Sample holder for x-ray powder diffraction, diffraction testing system and method

Abstract

This disclosure provides a sample holder, diffraction testing system, and method for X-ray powder diffraction. The sample holder includes: a clamping part capable of clamping onto an XYZ triaxial base and being positionally adjusted along the XYZ axes by the base; the clamping part includes a hollow cylindrical portion and a hollow frustum portion located above the hollow cylindrical portion, the hollow cylindrical portion and the hollow frustum portion being coaxial and having the same inner diameter; a loading part including a first cylindrical portion and an annular portion located above the first cylindrical portion, the annular portion having holes for filling the sample, and the first cylindrical portion being insertable into the hollow frustum portion from above; and a pressing needle part including a second cylindrical portion for holding and a third cylindrical portion for filling and compacting the sample into the loading part. The X-ray powder diffraction sample holder of this disclosure can effectively fix experimental samples for X-ray powder diffraction.

Description

Technical Field

[0001] This disclosure relates to the field of materials testing equipment, and more particularly to a sample holder, X-ray powder diffraction testing system, and method for X-ray powder diffraction. Background Technology

[0002] X-ray powder diffraction is one of the most commonly used experimental techniques in scientific research in physics, chemistry, materials science, and related disciplines. It is used to analyze the phase composition, content, and particle size of prepared materials. In the early stages of research, when the sample quantity is small, a trace amount of powder sample can be placed in a glass capillary tube for testing, or it can be mixed with a suitable amount of glue and attached to the tip of a glass wire. However, the diffraction peaks of the trace powder sample are originally quite weak, and the glass capillary tube or glue will produce a significant background, thus masking the sample signal and affecting the accuracy of the analysis results. In addition, when using the latter method, the trace powder sample mixed with glue is difficult to recover.

[0003] How to fix the trace powder sample during X-ray powder diffraction in order to obtain high-quality diffraction data using appropriate methods is a technical problem that urgently needs to be solved. Summary of the Invention

[0004] In view of this, the present disclosure provides a sample fixture, an X-ray powder diffraction testing system, and a method for X-ray powder diffraction, in order to solve the technical problem that powder samples are difficult to fix during X-ray powder diffraction testing in the prior art.

[0005] To achieve the above objectives, the technical solution adopted in this disclosure is as follows: A first aspect of this disclosure provides a sample holder for X-ray powder diffraction, comprising: a clamping member capable of being clamped on an XYZ triaxial base and adjusted in position along the three XYZ axes under the drive of the base; the clamping member includes a hollow cylindrical portion and a hollow frustum portion located above the hollow cylindrical portion, the hollow cylindrical portion and the hollow frustum portion being coaxial and having the same inner diameter; and a loading member comprising a first cylindrical portion and an annular portion located above the first cylindrical portion, the holes of the annular portion being used to fill the sample, and the first cylindrical portion being capable of being inserted into the hollow frustum portion from above.

[0006] In some embodiments, the outer diameter of the lower end of the hollow frustum portion is the same as the outer diameter of the hollow cylinder portion.

[0007] In some embodiments, the sample fixture further includes a pressure needle, which includes a second cylindrical portion and a third cylindrical portion located above the second cylindrical portion and having an outer diameter smaller than that of the second cylindrical portion. The outer diameter of the third cylindrical portion is smaller than the inner diameter of the annular portion, and the difference between the outer diameter of the third cylindrical portion and the inner diameter of the corresponding annular portion is 0.15 mm to 0.25 mm.

[0008] In some embodiments, the thickness of the annular portion is 1.8 mm to 2.2 mm.

[0009] In some embodiments, the difference between the outer diameter of the first cylindrical portion and the inner diameter of the hollow frustum portion is 0.15 mm to 0.25 mm.

[0010] In some embodiments, the height of the first cylindrical portion is less than the height of the clamping member, and the height of the clamping member is equal to the sum of the height of the hollow frustum portion and the height of the hollow cylindrical portion.

