CN107247061A - Neutron powder diffractometer detector Zero calibration method - Google Patents

Neutron powder diffractometer detector Zero calibration method Download PDF

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Publication number
CN107247061A
CN107247061A CN201710407455.9A CN201710407455A CN107247061A CN 107247061 A CN107247061 A CN 107247061A CN 201710407455 A CN201710407455 A CN 201710407455A CN 107247061 A CN107247061 A CN 107247061A
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China
Prior art keywords
detector
neutron
diffraction
powder diffractometer
diffraction spectra
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CN201710407455.9A
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Inventor
张洁
夏元华
谢超美
张莹
庞蓓蓓
王云
潘建
孙光爱
李建
黄朝强
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Institute of Nuclear Physics and Chemistry China Academy of Engineering Physics
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Institute of Nuclear Physics and Chemistry China Academy of Engineering Physics
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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
    • G01N23/207—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions
    • G01N23/2073—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions using neutron detectors
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/05—Investigating materials by wave or particle radiation by diffraction, scatter or reflection
    • G01N2223/056—Investigating materials by wave or particle radiation by diffraction, scatter or reflection diffraction
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/10—Different kinds of radiation or particles
    • G01N2223/106—Different kinds of radiation or particles neutrons
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/30—Accessories, mechanical or electrical features
    • G01N2223/303—Accessories, mechanical or electrical features calibrating, standardising
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/50—Detectors
    • G01N2223/501—Detectors array
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/60—Specific applications or type of materials
    • G01N2223/62—Specific applications or type of materials powders

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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Analytical Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)

Abstract

The invention discloses a kind of neutron powder diffractometer detector Zero calibration method, described method comprises the following steps：Neutron diffraction spectrum, background Ping Qu and diffraction peak intensity for estimating diffraction spectra are quickly measured using neutron powder diffractometer；Composed using the polarizers of big angle scope neutron diffraction of neutron powder diffractometer measurement standard powder sample；Part diffraction spectra data separating measured by every detector is come out, and the angle value of diffraction modal data is subtracted after the estimation initial value for corresponding to detector zero point, a diffraction spectra data file is individually preserved into；The part diffraction spectra measured using the diffraction spectra structure refinement analysis software of specialty to every detector carries out data Fitting Analysis, determines the null offset amount of every detector；The estimation initial value of every detector subtracts corresponding null offset amount and can be used as detector zero point.The characteristics of method of the present invention has wide adaptability, the degree of accuracy is high.

