Spectrometer

Abstract

To provide a spectrometer that enables remote positioning of a crystal analyzer and a detector.SOLUTION: A first motor is configured to rotate a first arm for positioning a crystal analyzer, and a second motor is configured to rotate a fourth arm for positioning a detector via a third arm and a second arm. The first motor and the second motor operate independently so as to allow the detector and the crystal analyzer to rotate about a first axis and to move independently of each other.SELECTED DRAWING: Figure 3

Description

[Technical Field]

[0001] CROSS-REFERENCE TO RELATED APPLICATIONS This application supersedes U.S. Provisional Application No. 62 / 924,009, filed October 21, 2019. No. 6,239,999, filed on Oct. 1, 2003, which is incorporated by reference in its entirety.

[0002] STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT Not applicable

[0003] INCORPORATION-BY-REFERENCE OF MATERIAL SUBMITTED ON A COMPACT DISC Not applicable [Background technology]

[0004] A spectrometer (hereinafter referred to as "spectrometer") separates the target X-rays for quantitative analysis. The general process of wavelength dispersive fluorescence spectroscopy is to first detect a radiation source, e.g., X Incident X-rays from a ray tube or synchrotron beam, or electrons, protons, or ions The use of incident particle radiation, such as a beam of electrons, to induce the production of X-rays characteristic of a particular element. Once X-rays are generated in the sample, they are analyzed by a crystal analyzer with a defined lattice spacing. The X-rays from the sample hit the crystal analyzer at a specific angle. When the sample is irradiated, only X-rays with wavelengths that satisfy Bragg's law are diffracted. By controlling the length, the X-rays emitted from different regions of the sample with energy bands can be measured. The rays can be diffracted by interacting with a crystal analyzer. d) In the circular geometry, the X-rays are re-imaged onto the Rowland circle. Diffraction occurs in such a way that the energy of the light is spatially selected. By combining it with a type X-ray detector (hereinafter referred to as the detector) and placing the detector on this circle, The refocused X-rays from the beam are measured, and the X-rays measured on the detector are determined by the refocused position and energy. Alternatively, a single channel detector ( When using a point-to-point focusing (non-position sensitive), the spectrometer It can be operated in point-to-point focus mode. In this mode, a single X-ray energy is measured by the detector at each point. do.

[0005] In the Rowland circle geometry, the Rowland circle is determined by the position of the crystal analyzer. The detector should ideally be tangent to this circle. Once the Rowland circle is determined, In order for the analyzed X-rays to diffract towards the detector, the sample and detector must be positioned relative to the crystal analyzer. Generally, the sample must be positioned symmetrically relative to the exciting X-ray or incident beam. The crystal and detector are fixed in place, so the angle between the crystal and the detector can be changed to Change the Bragg angle of the X-rays from the material or source and the energy range being measured. Then, both the crystal analyzer and the detector must be moved to maintain the Rowland geometry. It must be.

[0006] Therefore, analyzing the fluorescence lines of various elements in a sample using a spectrometer is similar to analyzing with a crystal analyzer. The output devices must be constantly repositioned. There is a need for a spectrometer that can be reoriented as needed. The re-insertion device should be placed in an environment such as a vacuum or inert air glove box or chamber. In one embodiment, an inert The air glove box or chamber is filled with helium. In this case, the spectrometer is placed in a vacuum chamber or a chamber filled with helium. Such a spectrometer has two main applications. First, it measures the radiation emitted from the sample. This fluorescent X-ray may be used to measure the energy spectrum of the X-ray photons. When spectroscopy is performed with very high energy resolution, it is called X-ray emission spectroscopy (XES) This method is possible because X-rays are incident on the sample. Alternatively, electrons or other charged particles may be incident on the specimen, e.g., in an electron microscope. , or in a system for proton-induced XES. The tube or source detects the spectrum of photon energy being emitted by the X-ray source itself. The spectrometer may be directed to the entrance of the spectrometer so that the spectrometer is formed on the spectrometer.

[0007] In this case, the sample is inserted between the source and the analyzer, or between the analyzer and the detector. The change in the spectral intensity due to the insertion of the sample was analyzed to obtain the X-ray absorption fine structure (X Described herein are crystal analyzers and detectors that can determine the AFS. It is a spectrometer having a platform for manipulating and positioning the particles. Summary of the Invention

[0008] The invention described herein allows for the crystal analyzer and detector to be remotely located. It is a spectrometer having components that perform the following functions.

