CN110887856B - Sample table for X-ray diffractometer, application of sample table and X-ray diffractometer - Google Patents
Sample table for X-ray diffractometer, application of sample table and X-ray diffractometer Download PDFInfo
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- CN110887856B CN110887856B CN201911066181.7A CN201911066181A CN110887856B CN 110887856 B CN110887856 B CN 110887856B CN 201911066181 A CN201911066181 A CN 201911066181A CN 110887856 B CN110887856 B CN 110887856B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
- G01N23/20025—Sample holders or supports therefor
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Abstract
The invention discloses a sample stage for an X-ray diffractometer, application of the sample stage and the X-ray diffractometer, and relates to the field of X-ray diffractometers. The sample table for the X-ray diffractometer comprises a sample table framework and an amorphous structure membrane, wherein the top of the sample table framework is connected with the bottom surface of the amorphous structure membrane to support the amorphous structure membrane, and one side of the sample table framework is used for being inserted into the X-ray diffractometer. The application provides a sample platform for X-ray diffractometer convenient to use, the low price does not influence original experimental mode, and the measurement background is low for only measuring of a small amount of material samples becomes probably and test data is accurate reliable. In addition, the application also provides the application of the sample stage for the X-ray diffractometer in the X-ray diffractometer for testing thin-film materials and samples of materials with small powder quantity. The X-ray diffractometer comprises the sample stage for the X-ray diffractometer.
Description
Technical Field
The invention relates to the field of X-ray diffractometers, in particular to a sample table for an X-ray diffractometer, application of the sample table and the X-ray diffractometer.
Background
The English name of the X-ray diffractometer is X-ray Powder diffractometer which is abbreviated as XPD or XRD. The X-ray diffractometer is used for accurately measuring the crystal structure, texture and stress of a substance by utilizing the diffraction principle, and accurately performing phase analysis, qualitative analysis and quantitative analysis. The method is widely applied to the fields of metallurgy, petroleum, chemical industry, scientific research, aerospace, teaching, material production and the like.
The standard sample stage used by most X-ray diffractometers is made of quartz glass and is in the shape of a cuboid, one side of the cuboid is provided with a rectangular sample groove perpendicular to the cuboid, the depth of the rectangular sample groove is about 0.5mm, and the standard sample stage is generally applicable to general powder XRD tests, but the standard sample stage is not applicable to measurement of materials with small powder quantity or thin film material samples, and a glass substrate generates obvious interference peaks (in the range of 20-40 degrees) and extremely strong backgrounds (shown in figure 5: the uppermost measurement line), so that the measurement data are inaccurate and difficult to quantitatively analyze. Currently, there is a sample stage for an X-ray diffractometer manufactured by using single crystal silicon, which has a very low background and generates few background peaks, but has a very complicated manufacturing process and a high price (about 2000 RMB).
In view of this, the invention is particularly proposed.
Disclosure of Invention
The first purpose of the present invention is to provide a sample stage for an X-ray diffractometer, which has a low measurement background and can realize the measurement of a diffraction pattern of a very small amount of powder sample.
The second purpose of the invention is to provide an application of the sample stage for the X-ray diffractometer in the X-ray diffractometer for testing thin-film materials and materials with small powder quantity.
A third object of the present invention is to provide an X-ray diffractometer having a wider application range.
The invention is realized by the following steps:
the utility model provides a sample platform for X-ray diffractometer, its includes sample platform skeleton and amorphous structure membrane, the top of sample platform skeleton with the bottom surface of amorphous structure membrane is connected in order to support amorphous structure membrane, one side of sample platform skeleton is used for inserting and locates in the X-ray diffractometer.
In an optional embodiment, the sample stage skeleton of the sample stage for the X-ray diffractometer includes an outer frame section and an inner partition section, which are connected to each other, the outer frame section is partitioned by the inner partition section to form a first frame and a second frame, the first frame corresponds to the amorphous structure film and serves as a sample bearing surface, and the second frame is inserted into a fixing clip of the X-ray diffractometer.
