CN109632854B - Massive uranium ore multi-element online X fluorescence analyzer with double detection structures - Google Patents

Massive uranium ore multi-element online X fluorescence analyzer with double detection structures Download PDF

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CN109632854B
CN109632854B CN201910031401.6A CN201910031401A CN109632854B CN 109632854 B CN109632854 B CN 109632854B CN 201910031401 A CN201910031401 A CN 201910031401A CN 109632854 B CN109632854 B CN 109632854B
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detection
uranium ore
uranium
fluorescence
detector
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CN109632854A (en
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张焱
汤彬
王仁波
张雄杰
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East China Institute of Technology
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating 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
    • G01N23/22Investigating 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 measuring secondary emission from the material
    • G01N23/223Investigating 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 measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence

Abstract

The invention relates to a massive uranium ore multi-element online X-ray fluorescence analyzer with a double-detection structure, which consists of an excitation light source, a double-detection analysis device, a conveying belt and auxiliary equipment, wherein the excitation light source comprises a high-power X-ray tube, a collimator arranged at the outlet of the X-ray tube and X-ray tube high pressure; x rays emitted by an excitation light source vertically irradiate the massive uranium ore samples on the conveyor belt, and multi-element characteristic X fluorescence information of different positions in the massive uranium ore samples is excited and then received by double detection devices with different detection structures. Through the coupling model of two detection structures, can overcome the influence of geometric effect that cubic uranium ore surface unevenness brought to online X fluorescence analysis appearance analysis result degree of accuracy, improve online X fluorescence analysis appearance analysis degree of accuracy, easy operation measures fast, and the precision is high, safety ring protects.

