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Wide-angle scattering test method and device based on single-crystal diffractometer

A single crystal diffractometer and testing method technology, applied in the field of optics, can solve the problems of high maintenance cost, data extraction and analysis limitations, and limit the application field of analysis methods, etc., and achieve the effect of high signal-to-noise ratio

Pending Publication Date: 2021-06-29
WESTLAKE UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] 1. The equipment purchase is expensive and the maintenance cost is high;
[0004] 2. The traditional small-angle scattering instrument is usually tested at room temperature, which limits the application field of the analysis method to a large extent;
[0005] 3. The wide-angle scattering two-dimensional spectrum collected by the small-angle scattering instrument is usually a part of the Debye ring, and the data collection takes a long time, which has certain limitations on data extraction and analysis
[0006] In the prior art, there is no method for wide-angle scattering testing by single crystal diffractometer. The classic application of single crystal diffractometer (single crystal XRD) is to test the single crystal structure, but the purchase cost of small angle diffractometer SAXS is high, so there is an urgent need A wide-angle scattering test method and device based on a single crystal diffractometer for solving the above-mentioned technical problems

Method used

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  • Wide-angle scattering test method and device based on single-crystal diffractometer
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  • Wide-angle scattering test method and device based on single-crystal diffractometer

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Experimental program
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Effect test

Embodiment 1

[0050] This protocol is for transmissive samples, the specific steps are:

[0051] The first step: sample preparation: solid powder, fiber, polymer and other large particle materials can be fixed on the crystal ring column; gel and liquid sample preparation can be directly fixed in the crystal ring;

[0052] Step 2: Sample centering: Center the sample with the center of the goniometer. In this step, since the single crystal XRD is a quaternary diffractometer, there are four rotational degrees of freedom Chi (tilt in the vertical direction), Phi (rotation in the horizontal direction), 2Theta (rotation of the detector) and Omega (rotation of the sample), and Coupled with the height adjustment on the goniometer head, the adjustment of the left and right and front and back positions, it can accurately locate the center of the sample, have higher operation controllability and improve the collection of scattered signals, where the goniometer head is a part of the goniometer;

[005...

Embodiment 2

[0056] The difference between this embodiment 2 and embodiment 1 lies in the difference of the samples to be tested.

[0057] Step 1: Sample preparation and sample fixation: The sample preparation of the grazing incidence method can use the crystal base (remove the loop ring on the top), and fix the thick sample or the sample grown on the thick substrate (the substrate is thicker than 1mm) on the The crystal ring base is ready.

[0058] The second step: sample centering: center the sample with the center of the single crystal XRD light path.

[0059] Step 3: Select X-ray light source 5: Single crystal XRD can have 2 kinds of light sources to choose from, copper target or molybdenum target.

[0060] Step 4: Select an appropriate distance between the sample and the detector, and set an appropriate exposure time to collect scattered signals.

Embodiment 3

[0062] The first step: select Cu target X-rays, first increase the Cu target X-ray light source 5 to full power (50kV, 1.2mA), and set the two-dimensional surface detector 1 to a suitable distance from the sample, such as 60mm or more from the sample , adjust the sample to the center of the goniometer in the field of view of the camera, set a suitable exposure time, such as 30s or longer, and then the two-dimensional detector collects the X-ray two-dimensional scattering map.

[0063] Step 2: Use Bruker APEX3 and EVA software to integrate the two-dimensional scattering diagram to obtain the X-ray one-dimensional diffraction angle 2theta diagram or phase angle gamma diagram, such as Figure 4 It is the diffraction angle 2theta diagram, the ordinate in this figure represents the signal strength counts, and the abscissa represents the 2theta diffraction angle, such as Figure 5 It is a phase angle gamma diagram, in which the ordinate represents the signal strength counts, and the...

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Abstract

The invention relates to a wide-angle scattering testing method and device based on a single-crystal diffractometer. According to the scheme, the wide-angle scattering testing method comprises the following steps: preparing and placing a sampleon a sample table; centering the sample with the single crystal XRD center; selecting an X-ray light source, so that the X-ray light source is aligned with the sample, and the X-ray light source is a copper target and a molybdenum target which are switched and matched; setting the distance between the sample and the single crystal XRD surface detector, and setting exposure time to collect scattered signals; collecting the scattered X-rays through a two-dimensional surface detector; and integrating the two-dimensional scattering spectrogram to obtain an X-ray one-dimensional diffraction angle 2theta diagram or a phase angle gamma diagram. The scheme combines the characteristics of spot focusing and two-dimensional surface detection of the single crystal XRD, expands the application field of the single crystal XRD, is compatible with the characterization of solid and liquid materials, has extremely high tolerance to the materials, gives consideration to wide-angle scattering of transmission and grazing incidence modes, and is rapid, efficient and economical.

Description

technical field [0001] The invention relates to the field of optical technology, in particular to a wide-angle scattering test method and device based on a single crystal diffractometer. Background technique [0002] At present, the traditional wide-angle scattering test needs to be completed by specific equipment, such as a small-angle scattering meter, but it has the following disadvantages: [0003] 1. The equipment purchase is expensive and the maintenance cost is high; [0004] 2. The traditional small-angle scattering instrument is usually tested at room temperature, which limits the application field of the analysis method to a large extent; [0005] 3. The wide-angle scattering two-dimensional spectrum collected by the small-angle scattering instrument is usually a part of the Debye ring, and the data collection takes a long time, which has certain limitations on the extraction and analysis of the data. [0006] In the prior art, there is no method for wide-angle s...

Claims

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Application Information

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IPC IPC(8): G01N23/207
CPCG01N23/207
Inventor 缪晓和
Owner WESTLAKE UNIV
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