Description

Neutron powder diffractometer detector Zero calibration method
Technical field
The invention belongs to neutron diffraction field of measuring technique, and in particular to a kind of neutron powder diffractometer detector zero point Scaling method.
Background technology
Neutron powder diffractometer is widely used in physics and Material Field, its specific application field include but is not limited to Lower research field：The demarcation of the crystal structure and magnetic structure of powder and Polycrystalline；Material structure under condition of different temperatures is drilled Change process study；The accurate position for determining light atom and neighbour's atom and isotope in crystal structure；Set up in-situ chemical Gas-solid reaction kinetic equation.The operation principle of common neutron powder diffractometer is as described below：Drawn from reactor channel " white " continuous neutron beam, launches through the limitations of first collimator α 1 direction and is oriented to monochromator, monochromator is generally tabular monocrystalline Body, neutron monochromatic its a length of λ of specific family of crystal planes selection incident neutron Shu Zhongbo, they are reflected and is oriented to, accurate by second Straight device is to the testing sample being placed on sample stage；After incident " monochrome " neutron beam is scattered by sample elastic, according to different The different direction of family of crystal planes difference directive, the neutron for meeting Bragg equations is interfered in space, and scattered neutron intensity is by collimating The detector system step-scan of device and neutron counter composition, is used as the angle of diffraction 2θFunction be collected record so that shape Into neutron diffraction spectrum.During detector zero point is defined as every detector step-scan by direct puncture beam, the counting measured is most It is big to be worth the corresponding detector anglec of rotation in place.Detector relative efficiency is defined as every detector relative to a certain branch detector Counting efficiency.
From the operation principle of neutron powder diffractometer, the formation of neutron diffraction spectrum contains both sides key element：Visit Device is surveyed to count and the angle of diffraction.The degree of accuracy of detector relative efficiency demarcation directly affects the degree of accuracy of diffraction spectra counting, detection The degree of accuracy of device Zero calibration directly affects the degree of accuracy of the angle of diffraction.Therefore, it is to have to seek the high scaling method of the degree of accuracy very much It is necessary.The demarcation of conventional detector relative efficiency and detector zero point is through list by using all detector step-scans The monochromatic neutron beam of color device, every detector will obtain a neutron counting with the distribution of the detector anglec of rotation, and this is distributed Corresponding amplitude is set to explorer count at peak value, and the corresponding anglec of rotation at the peak value of the distribution is set into detector zero point, So as to obtain the relative efficiency and zero point value of detector.Detector zero point is demarcated using conventional method, its step is more simple, but The degree of accuracy is not high, especially in the case where beam intensity height and the 3rd collimater installation situation are less satisfied with, causes peak shape not Symmetrical and peak change difference is big, prevents detector zero point from obtaining accurate numerical value.
At present, no document report crosses relation technological researching.Therefore, on earth how in all cases can accurate calibration The detector zero point of neutron powder diffractometer, then be the problem of having to be solved in the prior art.
The content of the invention
In order to overcome the above-mentioned deficiencies of the prior art, the invention discloses a kind of neutron powder diffractometer detector zero point mark Determine method, demarcated exactly for the detector zero point to neutron powder diffractometer.
A kind of neutron powder diffractometer detector Zero calibration method, is comprised the following steps by the sequencing of execution：（1） Neutron diffraction spectrum, background Ping Qu and diffraction peak intensity for estimating diffraction spectra are quickly measured using neutron powder diffractometer；（2） Composed using the polarizers of big angle scope neutron diffraction of neutron powder diffractometer measurement standard powder sample；（3）Every detector is surveyed The part diffraction spectra data separating obtained is come out, and the angle value of diffraction modal data is subtracted to the estimation initial value for corresponding to detector zero point Afterwards, a diffraction spectra data file is individually preserved into；（4）Every is detected using the diffraction spectra structure refinement analysis software of specialty The part diffraction spectra that device is measured carries out data Fitting Analysis, determines the null offset amount of every detector；（5）Every detector Estimation initial value subtracts corresponding null offset amount and can be used as detector zero point.
Detector used in the neutron powder diffractometer be one group as combined by branched proportional counter tube into arc Detector array, the detector array can rotate around sample center for axle, and stepping angle is less than 0.1 °.
The standard powder sample has the crystal structure determined, and neutron diffraction peak intensity is high, quantity is more, distribution model Enclose it is wide, be evenly distributed, such as Y2O3Standard powder sample.
The top of the neutron diffraction spectrum counts amplitude and is more than 5000.
The diffraction spectra angular range comprises at least two obvious diffraction with the part diffraction spectra measured by every detector Peak is defined, generally, and the angular range needs to be more than 15 °.
The diffraction peak-to-peak amplitude and background Ping Qu ratio should be greater than 1.5.
Compared to the scaling method of traditional step-scan direct puncture beam, scaling method of the invention has higher adaptability, The situation of accurate calibration is unable to for various conventional methods（Such as monochromatic neutron streaming intensity height and the 3rd collimater installation situation Situation about being less satisfied with）, this method remains to accurate calibration detector zero point.
Embodiment
A kind of neutron powder diffractometer detector Zero calibration method, and in particular to one kind is used for neutron powder diffractometer Detector zero point accurate calibration method.
A kind of neutron powder diffractometer detector Zero calibration method, comprises the following steps：
The first step, diffraction count estimation：Neutron diffraction spectrum is quickly measured using neutron powder diffractometer, for estimating diffraction spectra Background Ping Qu and diffraction peak intensity；
Second step, neutron diffraction spectrometry：Use the polarizers of big angle scope neutron of neutron powder diffractometer measurement standard powder sample Diffraction spectra；
3rd step, data are preserved：Part diffraction spectra data separating measured by every detector is come out, and by diffraction modal data Angle value subtract after the estimation initial value of correspondence detector zero point, individually preserve into a diffraction spectra data file；
4th step, data analysis：Spread out the part measured using the diffraction spectra structure refinement analysis software of specialty to every detector Penetrate spectrum and carry out data Fitting Analysis, determine the null offset amount of every detector；
5th step, determine zero point：The estimation initial value of every detector subtracts corresponding null offset amount and can be used as detector zero Point.
Described a kind of neutron powder diffractometer detector Zero calibration method, it is characterised in that the neutron powder spreads out Penetrate detector used in instrument be one group as combined by branched proportional counter tube into curved detector array, the detector array It can be rotated around sample center for axle, stepping angle is less than 0.1 °.
The standard powder sample has the crystal structure determined, and neutron diffraction peak intensity is high, quantity is more, distribution model Enclose it is wide, be evenly distributed, such as Y2O3Standard powder sample.
The top of the neutron diffraction spectrum counts amplitude and is more than 5000.
The diffraction spectra angular range comprises at least two obvious diffraction with the part diffraction spectra measured by every detector Peak is defined, generally, and the angular range needs to be more than 15 °.
The diffraction peak-to-peak amplitude and background Ping Qu ratio should be greater than 1.5.
Embodiments of the invention are elaborated below, the present embodiment is directed under premised on technical solution of the present invention Specific neutron powder diffractometer（High-resolution neutron powder diffractometer）Implemented, give detailed embodiment and tool The operating process of body, but protection scope of the present invention is not limited to following embodiments.
Embodiment：
Neutron powder diffractometer detector Zero calibration specific implementation step sequentially performs as follows：
（1）By standard sample Y2O3Load after Special sample bar, be placed in sample stage center, and with positioner special in sample The heart is highly adjusted to beam center height；
（2）Rotary switch on additional gate switch board is allocated to " opening " shelves, additional gate is opened；
（3）After gate is fully opened, operation high-resolution Neutron diffractometer program carries out diffraction spectra and quickly measured, and uses monitor Count mode（Watchdog count is set, and each point time of measuring is about 1min）, detector anglec of rotation start angle is 160 °, Termination point is 163 °, and measurement step pitch is 0.05 °；
（4）After being quickly measured, high-resolution Neutron diffractometer program is reruned, watchdog count pattern is used（According to Previous step measurement result, estimates the watchdog count that should be set, it should be ensured that each point time of measuring is more than 5min）, detector rotation Gyration start angle is 150 °, and termination point is 170 °, and measurement step pitch is 0.05 °；
（5）Click on " START " button in high-resolution Neutron diffractometer program and start measurement neutron diffraction spectrum；
（6）High-resolution Neutron diffractometer program is obtained after complete neutron diffraction spectrum automatically, using the program by experimental data Save as text formatting（*.txt）；
（7）Rotary switch on additional gate switch board is allocated to " closing " shelves, additional gate is closed, gate to be appended is closed completely After closing, remove sample and be under lock and key；
（8）Separated every detector is recorded from the experimental data for preserving into text formatting, it is each to count pair The angle value answered subtracts the initial value C of correspondence detector0[i]（C0[i]=2.5*（5-i）, wherein i represent detector number）Afterwards, Diffraction spectra data file is saved as by the value is corresponding with each explorer count；
（9）Diffraction modal data obtained by every detector measurement is fitted using FullProf softwares, every detection is obtained by fitting The null offset amount P of device0[i]；
（10）The initial value C of correspondence detector0[i] subtracts null offset amount P0[i] is that can determine that detector zero point.

