CN204832070U - Radiographic inspection recording system for X X -ray diffractometer based on SDD detector - Google Patents

Radiographic inspection recording system for X X -ray diffractometer based on SDD detector Download PDF

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CN204832070U
CN204832070U CN201520522655.5U CN201520522655U CN204832070U CN 204832070 U CN204832070 U CN 204832070U CN 201520522655 U CN201520522655 U CN 201520522655U CN 204832070 U CN204832070 U CN 204832070U
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ray
detector
sdd detector
sdd
diffractometer
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徐晓明
苗伟
陶琨
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Tsinghua University
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Tsinghua University
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Abstract

The utility model discloses a radiographic inspection recording system for X X -ray diffractometer based on SDD detector, including SDD detector, single track pulse analyzer, the SDD detector is used for receiving the X ray and shines the diffracted ray that the sample produced, the SDD detector, the single track pulse analyzer connects gradually, connects with X X -ray diffractometer data logging system again. The utility model has the advantages of as follows: do not need the graphite monochromator can get rid of cu K -beta ray to increase strength 3 -4 doubly, SDD detector itself does not need the water -cooling, does not need the forced air cooling even, and the fault rate is low, installation and simple to use, energy -conservation nature is good, the feature of environmental protection is good, with low costs, easy maintenance.