[0011] In some embodiments, there are multiple loading components, one of which is selectively inserted into the clamping component during use; the inner diameter of the annular portion of the multiple loading components includes 1 mm, 2 mm or 3 mm.

[0012] In some embodiments, the diameter of the first cylindrical portion is smaller than the thickness of the annular portion.

[0013] A second aspect of this disclosure provides an X-ray powder diffraction testing system, including an X-ray generator, a diffraction light detector, a test controller, and a sample holder for X-ray powder diffraction as described in the first aspect of this disclosure; wherein, X-rays generated by the X-ray generator pass through a sample in the sample holder and form a diffraction pattern on the diffraction light detector, and the test controller receives and processes the diffraction pattern data sent by the diffraction light detector.

[0014] A third aspect of this disclosure provides an X-ray powder diffraction testing method applied to the X-ray powder diffraction testing system of the second aspect of this disclosure. The method includes: after X-rays generated by an X-ray generator pass through a sample in a sample holder and form a diffraction pattern on a diffraction light detector, acquiring diffraction pattern data sent by the diffraction light detector; and acquiring diffraction intensity, diffraction angle, and the position and shape of diffraction peaks based on the diffraction pattern data.

[0015] The beneficial effects of this embodiment compared with the prior art are as follows: the technical solution in this embodiment is designed to include a clamping component that can be installed on an XYZ triaxial base, and a loading component that can be inserted into the clamping component. The loading component is designed with an annular portion that can be filled with a trace amount of powder sample. By adjusting the XYZ triaxial base, the position of the trace amount of powder sample can be adjusted, thereby aligning the powder sample with the X-rays. This allows for better fixation of the trace amount of powder sample during X-ray powder diffraction. Attached Figure Description

[0016] To more clearly illustrate the technical solutions in the embodiments of this disclosure, the accompanying drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the accompanying drawings described below are only some embodiments of this disclosure. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0017] Figure 1 This is a schematic diagram of the exploded structure of a sample holder for X-ray powder diffraction provided in an embodiment of this disclosure; Figure 2 This is a schematic diagram of the X-ray powder diffraction sample holder after installation, provided in an embodiment of this disclosure. Figure 3 This is a schematic diagram of the structure of a pressure needle provided in an embodiment of this disclosure; Figure 4 This is a schematic diagram of an X-ray powder diffraction testing system and method provided in an embodiment of this disclosure; Figure 5 This is a comparison chart showing the conversion between powder diffraction data and conventional powder diffraction patterns. Detailed Implementation

[0018] To make the technical problems, technical solutions, and beneficial effects to be solved by this disclosure clearer, the disclosure will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only for explaining this disclosure and are not intended to limit this disclosure.

[0019] The sample holder, X-ray powder diffraction testing system, and method according to embodiments of the present disclosure will now be described in detail with reference to the accompanying drawings.

[0020] Figure 1 This is a schematic diagram of the exploded structure of a sample holder for X-ray powder diffraction provided in an embodiment of this disclosure; Figure 2 This is a schematic diagram of the X-ray powder diffraction sample holder after installation, provided in an embodiment of this disclosure. Figure 3 This is a schematic diagram of the structure of a pressure needle provided in an embodiment of this disclosure; Figure 4This is a schematic diagram of an X-ray powder diffraction testing system and method provided in an embodiment of this disclosure. Figure 5 This is a comparison chart showing the conversion between powder diffraction data and conventional powder diffraction patterns. Below is a combination of... Figures 1 to 5 The present disclosure describes the sample fixture and X-ray powder diffraction testing system and method provided in the embodiments of this disclosure.

