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Combined device for small-angle and wide-angle X-ray scattering and experiment test method of combined device

An X-ray and wide-angle technology, which is applied in small-angle and wide-angle X-ray scattering devices and its experimental testing field, can solve problems such as research that is difficult to specialize, limited space, and restrictions, and achieves continuous adjustable spot size and light source High flux and brightness, easy installation and debugging

Active Publication Date: 2015-01-14
合肥中科优材科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the two major international X-ray instrument manufacturers Bruker (NanoStar) and Rigaku (S-Max3000) have commercialized small-angle X-ray scattering instruments, but there is no very mature small-angle and wide-angle X-ray scattering combined device.
At the same time, commercial instruments focus on universality and are mostly used for analysis, but it is difficult to use them for specialized research
For example, although the sample environment provides a variety of configurations, the relatively limited space and vacuum requirements greatly limit the research on in situ structural changes.

Method used

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  • Combined device for small-angle and wide-angle X-ray scattering and experiment test method of combined device
  • Combined device for small-angle and wide-angle X-ray scattering and experiment test method of combined device
  • Combined device for small-angle and wide-angle X-ray scattering and experiment test method of combined device

Examples

Experimental program
Comparison scheme
Effect test

experiment example 1

[0055] One-dimensional linear detector detects wide angle range test.

[0056] experiment procedure:

[0057] Firstly, the micro-focus X-ray light source is raised to full power (45KV, 650μA), and the three four-knife slit collimation optical paths are evacuated to the normal state (3×10 -1 mbar). Place the one-dimensional linear detector at a suitable position 90mm away from the sample. Turn on the argon / methane (90 / 10) mixed gas, adjust the pressure to 7.5 bar, the gas flow rate is 0.17-0.45 I Ar / h, and flush the detector for 30 min. Adjust the bias voltage of the one-dimensional linear detector to 3.3KV, and then slowly increase the bias voltage to 3.7KV, so that the energy spectrum peak position is at the channel number of 650-700. Turn on the light source shutter and the one-dimensional linear detector acquisition software to collect the X-ray one-dimensional scattering diagram of isotactic polypropylene.

[0058] Experimental results:

[0059] Figure 5 It is the o...

experiment example 2

[0061] Largest-scale testing of small-angle measurements in two-dimensional multi-filament gas detectors.

[0062] experiment procedure:

[0063] Adopt 1600mm vacuum pipe, 4×4.2mm 2 The straight-through light blocker combination is installed to adjust the light path. Three four-blade slit collimation optical paths and vacuum pipes are evacuated to normal state (3×10 -1 mbar), raise the microfocus X-ray source to full power (45KV, 650μA). Adjust the slit collimation light path, define a certain spot size, and block stray light. Bovine tendon collagen was placed on the sample stage as a standard sample for detection.

[0064] Experimental results:

[0065] Image 6 It is the two-dimensional small-angle scattering diagram of bovine tendon collagen under this test condition and the one-dimensional scattering curve obtained by integrating the two-dimensional small-angle scattering diagram. Experimental results show that the largest scale of the small-angle test is larger tha...

experiment example 3

[0067] In situ study of the structural evolution of the nanolayered sample S6 during the swelling process.

[0068] experiment procedure:

[0069] Adopt 800mm vacuum pipe, 6×6mm 2 The straight-through light blocker combination is installed to adjust the light path. Three four-blade slit collimation optical paths and vacuum pipes are evacuated to normal state (3×10 -1 mbar), raise the microfocus X-ray source to full power (45KV, 650μA). Adjust the bias voltage of the one-dimensional linear detector to 3.3KV, and then slowly increase the bias voltage to 3.7KV, so that the energy spectrum peak position is at the channel number of 650-700. Turn on the 2D multifilament gas detector power and bias. The S6 sample was placed in the sample cell, and the one-dimensional linear detector and the two-dimensional multi-wire gas detector were turned on at the same time to collect wide-angle and small-angle signals. During the experiment, a micro-injector was used to gradually add water ...

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Abstract

The invention provides a combined device for small-angle and wide-angle X-ray scattering and an experiment test method of the combined device. The device adopts a microfocus X-ray source used for providing parallel, high-brightness and high-quality X-rays. Three four-knife-edge-slit collimating light paths are arranged to precisely define the light spot pattern and filter off stray lights. A one-dimensional linear detector and a two-dimensional multi-wire gas detector are combined to respectively detect wide-angle and small-angle X-ray scattered signals so as to obtain a material structure from 0.1 nanometers to 100 nanometers. Different lengths of vacuum pipes and different sizes of direct light barriers are arranged in the device, so that the device can adjust the distance between a sample and the detector and can ensure high luminous flux and spatial resolution of the scattered signals under the premise of meeting the requirement on angle testing. The device provided by the invention has the advantages of large test range, easiness in adjustment and so on, and is very suitable for in-situ detection, so that the device is a good tool for studying high polymer materials, inorganic nano-materials, biomedical materials, other soft materials and so on.

Description

technical field [0001] The invention relates to a technology for in-situ research on material structure evolution by combining small-angle and wide-angle X-ray scattering, in particular to a combined small-angle and wide-angle X-ray scattering device and an experimental testing method thereof. Background technique [0002] The power of X-rays lies in the combination of small-angle and wide-angle X-ray scattering. Combining small-angle and wide-angle X-ray scattering, it is possible to simultaneously detect material structures ranging from 0.1 nanometers to 100 nanometers, that is, from molecular arrangements to nanometer self-assembled structures. With the help of the development of X-ray generators, optics and detectors in recent years and some sample environment control devices, the small-angle and wide-angle X-ray scattering combined devices can be used to study chemical reactions, material processing, and structure and performance changes in organisms in situ in real tim...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N23/203
Inventor 李良彬崔昆朋孟令蒲刘艳萍赵佰金
Owner 合肥中科优材科技有限公司
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