Description

X-ray diffractometer based on SDD detector X-ray detection X register system
Technical field
The utility model relates to X-ray diffraction analysis field, is specifically related to a kind of X-ray diffractometer X-ray detection X register system based on SDD detector.
Background technology
The main performance index of X-ray diffractometer is angular accuracy and diffracted intensity etc.
General use X ray light pipe produces copper target X ray.
Have two kinds of approach for improving intensity (improve the data precision and work efficiency), one is adopt rotary target, can bring up to 8kW by the 1.6kW of X-ray tube, but its shortcoming is cost increase is about 4-6 ten thousand dollars.Meanwhile, power consumption increase about 12kW (comprising water-cooled power).
Another approach improves detector.
Historical development develops into proportional counter and scintillation detector from Geiger counter tube (not having energy resolution), until 1996.The shortcoming of these two kinds of detectors is that energy resolution is respectively about 25% and 50%.Therefore in most cases, when using above-mentioned detector to detect CuK-alpha diffracted ray (8.05keV), the CuK-beta ray that energy is 8.9keV can not be got rid of, cause correctly analyzing.Meanwhile, during as contained the elements such as Fe, Ni, Cr, Mn in sample, the background that its fluorescence causes is extremely serious, and the peak back of the body is doubly even more than decline tens.Fig. 1 is the diffraction geometrical light-path schematic diagram of the diffractometer being furnished with scintillation detector or proportional detector.Because the energy resolution of scintillation detector and proportional detector is not high, CuK-beta ray can not be got rid of, so graphite monochromator must be added before the detectors, remove CuK-beta ray and fluorescence, and the efficiency of graphite monochromator is about 25%, cause loss of strength about 75%.
1996, the X-ray part (Xian Gaishu Brooker company) of former Siemens Company releases Si (Li) detector of powder diffractometer use, its energy resolution reaches about 260eV, then can get rid of CuK-beta ray, can exempt from dress graphite monochromator and improve intensity about 4 times.But its problem is linear gauge digit rate scope only can reach about 50kcps, and needs detector fills water-cooling system.Fragile and namely eliminated soon.
PANalytical company was proposed Si detector array in 1999.Inside establish nearly ~ 100 bar shaped detectors, the intensity of including when they being in separately certain same angle of diffraction add and, as the diffracted intensity of this angle, then intensity can become the increase of tens times.
But this kind of detector array has its own shortcomings:
1. its energy resolution is ~ 25%, can not get rid of CuK-beta ray and fluorescent.After improving for many years, still can only reach ~ 1keV, still cannot solve the problem.
2. can not record the diffraction peak that angle of diffraction is less than 3 °, and some samples, as clay mineral etc., need record from less than 3 °, even record from 0.6 °, thus can not use.
3. can not be used for the test analysis of some relatively more special (also often using), as phi scanning, rocking curve, pole figure tests, In-Plane Measurement and analysis, small angle scattering analysis etc.
4. cost is high, is equipped with import with external diffractometer main frame, needs 20,000 dollars.And as improved on existing machines, or be equipped with domestic diffractometer, need 40,000 dollars.Domestic diffractometer producer once outside associated country regarding businesses be that China produces, offer as design charges 8,000,000 yuans and development expense 8,000,000 yuans, later price is not also interior.
Therefore, the domestic annual diffractometer about 100 produced now, can only maintain the level of low diffracted intensity.Meanwhile, the diffractometer of import, when doing pole figure, In-Plane analysis, small angle scattering analysis, phi scanning, low angle diffraction etc. and analyzing, is also that intensity is not enough, analyzes trouble.
Utility model content
The utility model is intended at least one of solve the problems of the technologies described above.
For this reason, the purpose of this utility model is to propose a kind of X-ray diffractometer X-ray detection X register system based on SDD detector.
To achieve these goals, the embodiment of first aspect of the present utility model discloses a kind of X-ray diffractometer X-ray detection X register system based on SDD detector, comprise SDD detector, single-channel analyzer, the diffracted ray that described SDD detector produces for receiving x-ray bombardment sample, described SDD detector, described single-channel analyzer connect successively, then are connected with X-ray diffractometer digital data recording system.
According to the X-ray diffractometer based on SDD detector of the utility model embodiment X-ray detection X register system, do not need graphite monochromator can get rid of CuK-beta ray, and improve intensity 3-4 doubly; SDD detector itself does not need water-cooled, does not even need air-cooled, failure rate is low, installs and uses simple; Good energy saving property, the feature of environmental protection are good, cost is low, easy to maintenance.
In addition, according to the X-ray diffractometer based on SDD detector of the utility model above-described embodiment X-ray detection X register system, following additional technical characteristic can also be had:
Further, the energy resolution of described SDD detector to CuK-alpha ray is better than 200eV, can get rid of CuK-beta ray.
Further, the useful detection area of described SDD detector is greater than 150mm 2or the yardstick of Received signal strength on certain direction is greater than 13mm.
Additional aspect of the present utility model and advantage will part provide in the following description, and part will become obvious from the following description, or be recognized by practice of the present utility model.
Accompanying drawing explanation
Above-mentioned and/or additional aspect of the present utility model and advantage will become obvious and easy understand from accompanying drawing below combining to the description of embodiment, wherein:
Fig. 1 is the diffractometer light channel structure block diagram being furnished with flicker/proportional detector of the prior art;
Fig. 2 is the diffractometer light channel structure block diagram being furnished with SDD detector of the utility model embodiment;
Fig. 3 is the CuK-alpha ray multiple tracks energy spectrogram with SDD detector test Si powder sample of the utility model embodiment;
Fig. 4 is the diffracting spectrum with SDD detector test Si powder sample of the utility model embodiment;
Fig. 5 is the collection of illustrative plates comparison diagram installing scintillation detector and SDD detector test Si powder on import diffractometer of the utility model embodiment;
Fig. 6 is the collection of illustrative plates comparison diagram installing proportional detector and SDD detector test Si powder on domestic diffractometer of the utility model embodiment;
Fig. 7 is the collection of illustrative plates comparison diagram installing scintillation detector and SDD detector test Fe2O3 sample on import diffractometer of the utility model embodiment
Fig. 8 is the collection of illustrative plates comparison diagram installing proportional detector and SDD detector test Fe2O3 sample on domestic diffractometer of the utility model embodiment.
Embodiment
Be described below in detail embodiment of the present utility model, the example of described embodiment is shown in the drawings, and wherein same or similar label represents same or similar element or has element that is identical or similar functions from start to finish.Being exemplary below by the embodiment be described with reference to the drawings, only for explaining the utility model, and can not being interpreted as restriction of the present utility model.
In description of the present utility model, it will be appreciated that, term " " center ", " longitudinal direction ", " transverse direction ", " on ", D score, " front ", " afterwards ", " left side ", " right side ", " vertically ", " level ", " top ", " end ", " interior ", orientation or the position relationship of the instruction such as " outward " are based on orientation shown in the drawings or position relationship, only the utility model and simplified characterization for convenience of description, instead of indicate or imply that the device of indication or element must have specific orientation, with specific azimuth configuration and operation, therefore can not be interpreted as restriction of the present utility model.In addition, term " first ", " second " only for describing object, and can not be interpreted as instruction or hint relative importance.
In description of the present utility model, it should be noted that, unless otherwise clearly defined and limited, term " installation ", " being connected ", " connection " should be interpreted broadly, and such as, can be fixedly connected with, also can be removably connect, or connect integratedly; Can be mechanical connection, also can be electrical connection; Can be directly be connected, also indirectly can be connected by intermediary, can be the connection of two element internals.For the ordinary skill in the art, concrete condition the concrete meaning of above-mentioned term in the utility model can be understood.
With reference to description below and accompanying drawing, by these and other aspects of clear embodiment of the present utility model.In these descriptions and accompanying drawing, specifically disclose some particular implementation in embodiment of the present utility model, represent some modes of the principle implementing embodiment of the present utility model, but should be appreciated that the scope of embodiment of the present utility model is not limited.On the contrary, embodiment of the present utility model comprise fall into attached claims spirit and intension within the scope of all changes, amendment and equivalent.