[0021] like Figure 1 , Figure 2 and Figure 3 As shown, the X-ray powder diffraction sample holder of this disclosure includes: a clamping member capable of being clamped on an XYZ triaxial base of a device adapted to the sample holder, and whose position can be adjusted along the three directions of the XYZ axis under the drive of the base; the clamping member includes a hollow cylindrical part 111 and a hollow frustum part 112 located above the hollow cylindrical part; the hollow cylindrical part 111 and the hollow frustum part 112 are coaxial and have the same inner diameter; a loading member including a first cylindrical part 121 and an annular part 122 located above the first cylindrical part; the hole of the annular part is used to fill the sample; the first cylindrical part can be inserted into the hollow frustum part from above; and a pressing needle member including a second cylindrical part 311 for holding and a third cylindrical part 312 for filling and compacting the sample into the loading member.

[0022] X-ray single-crystal diffraction experiments require very small samples, typically a single crystal of 0.1 cubic millimeters. The technical solution of this disclosure allows for the accurate measurement of diffraction data from trace samples using X-ray single-crystal diffraction methods. Furthermore, the powder sample can be recovered for other tests. Using the technical solution of this disclosure, the volume of the sample required for measurement can be reduced to 3% to 5% of the original sample volume, for example, to tens or hundreds of cubic millimeters, while maintaining the accuracy of the data at the level of conventional measurements. This allows for powder diffraction experiments to be performed on an X-ray single-crystal diffractometer, precisely measuring the diffraction data of trace powder samples.

[0023] During testing, the sample fixture must first be placed on the XYZ triaxial base to ensure that the sample position can be adjusted in the XYZ directions. This base can be fixed to the goniometer of the X-ray single-crystal diffractometer using nuts.

[0024] By employing the technical solution of this disclosure embodiment, the design of the loading component allows for convenient addition and removal of the sample from the hole in the annular portion by holding the first cylindrical part. By designing the clamping component, the final height of the powder sample can be adjusted by changing the depth of the first cylindrical part inserted into the hollow frustum portion, thereby adapting the height of the powder sample to the X-ray propagation path and forming a more distinct diffraction pattern.

[0025] To facilitate clamping, the outer diameter of the hollow cylindrical portion can be designed to be 3mm. Correspondingly, the upper base diameter of the hollow frustum portion can be designed to be 2mm, and the lower base diameter to be 3mm. In the technical solution of this embodiment, the lower outer diameter of the hollow frustum portion can be designed to be the same as the outer diameter of the hollow cylindrical portion, thereby making the junction between the hollow frustum portion and the hollow cylindrical portion smoother, which is beneficial to aesthetics and ease of use. Alternatively, the outer diameter of the hollow cylindrical portion can be designed to be any value from 2.5mm to 3.5mm. Correspondingly, the lower base diameter of the hollow frustum portion can be designed to be any value from 2.5mm to 3.5mm, and the upper base diameter of the hollow frustum portion can be designed to be any value from 1.5mm to 2.5mm.

[0026] like Figure 2 As shown, the first cylindrical portion can be inserted into the hollow frustum portion. In this embodiment, the difference between the outer diameter of the first cylindrical portion and the inner diameter of the hollow frustum portion is 0.15 mm to 0.25 mm. Preferably, the difference between the outer diameter of the first cylindrical portion and the inner diameter of the hollow frustum portion is 0.2 mm. A difference between the outer diameter of the first cylindrical portion and the inner diameter of the hollow frustum portion allows for easier insertion of the first cylindrical portion into the hollow frustum portion; a smaller difference between the outer diameter of the first cylindrical portion and the inner diameter of the hollow frustum portion allows for easier and more stable insertion of the first cylindrical portion into the hollow frustum portion.

[0027] Specifically, the outer diameter of the first cylindrical portion can be 0.8 mm, but is not limited to this. Correspondingly, the inner diameter of both the hollow frustum and the hollow cylinder can be designed to be 1 mm; the inner diameter of both the hollow frustum and the hollow cylinder can be designed to be 0.95 mm; the inner diameter of both the hollow frustum and the hollow cylinder can be designed to be 1.05 mm. Furthermore, the inner diameters of both the hollow frustum and the hollow cylinder can be designed to be any value between 0.95 mm and 1.05 mm.