[0009] Other features and advantages of the present invention will become apparent from the following detailed description of preferred embodiments with reference to the accompanying drawings. This will become clear in the detailed description below (which will be established once the drawings are established). [Brief explanation of the drawings]

[0010] [Figure 1] FIG. 1 is a side view of a spectrometer; [Figure 2a] Figure 2a is a top view of the spectrometer; [Figure 2b] FIG. 2b is a perspective view showing an embodiment of a spectrometer; [Figure 2c] FIG. 2c is a side view showing an embodiment of a spectrometer; [Figure 3] FIG. 3 is a side view illustrating an embodiment of a spectrometer; [Figure 4a] FIG. 4 a is a side view showing an embodiment of a spectrometer; [Figure 4b] FIG. 4b is a side view showing an embodiment of a spectrometer; [Figure 5] FIG. 5 is a side view showing an embodiment of a spectrometer; [Figure 6] FIG. 6 is an environmental diagram illustrating an embodiment of a spectrometer; [Figure 7a] Figure 7a shows an example of a characteristic X-ray spectrum obtained using the spectrometer; [Figure 7b] Figure 7b shows another example of a characteristic X-ray spectrum obtained using the spectrometer; [Figure 7c] Figure 7c shows another example of a characteristic X-ray spectrum obtained using the spectrometer; [Figure 8a] FIG. 8a is an exemplary embodiment of a spectrometer showing a Bragg angle of 80°; [Figure 8b] FIG. 8b is an exemplary embodiment of a spectrometer showing a Bragg angle of 70°; [Figure 8c] FIG. 8c is an exemplary embodiment of a spectrometer showing a Bragg angle of 60°; [Figure 8d] FIG. 8d is an exemplary embodiment of a spectrometer exhibiting a Bragg angle of 50°. DETAILED DESCRIPTION OF THE INVENTION

[0011] In the following detailed description, reference is made to the accompanying drawings, which form a part hereof. In the drawings, the use of similar or identical symbols in different drawings This typically refers to similar or identical items unless the context dictates otherwise. show.

[0012] The exemplary embodiments described in the detailed description, drawings, and claims are intended to be limiting. It is not intended to deviate from the spirit or scope of the subject matter presented herein. Other embodiments may be utilized and other changes may be made without departing from the spirit and scope of the invention.

[0013] Those skilled in the art will recognize the components (e.g., operations), devices, objects, and The following and their accompanying discussions are used as examples to clarify concepts, and It will be recognized that various modifications of the design and construction are contemplated. As used in this document, the specific examples provided and the accompanying discussion are not intended to be limiting unless otherwise specified. The examples are intended to be representative of the general category. Even if it is, it is intended to be representative of its class and does not represent a particular configuration. A claim is not limited simply because it does not include elements (e.g., actions), devices, and objects. should not be interpreted.

[0014] This application uses formal summary headings for clarity of presentation. However, summary headings are for presentation purposes and various types of subject matter are It should be understood that there may be cases discussed throughout this application (e.g., where a device / structure may be described under the heading of a process / action and / or the process / action is may be considered under the heading of production / process and / or relate to a single topic (The description may cover more than one topic heading.) Therefore, a formal summary heading The use of is not intended to be limiting in any way. It's not something like that.

[0015] Referring to FIG. 1, according to one embodiment, the spectrometer (100) rotates around a first axis. a detector (40) and a crystal analyzer (30), which may be movably positioned; In some embodiments, the axis is centered on a Rowland circle (60) having a radius r. The detector (40) and the crystal analyzer (30) are connected to each other by the Bragg diffraction pattern generated by the crystal analyzer (30). The radiation source (51) is located within the receiving area of ​​the beam, and the beam is then moved along the Rowland circle (60). They may be placed independently.