Describe according to the X-ray diffractometer based on SDD detector of the utility model embodiment X-ray detection X register system below in conjunction with accompanying drawing.
Fig. 2 is the structured flowchart (technical scheme) of the diffractometer being furnished with SDD detector.As we can see from the figure, compared to Figure 1, this detector is used to eliminate graphite monochromator.When the angular instrument of diffractometer is in a certain angle place, incident X-rays produces diffracted ray on sample, and this ray directly enters SDD detector afterwards.SDD detector enters the light signal of detector by photoelectric effect detection, and this signal is changed into the pulse of certain form and exports.The pulse signal exported enters into single channel pulse height analyzer.Through experiment, the energy window of single channel pulse height analyzer can be set, only allow the pulse signal in this energy window to pass through, and enter into the counting circuit of diffractometer, thus obtain the diffracted intensity at this angle of diffraction place.
With the contrast of prior art:
Sum up, in the world today for the configuration of X-ray diffractometer, a few like this class can be divided into: the first kind: X ray light pipe+graphite monochromator+flicker/proportional detector; Equations of The Second Kind: X ray light pipe+detector array; 3rd class: rotary target X ray+graphite monochromator+flicker/proportional detector; 4th class: rotary target X ray+detector array.
X-ray diffractometer uses this technical scheme of SDD detector, and compared with configuring with the above-mentioned first kind, its advantage is:
1. because resolution is higher, can graphite monochromator be saved, thus intensity 3-4 can be improved doubly, increase work efficiency;
2. cost can decrease;
X-ray diffractometer uses this technical scheme of SDD detector, and compared with configuring with above-mentioned Equations of The Second Kind, its advantage is:
1. can be used for some special test analysis, as phi scanning, rocking curve, pole figure tests, In-Plane Measurement and analysis, small angle scattering analysis etc.;
2., for the sample containing fluorescent element, the peak back of the body of test is than improving decades of times;
3. purchase and reduce with maintenance cost;
X-ray diffractometer uses this technical scheme of SDD detector, and compared with configuring with above-mentioned 3rd class, its advantage is:
1. test intensity suitable, but a large amount of electric power can be saved, be conducive to energy-conserving and environment-protective;
2. acquisition cost significantly reduces;
X-ray diffractometer uses this technical scheme of SDD detector, and compared with configuring with above-mentioned 4th class, its advantage is:
1., although the intensity of test is lower, can be used for some special test analysis, as phi scanning, rocking curve, pole figure tests, In-Plane Measurement and analysis, small angle scattering analysis etc.;
2., for the sample containing fluorescent element, the peak back of the body of test is than increasing substantially;
3. purchase and significantly reduce with maintenance cost;
In addition, SDD detector can also use CuK-beta to carry out diffraction analysis, and this is that above-mentioned four kinds of configurations all cannot.So X-ray diffractometer uses SDD detector, be a kind of Full Featured technical scheme, and compared with some configures, efficiency is strong, and cost is low.
It should be noted that, the useful detection area of SDD detector used herein can not be too little, generally should be greater than 150mm 2or the yardstick of Received signal strength on certain direction is greater than 13mm.In early days due to the restriction of various technical reason, the useful area of SDD detector is too small, makes the angular instrument axial dimension of Received signal strength too small, causes the diffracted intensity of record too low.Over the past two years, the manufacturer of SDD detector, when ensureing not reduce energy resolution and the counting rate range of linearity, constantly releasing large-area SDD detector, and making SDD detector the application on X-ray diffractometer can become possibility.
Fig. 3 is the CuK-alpha ray multiple tracks energy spectrogram with SDD detector test Si powder sample, and the energy resolution of this detector very well (~ 180eV) as we can see from the figure, and can't see the ray of CuK-beta completely.
SDD detector system is arranged on an import diffractometer by Fig. 4, tests Si powder sample.As we can see from the figure, because the energy resolution of this detector is fine, so take measurement of an angle in scope whole, CuK-beta is removed completely.Wherein, the peak height of 28 degree of diffraction peaks of Si is 42865cps, and the background intensity at 23 degree of places is 132cps, calculates the peak back of the body than being 325.
In Fig. 5, a is the diffracting spectrum installing SDD detector test Si powder sample on an import diffractometer; And b is the diffracting spectrum that scintillation detector (without graphite monochromator) (comprises voltage, electric current, slit etc.) and test identical Si powder sample under identical experiment condition in Fig. 5.As we can see from the figure, the background of the diffracting spectrum that SDD detector records, especially low-angle background obviously reduces.And the intensity that the intensity of each diffraction peak recorded with SDD detector and scintillation detector (without graphite monochromator) are tested, roughly the same.For the ease of observing, the view mode of this group correlation data being changed into three dimensional constitution, can be clearly seen that the intensity contrast of these two kinds of detector tests.
It should be noted that, the diffractometer of nearly all installation flicker (or direct ratio) detector all must install graphite monochromator, then its intensity is intensity ~ 1/4 of Fig. 5, then use the intensity of SDD detector can improve 3-4 doubly than the intensity of existing configuration.
Fig. 6 is contrast experiment's test result of carrying out on domestic diffractometer, and wherein (a) is the diffracting spectrum of SDD detector test Si powder sample; B () is the diffracting spectrum that proportional detector (without graphite monochromator) (comprises voltage, electric current, slit etc.) and test identical Si powder sample under identical experiment condition; C () is the diffracting spectrum that proportional detector (comprises voltage, electric current, slit etc.) with graphite monochromator and test identical Si powder sample under identical experiment condition.As we can see from the figure, coming to the same thing shown in the test result of this experiment and Fig. 5, the intensity that the intensity of each diffraction peak namely recorded with SDD detector and proportional detector (without graphite monochromator) are tested is roughly the same.The intensity of each diffraction peak recorded with SDD detector is 3-4 times of proportional detector+graphite monochromator test intensity.Also for ease of and be convenient to observe, the view mode of this group correlation data is changed into three dimensional constitution, can be clearly seen that the intensity contrast of these two kinds of detector tests.
In Fig. 7, a installs the diffracting spectrum that Fe2O3 sample tested by scintillation detector (without graphite monochromator) on import diffractometer; In Fig. 7, b installs SDD detector, tests the diffracting spectrum of this sample under the same conditions.In Fig. 8, a installs the diffracting spectrum that Fe2O3 sample tested by proportional detector (without graphite monochromator) on domestic diffractometer; In Fig. 8, b installs SDD detector, tests the diffracting spectrum of this sample under the same conditions.It should be noted that, the ordinate of Fig. 7 and Fig. 8 is without any data processing, and the difference of the background intensity just recorded due to two kinds of detectors causes diffracting spectrum to separate up and down under same coordinate.By these two Comparative result to Fe2O3 sample test, can obviously see, SDD detector records the peak back of the body of diffracting spectrum than the raising having decades of times, shows that SDD detector can well remove the interference of fluorescence in sample.
In addition, other formation of the X-ray diffractometer X-ray detection X register system based on SDD detector of the utility model embodiment and effect are all known for a person skilled in the art, in order to reduce redundancy, do not repeat.
In the description of this instructions, specific features, structure, material or feature that the description of reference term " embodiment ", " some embodiments ", " example ", " concrete example " or " some examples " etc. means to describe in conjunction with this embodiment or example are contained at least one embodiment of the present utility model or example.In this manual, identical embodiment or example are not necessarily referred to the schematic representation of above-mentioned term.And the specific features of description, structure, material or feature can combine in an appropriate manner in any one or more embodiment or example.
Although illustrate and described embodiment of the present utility model, those having ordinary skill in the art will appreciate that: can carry out multiple change, amendment, replacement and modification to these embodiments when not departing from principle of the present utility model and aim, scope of the present utility model is by claim and equivalency thereof.