[0028] After easily inserting the first cylindrical part into the hollow frustum, a clay-like substance can be used to bond the first cylindrical part and the hollow frustum to further secure them. After the experiment, remove the clay, clean the loading component and the clamping component, and it is ready for the next test. The hollow frustum on the clamping component is designed to facilitate the bonding of the clay to the loading component and the clamping component.

[0029] Furthermore, with the aid of the gel-like substance's fixing effect, the length of the first cylindrical portion inserted into the hollow frustum can be adjusted. Specifically, the first cylindrical portion can be inserted entirely into the hollow frustum, or only a portion of the first cylindrical portion can be inserted. In practical applications, the depth of the first cylindrical portion inserted into the hollow frustum can be adjusted according to the set height of the powder sample.

[0030] Furthermore, the length of the first cylindrical portion can be greater than the height of the hollow frustum portion, and the end of the first cylindrical portion can be inserted into the hollow cylindrical portion.

[0031] like Figure 3 As shown, the sample holder further includes a pressure needle, which comprises a second cylindrical portion and a third cylindrical portion located above the second cylindrical portion and having an outer diameter smaller than that of the second cylindrical portion. The outer diameter of the third cylindrical portion is smaller than the inner diameter of the annular portion, and the difference between the outer diameter of the third cylindrical portion and the inner diameter of the annular portion is 0.15 mm to 0.25 mm, preferably 0.2 mm. The second cylindrical portion is used for holding, and the third cylindrical portion serves as a pressure needle, which can be used to fill the sample into the hole of the annular portion and to remove the sample from the hole of the annular portion. In embodiments of this disclosure, the pressure needle can be made of stainless steel or copper.

[0032] In this embodiment, the thickness of the annular portion is 1.8 mm to 2.2 mm. Preferably, the thickness of the annular portion is 2 mm. The thickness of the annular portion can be designed to be 2 mm. Setting the thickness of the annular portion to 2 mm allows the powder sample to fill with a thickness of 2 mm. Using a powder sample of this thickness for X-ray powder diffraction testing can yield more accurate test results.

[0033] In this embodiment of the present disclosure, the diameter of the first cylindrical portion is smaller than the thickness of the annular portion, thereby making the loading component smaller in size and easier to hold.

[0034] In this embodiment, the height of the first cylindrical portion is less than the height of the clamping member, and the height of the clamping member is equal to the sum of the height of the hollow frustum portion and the height of the hollow cylindrical portion. The technical solution of this embodiment adjusts the height of the powder sample by adjusting the depth of the first cylindrical portion inserted into the clamping member. To ensure the powder sample has an appropriate height, the height of the clamping member can be designed to be an appropriate value; generally, setting the height of the first cylindrical portion to be less than the height of the clamping member is sufficient, thereby ensuring the relative stability of the clamping member and the loading member during use.

[0035] Specifically, the height of the first cylindrical portion can be 20mm, but is not limited to this. The height of the hollow frustum portion can be 8mm, and the height of the hollow cylindrical portion can be 22mm, but is not limited to this.

[0036] In this embodiment, multiple loading components are provided, and any one can be inserted into the clamping component during use. The annular portions of the multiple loading components have different inner diameters to accommodate powder samples of different volumes. The outer diameter of the annular portion can be 6 mm, but is not limited to this. The inner diameter of the annular portion can be 1 mm, 2 mm, or 3 mm, and is not limited to this. Correspondingly, the outer diameter of the third cylindrical portion of the pressure needle can be 0.8 mm, 1.8 mm, or 2.8 mm.

[0037] According to the X-ray powder diffraction sample holder provided in the embodiments of this disclosure, a clamping member that can be mounted on an XYZ triaxial base and a loading member that can be inserted into the clamping member are designed. The loading member is designed with an annular portion that can be filled with a trace amount of powder sample. By adjusting the XYZ triaxial base, the position of the trace amount of powder sample can be adjusted so that the powder sample is aligned with the X-ray, thereby achieving better fixation of the trace amount of powder sample during X-ray powder diffraction.