[0016] The crystal analyzer (30) is operably attached to the first arm (1a) and Thus, the position of the first arm (1a) is controlled by the first electric motor (20a). The first arm (1a) has a distal end (21b) and a proximal end (21a). The first motor (20a) is operatively connected to the far end (21b) of the first arm (1a). The crystal analyzer (30) is attached to the distal end (21b) of the first arm (1a). In one embodiment, the crystal analyzer 30 can be mounted on any known column. The first motor (20a) is mounted to the far end (21b) using a mounting method. 30) in a tangent state, while moving the center of the Rowland circle. In one embodiment, the crystal analyzer (30) rotates relative to its mounting point. In one embodiment, the crystal analyzer is mounted so that the crystal analyzer is Its radial position r can be adjusted by moving it closer to or further from the axis. In one embodiment, the crystal analyzer 30 is mounted on a Johann The crystal surface is curved along a circle twice the size of the Rowland circle. In one embodiment, the crystal analyzer (30) is of the Johansson type. The crystal lattice planes are curved with a radius twice the size of the Rowland circle, The surface of the crystal is ground / prepared to have the same radius as the Rowland circle. In some embodiments, a diffraction grating is used instead of a crystal analyzer.

[0017] The first arm (1a) is operably attached to the second arm (1b). The arm (1b) has a proximal end (22a) and a distal end (22b). The proximal end (21a) of the first arm (1b) is operatively connected to the proximal end (22a) of the second arm (1b). The distal end (22b) of the second arm (1b) is operatively connected to a detector (40). In this embodiment, the detector (40) is mounted to the second arm using any known mounting method. In one embodiment, the detector (40) is mounted on the second arm (1b) with a detection surface. In one embodiment, the second arm (1b) is mounted perpendicular to the , the detector is mounted so that its radial position r can be adjusted.

[0018] The second arm (1b) is connected to the third arm (1c). The distal end (22b) of the second arm (1b) has a proximal end (23a) and a distal end (23b). ) is operatively connected to the proximal end (23a) of the third arm (1c). The second arm (1b) is connected to the first arm (1c) so that the detector (40) moves tangentially along the circle. 3 is operatively connected to the arm (1c).

[0019] The third arm (1c) is connected to the fourth arm (1d). The proximal end (23a) of the third arm (1c) has a distal end (24a) and a distal end (24b). The third arm (1d) is operatively connected to the proximal end (24a) of the fourth arm (1d). The distal end (24b) is operatively connected to a second electric motor (20b). The second motor (20b) is mounted to the fourth arm (1d) by any known mounting method. The second electric motor (20b) rotates the fourth arm (1d).

[0020] In one embodiment, a computing device (not shown) calculates the speed of the first electric motor (20a) and the speed of the second electric motor (20b). Figures 8a to 8d show examples of the spectrometer at several Bragg angles. 1 shows an exemplary embodiment.

[0021] Referring to Figures 1, 2a, 2b, and 2c, in one embodiment, a crystal analyzer (30) configured to receive X-rays emitted by or transmitted through the sample (51). In one embodiment, the crystal analyzer (30) is configured to measure the lattice spacing of the crystal analyzer (30) and and the orientation of the crystal analyzer (30) relative to the sample (51). It operates by selectively scattering radiation within a band via Bragg diffraction In another embodiment, the crystal analyzer (30) is configured to have a lattice spacing of the crystal analyzer (30) and a radiation source. and the orientation of the crystal analyzer (30) relative to (50), It operates by selectively scattering radiation within the range of 1000 Hz through Bragg diffraction. In some embodiments, the crystal analyzer 30 is cylindrically shaped. The analyzer 30 is shaped like a ring. In one embodiment, the crystal analyzer 30 is In one embodiment, the crystal analyzer 30 is shaped like a sphere. In another embodiment, the crystal analyzer 30 has a concentration circle having a diameter of about 20 to 100 In one embodiment, the detector (40) is a crystal analyzer. (30) Detect the count, intensity, and / or energy / wavelength of the diffracted X-rays. Those skilled in the art will appreciate that the detector 40 may be configured to emit a position-sensitive signal depending on the configuration. Those skilled in the art will recognize that the detector may be a single channel detector or a single channel detector. For example, the crystal analyzer (30) and the detector (40) may each be adjusted to achieve a desired configuration. It will be appreciated that the composition may comprise a variety of materials.