In an alternative embodiment, the outer frame section and the inner partition section of the sample stage for an X-ray diffractometer are integrally formed and are formed by bending support rods.
In an alternative embodiment, the outer frame section of the sample stage for an X-ray diffractometer has a first free end, and the inner partition section has a second free end, and the first free end is close to a side of the inner partition section away from the second free end.
In an alternative embodiment, the support rod of the sample stage for an X-ray diffractometer is a metal wire, preferably, the metal wire is any one of an iron wire, a copper wire, a stainless steel wire and a nickel wire; preferably, the wire of the sample stage for an X-ray diffractometer has a diameter of 0.1 to 0.3 mm.
In an alternative embodiment, the amorphous structure film includes any one of a polyimide film, a polyethyleneimine film, a polyoxymethylene film, and a polymethylmethacrylate film.
In an alternative embodiment, the amorphous structure film of the sample stage for an X-ray diffractometer has a thickness of 0.04 to 0.06 mm.
In an optional embodiment, the amorphous structure film of the sample stage for the X-ray diffractometer and the sample stage framework are attached by glue.
Use of the sample stage for an X-ray diffractometer according to any one of the above embodiments in an X-ray diffractometer for testing thin film materials, samples of materials with a small amount of powder.
An X-ray diffractometer comprising the sample stage for an X-ray diffractometer according to any one of the above embodiments.
The invention has the following beneficial effects:
sample platform skeleton is connected to the bottom surface of unformed structure membrane in this application, and sample platform skeleton plays the effect of supporting the unformed structure membrane to the top surface of unformed structure membrane has certain intensity and can bear the sample, and sample platform skeleton can insert and locate in original X-ray diffractometer, with the realization fixed to whole sample platform. Utilize the amorphous structure membrane to carry out the bearing sample in this application, make it as measuring platform, the amorphous structure membrane can see through X ray, it is low to measure the background, the function of amorphous structure membrane can make full use of, and convenient to use, the low price, do not influence original experimental mode, do not produce the extremely wide interference peak like glass promptly in 20-40 degrees diffraction angle within ranges, and measure the very low of background, make the measurement of only a small amount of material samples become for probably and test data is accurate reliable. The device is cheap and can replace the measurement sample table for the X-ray diffractometer of the monocrystalline silicon which is expensive (about 2000 RMB each) on the market at present. Furthermore, the sample stage for the X-ray diffractometer provided by the application does not change the normal use of the original X-ray diffractometer, namely when a material or film material sample with small powder amount needs to be tested, the standard sample stage can be replaced by the sample stage for the X-ray diffractometer provided by the application.
In addition, the application provides the sample stage for the X-ray diffractometer, which is used for testing thin-film materials and materials with small powder amount in the X-ray diffractometer. The measurement of the thin film material and the sample of the material with small powder amount is possible, and the test data is accurate and reliable. The application also provides an X-ray diffractometer, which comprises the sample stage for the X-ray diffractometer, wherein the sample stage for the X-ray diffractometer can be used by directly replacing the standard sample stage of the original X-ray diffractometer under the condition that the use of the X-ray diffractometer is not changed, and further the application range of the X-ray diffractometer is expanded.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
Fig. 1 is a schematic structural diagram of a sample stage framework of a sample stage for an X-ray diffractometer according to an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of a sample stage for an X-ray diffractometer according to an embodiment of the present invention;
FIG. 3 is a side cross-sectional view of a sample stage for an X-ray diffractometer according to an embodiment of the present invention;
FIG. 4 is a diagram of a sample stage for an X-ray diffractometer according to an embodiment of the present invention;
fig. 5 is a schematic diagram comparing the measurement background of a sample stage and a glass sample stage for an X-ray diffractometer according to an embodiment of the present invention.