[0038] like Figure 4 As shown, this disclosure also provides an X-ray powder diffraction testing system, including: an X-ray generator 411, a diffraction ray detector 413, a test controller 414, and the X-ray powder diffraction sample holder 100 in the above technical solution; wherein, the X-rays generated by the X-ray generator pass through the sample 412 in the sample holder and form a diffraction pattern on the diffraction ray detector, and the test controller receives and processes the diffraction pattern data sent by the diffraction ray detector.

[0039] The X-ray generator, diffraction ray detector, and test controller of this disclosure are part of an X-ray single-crystal diffractometer, thereby enabling precise measurement of X-ray powder diffraction data of trace powder samples on the X-ray single-crystal diffractometer. The diffraction ray detector is a detector of the X-ray single-crystal diffractometer.

[0040] X-ray single-crystal diffraction experiments require very small samples, typically a single crystal of 0.1 cubic millimeters. The technical solution of this disclosure allows for the accurate measurement of diffraction data from trace samples using X-ray single-crystal diffraction experiments. Furthermore, the powder sample can be recovered for other tests. Using the technical solution of this disclosure, the volume of the sample required for measurement can be reduced to 3% to 5% of the original sample volume, for example, to tens or hundreds of cubic millimeters, while maintaining the accuracy of the data at the level of conventional measurements. This allows for powder diffraction experiments to be performed on an X-ray single-crystal diffractometer, precisely measuring the diffraction data of trace powder samples.

[0041] During testing, the sample fixture must first be placed on the XYZ triaxial base to ensure that the sample position can be adjusted in the XYZ directions. This base can be fixed to the goniometer of the X-ray single-crystal diffractometer using nuts.

[0042] In this embodiment, the loading of trace samples can be performed under a low-power microscope if necessary. Adjusting the depth of the base and the first cylindrical portion inserted into the clamping member ensures that the rays pass just through the sample without hitting the surrounding rings, thus preventing the diffraction signal from being obscured by excessive signals caused by the ring material.

[0043] Because X-ray single-crystal diffractometers use two-dimensional detectors, powder diffraction data appears as Debye rings. Appropriate processing is necessary for comparison with conventional powder diffraction patterns. Data processing mainly includes two parts: background subtraction and integration along the Debye rings. The former can be achieved by pre-taking a blank background image and then subtracting it from the data image. The latter can be obtained by integrating Debye rings with equal interplanar spacing along a circumference. Figure 5 The image shown is a comparison of the conversion between powder diffraction data and conventional powder diffraction patterns.

[0044] The loading component of this embodiment can be filled with trace samples that are inorganic or organic, such as nanomaterials, for measurement by an X-ray single-crystal diffractometer.

[0045] This disclosure also provides an X-ray powder diffraction testing method, including: an X-ray powder diffraction testing system applied to the above technical solution, the method including: after X-rays generated by an X-ray generator pass through a sample in a sample holder and form a diffraction pattern on the diffraction light detector, acquiring diffraction pattern data sent by the diffraction light detector; and acquiring diffraction intensity, diffraction angle, and the position and shape of diffraction peaks based on the diffraction pattern data.

[0046] Furthermore, qualitative and quantitative phase analysis can be performed based on the position and intensity of diffraction peaks. By measuring the intensity of characteristic diffraction peaks of different phases and using various mathematical models for calculation, the mass percentage or volume percentage of each crystalline phase in the sample can be obtained.

[0047] Furthermore, detailed analysis of the diffraction peak positions can yield deeper structural information. The shape of the diffraction peaks can assess the degree of crystallinity of the sample. The average grain size in the sample can be estimated by observing the inverse relationship between the broadening of the diffraction peaks and the size of the grains along the diffraction direction. By measuring the shift in the diffraction peak positions, the magnitude and direction of the stress within the material can be calculated.

[0048] Based on the X-ray powder diffraction testing system and method provided in the embodiments of this disclosure, high-quality X-ray powder diffraction data are obtained using the X-ray single crystal diffraction test method.