[0022] Referring to Figures 1, 2a, 2b, and 2c, in one embodiment, a crystal analyzer ( 30) and the detector (40) to maintain a tangent to the Rowland circle (60). In one embodiment, the first arm (1a) and the second arm (1b) are formed. The first electric motor (20a) rotates the first arm (1a), and the second electric motor (20b ) is adjusted to change the angle A between the detector (40) and the crystal analyzer (30). The arm (1d) then rotates the other connected arms (1b, 1c). In this state, the first electric motor (20a) rotates the first arm (1a), and the second electric motor ( 20b) while the sample (51) remains stationary, the detector (40) and the crystal analyzer ( The angle A between the crystal analyzer (30) and the sample (51) and the angle B between the crystal analyzer (30) and the sample (51) are equal. The arm (1d) is then connected to the other connected arm (1b, In one embodiment, the first electric motor (20a) or the second electric motor (1c) is rotated. 20b) can be moved independently to adjust the position of the crystal analyzer (30) and the detector (40). By adjusting this angle, it is possible to change the wavelength of the radiation source or The X-rays from the sample (51) are measured by the detector (40) so as to satisfy Bragg's law. It becomes possible to determine

[0023] Referring to FIG. 3, in one embodiment, the spectrometer (100) includes a linear translation stage (70 The linear translation stage (70) moves the motorized spectrometer (100) By moving the sample (51) and the crystal at least from the first position X1 to the second position X2, The distance between the sample and the analyzer (30) is varied while keeping the sample-crystal-detector angle constant. Referring to FIG. 6, in one embodiment, the spectrometer (100) is housed in an inert air globe. In one embodiment, the spectrometer (100) is housed in a vacuum chamber. In one embodiment, the spectrometer ( 100) is oriented so that the Rowland circle is on a vertical plane. The light source (100) is oriented so that the Rowland circle is on a horizontal plane.

[0024] Referring to FIG. 4, in some embodiments, the radiation source (50) may be an X-ray tube, a synchrotron, This may be a laser plasma X-ray source, a scanning electron microscope, a proton beam, or an ion beam. The radiation source (50) emits radiation from the sample (51) towards the crystal analyzer (30). configured to emit X-rays generated by a source (50) and directed toward a sample (51); In this embodiment, the detector (40) measures the X-ray emission spectrum of the sample (51). As used herein, a sample (51) is any material. Those skilled in the art will understand that when referring to the sample (51), the radiation source is explicitly referenced. It is understood that the sample (51) is operatively connected to the radiation source, whether or not it is connected to a radiation source. You will recognize that this is what you are trying to achieve.

[0025] Referring to Figure 5, in one embodiment, the radiation source (50) is in the form of an X-ray tube. In an embodiment, the radiation source (50) is configured to emit X-rays toward the crystal analyzer (30). The sample (51) may be arranged between the radiation source (50) and the crystal analyzer (30). The sample ( ) may be placed between the crystal analyzer ( 30 ) and the detector ( 40 ). By comparing the signal on the detector (40) with and without the sample (51), In another embodiment, the radiation source (50) can determine the X-ray absorption fine structure of It may be in the form of a synchrotron or laser plasma X-ray source.

[0026] In some embodiments, the spectrometer is utilized to study actinides. In this context, the spectrometer is used to study air-sensitive electrode materials for electrical energy storage. In one embodiment, the spectrometer is used to study air-sensitive materials for chemical catalysis. will be done.

[0027] In one embodiment, the computing device is configured to connect the crystal analyzer (30) to the sample (51) or the radiation source (5 0), so that multiple angles can be realized between the motors (20a, 20b), and then In one embodiment, the control unit 100 is programmed to control the control units 1a, 1b, 1c, and 1d. The computing device controls the motors (20a, 20b) to operate the crystal analyzer (30) and the detector. The device (40) is positioned at a predetermined position, such as a specific energy of elemental radiation. In one embodiment, the second motor (1b) is pre-programmed with a detector (40). The fourth arm is moved while the crystal analyzer (30) remains stationary. (1d), and thus the other connected arms (1c, 1b, 1a).