Icon: a sample stage for a 100-X-ray diffractometer; 110-sample stage skeleton; 111-a support bar; 112-an outer frame section; 113-an internal compartment; 114-a first frame; 115-a second frame; 116-sample bearing surface; 117-first free end; 118-a second free end; 120-amorphous structured film.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings or the orientations or positional relationships that the products of the present invention are conventionally placed in use, and are only used for convenience in describing the present invention and simplifying the description, but do not indicate or imply that the devices or elements referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," "third," and the like are used solely to distinguish one from another and are not to be construed as indicating or implying relative importance.
Furthermore, the terms "horizontal", "vertical" and the like do not imply that the components are required to be absolutely horizontal or pendant, but rather may be slightly inclined. For example, "horizontal" merely means that the direction is more horizontal than "vertical" and does not mean that the structure must be perfectly horizontal, but may be slightly inclined.
In the description of the present invention, it should also be noted that, unless otherwise explicitly specified or limited, the terms "disposed," "mounted," "connected," and "connected" are to be construed broadly and may, for example, be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Examples
Referring to fig. 2 and 4, the present application provides a sample stage 100 for an X-ray diffractometer, which includes a sample stage framework 110 and an amorphous structure membrane 120, in the embodiment, the sample stage framework 110 is connected to a bottom surface of the amorphous structure membrane 120 to support the amorphous structure membrane 120.
Referring to fig. 1, the sample stage frame 110 in the present application is formed by bending a flexible supporting rod 111, and it should be understood that in other embodiments of the present invention, the sample stage frame 110 may be formed by splicing other rod-shaped structures.
Specifically, in this embodiment, the support rod 111 is formed by bending according to the size of a standard sample stage collocated at the time of shipment of the X-ray diffractometer. Generally, the standard sample stage is of a rectangular parallelepiped structure and is provided with a rectangular sample well therein, approximately 0.5mm deep. In the application, the supporting rod 111 is used for bending according to the size of a standard sample table, and one free end of the supporting rod is extended into the middle of the sample table framework 110 so as to split the sample table framework 110 into two intervals.
Specifically, the sample platform framework 110 in the present application includes an outer frame section 112 and an inner partition section 113 connected to each other, the outer frame section 112 and the inner partition section 113 are integrally formed, the outer frame section 112 has a first free end 117, the inner partition section 113 has a second free end 118, and the first free end 117 is close to a side of the inner partition section 113 away from the second free end 118. The rectangular frame formed by bending is roughly in a shape of a Chinese character ri, wherein the outer frame section 112 is separated by the inner separation section 113 to form a first frame 114 and a second frame 115, and the first frame 114 correspondingly serves as an amorphous structure film 120 as a sample bearing surface 116 (i.e., a part a in fig. 4). The sample carrying surface 116 is used for carrying a sample, and the sample stage 100 for the X-ray diffractometer provided by the application is particularly suitable for a material with small powder quantity or a film material sample.
Further, the support rod 111 is a metal wire, preferably, the metal wire is any one of an iron wire, a copper wire, a stainless steel wire and a nickel wire. The diameter of the metal wire is 0.1-0.3 mm.
It is worth to be noted that, in the present application, the support rod 111 is bent according to the size of the standard sample stage to form the sample stage framework 110, and it is crucial whether the sample stage framework 110 can be fixed with the fixing clip of the existing X-ray diffractometer, therefore, in the present application, the diameter of the metal wire is limited to 0.1-0.3mm, and it can be ensured that the sample stage framework 110 formed by bending can be accurately matched with the fixing clip of the existing X-ray diffractometer. In addition, after the second frame 115 of the sample stage framework 110 is inserted into the fixing clip, based on the fact that the sample stage framework 110 in the present application has a certain thickness, the bottom of the sample stage framework 110 and the amorphous structure film 120 are empty, and such a design can make the sample stage 100 for the X-ray diffractometer in the present application have a certain downward inclination angle (1-10 degrees). From the diffraction angle, the weak change of the inclination angle can cause a larger deviation in the diffraction angle 2 theta direction, so that the original diffraction geometry can not meet the Bragg law any more, and the background peak can be effectively annihilated, therefore, the sample stage 100 for the X-ray diffractometer has a lower measurement background, and is more suitable for measuring the diffraction pattern of a very small amount of powder samples.
