present invention and not limit the scope of the present invention. It is only to illustrate the technical concept and characteristics of the present invention. Its purpose is to allow those familiar with this technology to understand the content of the present invention and implement it accordingly. The protection scope of the present invention cannot be limited by this. All equivalent changes or modifications made according to the spirit of the present invention shall fall within the protection scope of the present invention. For example, no matter the vacuum chuck 3 is square, round, trapezoidal or stepped, no matter how many pieces the vacuum cavity 3-1 of the vacuum chuck 3 is sealed, no matter whether the seal is formed by O-ring, welding or tight fit , regardless of whether the vacuum interface 3-3 is on the side or the back of the vacuum cavity 3-1, whether the capillary 3-2 is round or square, whether the XRD texture measuring instrument is Bruker diffractometer, Ricoh diffractometer, or Panalitic diffraction instrument, all belong to the scope of the present invention. Finally the main purpose of the invention is the measurement of superconducting strips 8 , but the measurement of deformed thin strips in other fields of application should also be considered within the scope of the invention.

Claims (10)

1. A sample fixing device for XRD texture measurement of superconducting strips, comprising a vacuum chuck (3), a vacuum pump (1), and a vacuum pipeline connecting the vacuum chuck (3) and the vacuum pump (1) (2), characterized in that the vacuum chuck (3) includes a vacuum cavity (3-1) whose upper surface is used as a sample mounting surface, and several openings are provided on the upper surface of the vacuum cavity (3-1) and Capillary holes (3-2) communicating with the inside of the vacuum chamber (3-1), and provided on the side wall of the vacuum chamber (3-1) and used to communicate with the vacuum pipeline (2) and the The vacuum interface (3-3) of the vacuum cavity (3-1), the vacuum cavity (3-1) is fixed on the XRD sample stage (5) through the fixing device (4). 2. The sample fixing device for XRD texture measurement of superconducting tape according to claim 1, characterized in that the capillary hole (3-2) is on the upper surface of the vacuum cavity (3-1) The openings are arranged in a hexagonal close-packed structure. 3. The sample fixing device for XRD texture measurement of superconducting tape according to claim 1 or 2, characterized in that the diameter of the capillary hole (3-2) and the adjacent capillary hole (3-2 ) hole spacing is less than 1mm. 4. The sample fixing device for XRD texture measurement of superconducting tape according to claim 3, characterized in that the diameter of the capillary hole (3-2) and the diameter of the adjacent capillary hole (3-2) Hole spacing is less than 0.5mm. 5. The sample fixing device for XRD texture measurement of superconducting strips according to claim 1, characterized in that the sample fixing device further comprises a suction regulator (6), and the suction regulator (6) includes A needle valve arranged on the vacuum pipeline (2). 6. The sample fixing device for XRD texture measurement of superconducting strips according to claim 1, characterized in that the vacuum pump (1) is placed outside the XRD texture measurement instrument and passes through the vacuum pipeline ( 2) communicate with the vacuum cavity (3-1). 7. The sample fixing device for XRD texture measurement of superconducting strips according to claim 6, characterized in that the vacuum pump (1) is an oil-free micro-diaphragm vacuum pump. 8. The sample fixing device for XRD texture measurement of superconducting strips according to claim 6, characterized in that, the vacuum pipeline (2) is a rubber tube or a soft plastic tube, and its diameter ranges from 3 to 6 mm . 9. The sample fixing device for XRD texture measurement of superconducting strips according to claim 1, characterized in that the vacuum pump (1) is connected with a foot-operated vacuum switch (7). 10. The sample fixture for superconducting tape XRD texture measurement according to claim 1, characterized in that, the sample mounting surface is provided with a coordinate line, the center of the coordinate line and the XRD texture measuring instrument The zero-degree position and the center of the XRD texture measuring instrument coincide.