[0028] The high-resolution spectra of Figures 7a and 7b were obtained using a spectrometer (100) and Using motorization to tune to different energy ranges (i.e., emission lines), In an exemplary embodiment, the sample contains either phosphorus or sulfur containing compounds. For phosphorus and sulfur, the Kα spectrum consists of two closely spaced peaks. In the case of phosphorus compounds, the energy separation is about 0.85 eV, and in the case of sulfur compounds, the energy The energy separation is about 1.24 eV. demonstrates an energy resolution of <1 eV.

[0029] Figures 7a and 7b show the results for samples with very low oxidation states (e.g., S = -2 oxidation state). ZnS) and high oxidation state samples (e.g., CaSO4·2 with S=+6 oxidation state). This further illustrates the energy shift that occurs between the two atoms (H2O). For sulfur, the shift is about 1.35 eV. Measurement of the oxidation state allows determination of the chemical species in samples with mixed oxidation states. The first sample was CoS, but some of the sulfur was SO4 2- When indicating that the In one embodiment, the spectroscopic measurements are , to determine the oxidation state distribution of phosphorus and sulfur, e.g., the percentage oxidized and the percentage reduced. It is used to

[0030] Although various exemplary aspects and exemplary embodiments have been disclosed herein, other aspects and embodiments may be possible. Various exemplary aspects disclosed herein will be apparent to those skilled in the art. and the exemplary embodiments are for illustrative purposes only and are not intended to be limiting. It's not that.

Claims

1. A spectrometer comprising a detector and a crystal analyzer; the crystal analyzer being movable in a first arm. the detector is operably attached to the second arm; the detector is operably attached to the first arm; the first arm and the second arm are connected; and the detector and crystal analyzer rotate about a first axis. Spectrometers that move in a dynamic manner and independently of each other.

2. 2. The method of claim 1, wherein the axis is centered on a Rowland circle having a radius. Spectrometer as described.

3. The first arm and the front arm are aligned so that the crystal analyzer and the detector are tangent to a Rowland circle.

3. The spectrometer of claim 2, wherein the second arm is configured

4. 4. The spectrometer of claim 3, wherein the Rowland circle lies in a vertical plane.

5. 5. The spectrometer of claim 4, wherein the Rowland circle lies in a horizontal plane.

6. The crystal analyzer further includes a sample holder, the sample holder being configured to define a radiation path between the source and the crystal analyzer. The spectroscope of claim 1 located along a path.

7. a sample holder, the sample holder being positioned between the crystal analyzer and the detector; The spectrometer of claim 1 located along the radiation path.

8. 2. The method of claim 1, wherein the sample is within a range of the Bragg diffraction reception area of ​​the crystal analyzer. On-board spectrometer.

9. 10. The method of claim 9, wherein the radiation source is within a region of acceptance of Bragg diffraction by the crystal analyzer.

2. The spectrometer according to claim 1.

10. 10. The spectrometer of claim 1 used to study actinides.

11. The spectrometer of claim 1 , wherein the crystal analyzer has a cylindrical shape.

12. The spectrometer of claim 1 , wherein the crystal analyzer has a toroidal shape.

13. The spectrometer of claim 1 , wherein the crystal analyzer has a spherical shape.

14. 2. The spectrometer of claim 1, wherein the concentration circle has a diameter of between 10 cm and 100 cm.

15. and a linear translation stage, the linear translation stage moving the spectrometer to at least The spectrometer is moved from one first location to at least one second location.

10. The spectrometer of claim 1 , operably mounted to said linear translation stage.

16. 10. The spectrometer of claim 1 located in an inert gas chamber.

17. 17. The method of claim 16, wherein the method is used to study air-sensitive electrode materials for electrical energy storage. Spectrometer.

18. 17. The spectrometer of claim 16, for use in studying air-sensitive materials for chemical catalysis.

19. 10. The spectrometer of claim 1 located within a vacuum chamber.

20. 10. The spectrometer of claim 1, located in a chamber filled with helium.

21. 10. The spectrometer of claim 1, wherein the crystal analyzer is of the Johann type.

22. 10. The spectroscopic method of claim 1, wherein the crystal analyzer is of the Johansson type. vessel.

23. The method of claim 1 , wherein at least the first arm is operably attached to an electric motor. Spectrometer.

24. 10. The spectrometer of claim 1 used to measure oxidation state distribution.

25. 10. The spectrometer of claim 1, wherein a diffraction grating is used instead of a crystal analyzer.

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