Referring to fig. 2 and fig. 3, in the present embodiment, the amorphous structure film 120 and the sample stage framework 110 are adhered by glue. Glue can guarantee seamless laminating between the two, guarantees the compactness of connecting. The glue in the application can be for example the rhino brand quick-repairing glue (model: KWIK GRIP), or can also be attached by adopting the conventional glue.
The amorphous structure film 120 in this application includes any one of a polyimide film, a polyethyleneimine film, a polyoxymethylene film, and a polymethyl methacrylate film. The thickness of the amorphous structure film 120 is 0.04-0.06mm, and the amorphous structure film is thin, so that the measurement background can be effectively reduced, and especially in the range of diffraction angles of 30-70 degrees, the amorphous structure film is basically the substrate background of an X-ray diffractometer. Utilize the amorphous structure membrane 120 to attach and form the sample platform on sample platform skeleton 110 in this application, on the sample loading end 116 that the amorphous structure membrane 120 that will await measuring was placed in first frame 114 and is formed, utilize the X ray to test, the test result is accurate, and the noise is low, noiseless peak, and is significant to nano-material research field and novel functional material's development.
Preferably, a polyimide film is selected as the amorphous structure film 120, and the polyimide film includes a pyromellitic polyimide film and a biphenyl polyimide film. The former is a product from DuPont, USA, with the trade name of Kapton, and is prepared from pyromellitic anhydride and diaminodiphenyl ether. The latter is produced by Nippon corporation under the trade name Uplix and is prepared from biphenyltetracarboxylic dianhydride and diphenyletherdiamine (R type) or m-phenylenediamine (S type). Any of the two categories may be selected for use in the present application.
The direct utilization has the pliability in this application, the easy wire of bending is as bracing piece 111, form sample platform skeleton 110 through bending, the manufacture process of whole skeleton is simple, the raw materials are easily obtained, thereby very big reduction sample platform skeleton 110's cost, and sample platform skeleton 110's size in this application designs according to the size of the standard sample platform when X-ray diffractometer produces, after sample platform skeleton 110 preparation is accomplished, tailor amorphous structure membrane 120 according to sample platform skeleton 110's size, then the laminating to sample platform skeleton 110 the side of going up can. The side of the amorphous structure film 120 not connected to the sample stage frame 110, i.e. the top side of the amorphous structure film 120, is used as the front side, wherein the first frame 114 should be used as the sample bearing side for bearing the sample corresponding to the part of the amorphous structure film 120. The sample stage 100 for the X-ray diffractometer provided by the application does not change the normal use of the original X-ray diffractometer, namely, when a material with a small amount of powder or a film material sample needs to be tested, the standard sample stage is replaced by the sample stage 100 for the X-ray diffractometer provided by the application.
The specific detection method comprises the following steps: the material or thin film material sample with small powder amount to be tested is placed on the sample bearing surface 116 of the amorphous structure film 120 of the first frame 114 of the sample stage 100 for the X-ray diffractometer, and then the detection is performed according to the normal detection method, that is, the X-ray is directly irradiated on the sample surface uniformly coated on the sample bearing surface 116 to detect the sample.
In addition, the application also provides the application of the sample stage 100 for the X-ray diffractometer in the X-ray diffractometer for testing thin-film materials and samples of materials with small powder quantity.
In addition, the application also provides an X-ray diffractometer, which comprises the sample stage 100 for the X-ray diffractometer, and the sample stage 100 for the X-ray diffractometer can be directly used by replacing the standard sample stage of the original X-ray diffractometer under the condition of not changing the use of the X-ray diffractometer, so that the application range of the X-ray diffractometer is expanded.