Claims (5)

1. a kind of neutron powder diffractometer detector Zero calibration method, it is characterised in that described method comprises the following steps： Neutron diffraction spectrum, background Ping Qu and diffraction peak intensity for estimating diffraction spectra are quickly measured using neutron powder diffractometer；Make Composed with the polarizers of big angle scope neutron diffraction of neutron powder diffractometer measurement standard powder sample；By the portion measured by every detector Point diffraction spectra data separating comes out, and the angle value of diffraction modal data is subtracted after the estimation initial value of correspondence detector zero point, single Solely preserve into a diffraction spectra data file；Every detector is measured using the diffraction spectra structure refinement analysis software of specialty Part diffraction spectra carries out data Fitting Analysis, determines the null offset amount of every detector；The estimation initial value of every detector subtracts Corresponding null offset amount is gone to can be used as detector zero point.
2. neutron powder diffractometer detector Zero calibration method according to claim 1, it is characterised in that：The neutron Detector used in powder diffractometer be one group as combined by branched proportional counter tube into curved detector array, the detection Device array can rotate around sample center for axle, and stepping angle is less than 0.1 °.
3. neutron powder diffractometer detector Zero calibration method according to claim 1, it is characterised in that：The standard Powder sample is Y2O3。
4. neutron powder diffractometer detector Zero calibration method according to claim 1, it is characterised in that：The neutron The top of diffraction spectra counts amplitude and is more than 5000.
5. neutron powder diffractometer detector Zero calibration method according to claim 1, it is characterised in that：The diffraction Compose angular range and be more than 15 °.
CN201710407455.9A 2017-06-02 2017-06-02 Neutron powder diffractometer detector Zero calibration method Pending CN107247061A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107703168A (en) * 2017-10-13 2018-02-16 中国工程物理研究院材料研究所 A kind of crystal diffraction signal acquiring method
CN118032831A (en) * 2024-04-11 2024-05-14 南京航空航天大学 Powder diffraction analysis method and device based on gas detector

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CN104330427A (en) * 2014-10-24 2015-02-04 西安电子科技大学 Method applied to measurement of stress distribution information of c-surface GaN material along c axis
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CN103257150A (en) * 2012-08-31 2013-08-21 云南北方驰宏光电有限公司 Crystal direction finder for directly measuring deflecting angle in crystal orientation and measurement method thereof
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CN104330427A (en) * 2014-10-24 2015-02-04 西安电子科技大学 Method applied to measurement of stress distribution information of c-surface GaN material along c axis
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107703168A (en) * 2017-10-13 2018-02-16 中国工程物理研究院材料研究所 A kind of crystal diffraction signal acquiring method
CN118032831A (en) * 2024-04-11 2024-05-14 南京航空航天大学 Powder diffraction analysis method and device based on gas detector
CN118032831B (en) * 2024-04-11 2024-06-11 南京航空航天大学 Powder diffraction analysis method and device based on gas detector

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