[0049] According to the X-ray powder diffraction testing system and method provided in the embodiments of this disclosure, the X-ray powder diffraction testing system includes a sample holder for X-ray powder diffraction. The sample holder is designed with a clamping member that can be mounted on an XYZ triaxial base, and a loading member that can be inserted into the clamping member. The loading member is designed with an annular portion that can be filled with a trace amount of powder sample. By adjusting the XYZ triaxial base, the position of the trace amount of powder sample can be adjusted, thereby aligning the powder sample with the X-rays, thus achieving better fixation of the trace amount of powder sample during X-ray powder diffraction.

[0050] The above are merely preferred embodiments of this disclosure and are not intended to limit this disclosure. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of this disclosure should be included within the scope of protection of this disclosure.

Claims

1. A sample holder for X-ray powder diffraction, characterized in that, The sample fixture includes: The clamping component can be clamped on the XYZ three-axis base and adjusted in position along the three directions of the XYZ axis under the drive of the base. The clamping part includes a hollow cylindrical part and a hollow frustum part located above the hollow cylindrical part. The hollow cylindrical part and the hollow frustum part are coaxial and have the same inner diameter. The loading component includes a first cylindrical portion and an annular portion located above the first cylindrical portion. The holes in the annular portion are used to fill the sample. The first cylindrical portion can be inserted into the hollow frustum portion from above. The pressure needle includes a second cylindrical portion for hand-held use and a third cylindrical portion for filling and compacting the sample into the loading component.

2. The sample holder for X-ray powder diffraction according to claim 1, characterized in that, The outer diameter of the lower end of the hollow frustum is the same as the outer diameter of the hollow cylinder.

3. The sample holder for X-ray powder diffraction according to claim 1, characterized in that, The third cylindrical portion is located above the second cylindrical portion and has an outer diameter smaller than that of the second cylindrical portion. The outer diameter of the third cylindrical portion is smaller than the inner diameter of the annular portion, and the difference between the outer diameter of the third cylindrical portion and the corresponding inner diameter of the annular portion is 0.15 mm to 0.25 mm.

4. The sample holder for X-ray powder diffraction according to claim 1, characterized in that, The thickness of the annular portion is 1.8 mm to 2 mm.

5. The sample holder for X-ray powder diffraction according to claim 1, characterized in that, The difference between the outer diameter of the first cylindrical portion and the inner diameter of the hollow frustum portion is 0.15 mm to 0.25 mm.

6. The sample holder for X-ray powder diffraction according to claim 1, characterized in that, The height of the first cylindrical portion is less than the height of the clamping member, and the height of the clamping member is equal to the sum of the height of the hollow frustum portion and the height of the hollow cylindrical portion.

7. The sample holder for X-ray powder diffraction according to claim 1, characterized in that, The loading component is multiple, and one loading component is selected and inserted into the clamping component according to the amount of sample during use; The inner diameter of the annular portion of the plurality of loading components includes 1 mm, 2 mm, or 3 mm.

8. The sample holder for X-ray powder diffraction according to claim 1, characterized in that, The diameter of the first cylindrical portion is smaller than the thickness of the annular portion.

9. An X-ray powder diffraction testing system, characterized in that, The X-ray powder diffraction testing system includes an X-ray generator, a diffraction light detector, a test controller, and a sample holder for X-ray powder diffraction as described in any one of claims 1 to 8. The X-rays generated by the X-ray generator pass through the sample in the sample holder and form a diffraction pattern on the diffraction light detector. The test controller receives and processes the diffraction pattern data sent by the diffraction light detector.

10. An X-ray powder diffraction testing method, characterized in that, The method, applied to the X-ray powder diffraction testing system as described in claim 9, comprises: After the X-rays generated by the X-ray generator pass through the sample in the sample holder and form a diffraction pattern on the diffraction light detector, the diffraction pattern data sent by the diffraction light detector is acquired. The diffraction intensity, diffraction angle, and position and shape of the diffraction peaks are obtained from the diffraction pattern data.

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