Claims (3)

1. the X-ray detection X register system of the X-ray diffractometer based on SDD detector, it is characterized in that, comprise SDD detector, single-channel analyzer, the diffracted ray that described SDD detector produces for receiving x-ray bombardment sample, described SDD detector, described single-channel analyzer connect successively, then are connected with X-ray diffractometer digital data recording system.
2. the X-ray diffractometer X-ray detection X register system based on SDD detector according to claim 1, is characterized in that, the described energy resolution of SDD detector to CuK-alpha ray is better than 200eV, can get rid of CuK-beta ray.
3. the X-ray diffractometer X-ray detection X register system based on SDD detector according to claim 1, the useful detection area of described SDD detector is greater than 150mm 2or the yardstick of Received signal strength on certain direction is greater than 13mm.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105758880A (en) * 2016-04-11 2016-07-13 西北核技术研究所 Ultra-rapid X-ray diffraction imaging method and system based on flash X-ray machine

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105758880A (en) * 2016-04-11 2016-07-13 西北核技术研究所 Ultra-rapid X-ray diffraction imaging method and system based on flash X-ray machine
CN105758880B (en) * 2016-04-11 2019-02-05 西北核技术研究所 ULTRAFAST X-RAY DIFFRACTION imaging method and system based on flashing X-ray machine

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