In this example, the sample stage 100 for an X-ray diffractometer provided in the present application was compared with a standard sample stage (glass substrate) for an X-ray diffractometer. Please refer to fig. 5 for comparison results.
As can be seen from FIG. 5, the glass substrate produces a significant interference peak (in the range of 20-40 degrees) and a very strong background (FIG. 5: top measurement line), resulting in inaccurate measurement data and difficulty in quantitative analysis. The sample stage 100 for an X-ray diffractometer in the present application has an extremely low background, and substantially overlaps with the background of the X-ray diffractometer itself. The application uses the metal wire to be bent to form the sample table skeleton 110, and the amorphous structure membrane 120 is attached to the top of the sample table skeleton 110, so that the amorphous structure membrane 120 is used as a measuring platform, the function of the amorphous structure membrane 120 can be fully utilized, the use is convenient, the price is low, the original experimental mode is not influenced, the extremely wide interference peak like glass is not generated within the range of 20-40 degrees of diffraction angles, the measuring background is very low, and the measurement of only a small amount of material samples is possible and the test data is accurate and reliable.
In summary, the present application provides a sample stage 100 for an X-ray diffractometer, which has an extremely low background and no background diffraction peak, is inexpensive, and can replace the currently commercially available measurement sample stage for an X-ray diffractometer, which is expensive (about 2000 rmb each). The application uses the metal wire to bend to form the sample stage framework 110, and attaches the clean and smooth amorphous structure membrane 120 to the top of the sample stage framework 110, so that the sample stage framework is used as a measuring platform. The test result shows that the sample stage 100 for the X-ray diffractometer prepared by the method is superior to a glass-substrate sample stage device in effect and low in price (probably every 10 RMB).
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A sample stage for an X-ray diffractometer is characterized by comprising a sample stage framework and an amorphous structure membrane, the top of the sample stage skeleton is connected with the bottom surface of the amorphous structure membrane to support the amorphous structure membrane, one side of the sample table skeleton is used for being inserted into the X-ray diffractometer, the sample table skeleton comprises an outer frame section and an inner partition section which are mutually connected, the outer frame section is separated by the inner partition section to form a first frame and a second frame, the first frame is correspondingly used as a sample bearing surface of the amorphous structural membrane, the second frame is inserted into a fixing clamp of the X-ray diffractometer, the amorphous structure film comprises any one of a polyimide film, a polyethylene imine film, a polyformaldehyde film and a polymethyl methacrylate film, and the thickness of the amorphous structure film is 0.04-0.06 mm.
2. The sample stage according to claim 1, wherein the outer frame section and the inner partition section are integrally formed and bent from a support rod.
3. The sample stage of claim 2, wherein the outer frame section has a first free end and the inner divider section has a second free end, the first free end being proximate a side of the inner divider section distal from the second free end.
4. The sample stage according to claim 2, wherein the support rod is a metal wire, preferably any one of an iron wire, a copper wire, a stainless steel wire and a nickel wire; preferably, the diameter of the wire is 0.1-0.3 mm.
5. The sample stage of claim 1, wherein the amorphous structure membrane and the sample stage skeleton are glued together.
6. Use of a sample stage for an X-ray diffractometer according to any one of claims 1 to 5 in an X-ray diffractometer for testing thin film materials, samples of materials with low amounts of powder.
7. An X-ray diffractometer comprising the sample stage for an X-ray diffractometer according to any one of claims 1 to 5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911066181.7A CN110887856B (en) | 2019-11-04 | 2019-11-04 | Sample table for X-ray diffractometer, application of sample table and X-ray diffractometer |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911066181.7A CN110887856B (en) | 2019-11-04 | 2019-11-04 | Sample table for X-ray diffractometer, application of sample table and X-ray diffractometer |
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| CN110887856A CN110887856A (en) | 2020-03-17 |
| CN110887856B true CN110887856B (en) | 2022-04-08 |
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