Description

Massive uranium ore multi-element online X fluorescence analyzer with double detection structures
The technical field is as follows:
the invention relates to a massive uranium ore multi-element online X-ray fluorescence analyzer with a double-detection structure, in particular to an online X-ray fluorescence analyzer for analyzing the multi-element content in a massive sample, and belongs to the field of rapid uranium ore element analysis.
Background art:
uranium ore is a strategic resource in China, and the rapid online measurement of the uranium ore taste is particularly important. However, most of the current methods are based on chemical analysis methods, and generally, a sample needs to be burnt at a high temperature and then reacted with a chemical reagent to calculate the uranium ore content. This chemical analysis method requires a long measurement time due to the strict sample preparation process, and causes serious environmental pollution and damage to the health of users due to the use of chemical reagents.
The XRF (X-ray Fluorescence, XRF) analysis technology has wide application prospect in the aspect of realizing real-time on-line measurement of uranium ores due to the advantages of real-time on-line, convenience, rapidness, nondestructive measurement and the like. In laboratory XRF analysis, interference caused by a sample itself is usually eliminated through different sample preparation methods (such as tabletting, melting, digestion, and the like), but an online XRF analysis technology is a direct measurement for an unknown sample on site, and a sample preparation process is not available, so that interference factors for the accuracy of the online XRF analysis technology mainly come from the sample itself, such as surface unevenness (geometric effect) with different shapes and sizes, complex sample components, and the like. Meanwhile, in order to improve the accuracy of the on-line measurement of the bulk material XRF, the above interference factors must be corrected. In laboratory analysis, the influence can be eliminated by a specific sample preparation method such as melting, digestion and the like, but in online XRF analysis, a sample preparation process is not available, so that the measurement accuracy of an online XRF analysis technology is improved and the problem of geometric effect is not moderate aiming at massive materials.
Therefore, there is a need to improve the prior art to overcome the deficiencies of the prior art.
The invention content is as follows:
the invention provides a massive uranium ore multi-element online X fluorescence analyzer with a double detection structure, which has the advantages of no chemical pollution, no radioactive pollution, short measurement time, high precision, simple structure, safety and reliability.
The invention adopts the following technical scheme: the utility model provides a two blocky uranium ore multielement on-line X fluorescence analysis appearance of surveying structure, this analysis appearance includes excitation light source, two detection analytical equipment, transmission band, auxiliary assembly, the excitation light source includes X fluorescent tube, X fluorescent tube high pressure, and auxiliary assembly includes ship type sled scraper blade and laser range finder, and the fixed top of establishing at the transmission band of ship type sled scraper blade is established in one side of ship type sled scraper blade to the laser range finder, and X fluorescent tube high pressure are established on ship type sled scraper blade, two detection analytical equipment include two detection systems: the system comprises a reflection type detection system and a transmission type detection system, wherein the reflection type detection system comprises a silicon drift detector, a detector high voltage, a charge sensitive preamplifier connected with the silicon drift detector, a pulse forming amplifier connected with the charge sensitive preamplifier and a digital multichannel spectrometer connected with the pulse forming amplifier, and the silicon drift detector is arranged on one side of an X light pipe; the transmission type detection system comprises a cadmium telluride detector, a detector high voltage, a charge sensitive preamplifier connected with the cadmium telluride detector, a pulse forming amplifier connected with the charge sensitive preamplifier and a digital multichannel spectrometer connected with the pulse forming amplifier, wherein the cadmium telluride detector is arranged below a transmission belt; the energy spectrum information collected by the double detection systems is converted into an energy spectrum for analysis, and data processing control is carried out by a computer; the conveying belt is used for conveying blocky uranium ore samples on line; the big cubic uranium ore sample of ship type sled scraper blade adoption physics gravity principle flattening, the laser range finder assists and judges cubic uranium ore geometric variation, provides the judgement basis for different detection systems.
The method comprises the steps that a reflection type detection system and a transmission type detection system are adopted, a laser range finder is adopted for auxiliary judgment of geometric change of the bulk uranium ores, reflection type measurement is adopted when the geometric change of the bulk uranium ores is within 20mm, when X rays emitted by an X-ray tube irradiate on a bulk uranium ore sample, characteristic X fluorescence information of the uranium ores is excited, the fluorescence information is received by a silicon drift detector, and the fluorescence information is converted into an energy spectrum for analysis by a digital multichannel spectrometer after being formed and amplified by a charge sensitive preamplifier and a pulse forming amplifier; when the geometric variation range of the massive uranium ores is 20 mm-100 mm, the transmission type uranium ores play a role, when X rays emitted by an X-ray tube irradiate on a massive uranium ore sample, the characteristic X fluorescence information of the uranium ores is excited, the fluorescence information is received by a cadmium telluride detector, and the fluorescence information is converted into an energy spectrum for analysis by a digital multichannel spectrometer after being shaped and amplified by a charge sensitive preamplifier and a pulse shaping amplifier; the computer establishes a coupling model of a double detection structure by analyzing the distance information of the laser range finder and utilizing the detection response of different detectors to X fluorescence and the penetration capability of characteristic X fluorescence information with different energy, overcomes the influence of geometric effect caused by uneven surface of massive uranium ores on the characteristic X fluorescence intensity of multiple elements in a sample, and improves the analysis accuracy of the online X fluorescence analyzer.
The beryllium window of the silicon drift detector is 0.4 mm, and the detection range is 1-30keV.
The beryllium window of the cadmium telluride detector is 0.5 mm, and the detection range is 20-100keV.
The laser range finder has the range of 0-100 mm and the precision of 0.07mm, is fixed on a ship-shaped ski scraper to assist in judging geometric changes of the massive uranium ores, and provides judgment basis for different detection systems.
The high voltage of the X-ray tube is 80000V.
The distance between the silicon drift detector and the massive uranium ore sample is 6 millimeters, and the included angle is 90 degrees.
The distance between the cadmium telluride detector and the massive uranium ore sample is 5 millimeters, and the included angle is 90 degrees.
The boat-shaped ski scraper is a steel plate with the thickness of 5mm, and the weight of the boat-shaped ski scraper is more than or equal to 100kg.
The thickness of the conveying belt is 5mm.
The invention has the following beneficial effects: compared with the existing X fluorescent equipment, the X fluorescent equipment adopts the high-power X light tube as an excitation light source, and does not generate chemical pollution and radioactive pollution; compared with the existing X fluorescence equipment, the double detection system is adopted to overcome the influence of the geometric effect caused by uneven surface of the massive uranium ore on the multi-element characteristic X fluorescence intensity of the sample, and the analysis accuracy of the online X fluorescence analyzer is improved; because the prior advanced silicon drift and cadmium telluride detector and a multi-channel analyzer are adopted, the precision is high, the measurement range is wider, the human error is small, and the labor intensity of an operator is low; the laser range finder is adopted to monitor the change degree of the surface of the sample in real time, and the analysis accuracy of the on-line X fluorescence analyzer is improved; the invention does not need the sample preparation process, and can directly measure on line, with high speed and accurate result.
Description of the drawings:
FIG. l is a diagram illustrating the working principle of the present invention.
FIG. 2 is a spectrum of a silicon drift detection system according to the present invention.
FIG. 3 is a cadmium telluride detector system energy spectrum of the present invention.
Wherein:
1-X light pipe; 2-light pipe high pressure; a 3-silicon drift detector; 4-high detector voltage; 5-a charge sensitive preamplifier; 6-pulse shaping amplifier; 7-a cadmium telluride detector; 8-high voltage of the detector; 9-a charge sensitive preamplifier; 10-a pulse shaping amplifier; 11-digital multichannel spectrometer; 12-a laser rangefinder; 13-conveying belt; a uranium ore sample; 15-boat ski blades; 16-a computer.
The specific implementation mode is as follows:
referring to fig. 1 to 3, a bulk uranium ore multi-element online X fluorescence analyzer with a dual detection structure includes an excitation light source, a dual detection analysis device, a conveyor belt, and an auxiliary device, where the excitation light source includes an X light pipe and an X light pipe high voltage; the double detection analysis device comprises two detection systems (a reflection type and a transmission type), wherein the reflection type detection system is arranged on a silicon drift detector on the right side of an X-ray tube, a detector high voltage, a charge sensitive preamplifier connected with the silicon drift detector, a pulse forming amplifier connected with the charge sensitive preamplifier and a digital multichannel spectrometer connected with the pulse forming amplifier; the conveying belt is mainly used for conveying blocky uranium ore samples on line; the auxiliary assembly includes ship type sled scraper blade and laser range finder, and ship type sled scraper blade is used for fixed online X fluorescence analysis appearance and adopts the physics gravity principle to flatten great cubic uranium ore sample, and laser range finder assists and judges cubic uranium ore geometric variation, provides the judgement foundation for different detection systems.
The method comprises the steps that a double detection structure (a reflection type and a transmission type) is provided, a laser range finder is adopted for auxiliary judgment of geometric change of the bulk uranium ores, reflection type measurement is adopted when the geometric change of the bulk uranium ores is within 20mm, when X rays emitted by an X-ray tube irradiate on a bulk uranium ore sample, characteristic X fluorescence information of the uranium ores is excited, the fluorescence information is received by a silicon drift detector, and the fluorescence information is converted into an energy spectrum for analysis by a digital multichannel spectrometer after being formed and amplified by a charge sensitive preamplifier and a pulse forming amplifier; when the geometric variation range of the massive uranium ores is 20 mm-100 mm, the transmission type uranium ores play a main role, when X rays emitted by an X-ray tube irradiate on a massive uranium ore sample, characteristic X fluorescence information of the uranium ores is excited, the fluorescence information is received by a cadmium telluride detector, and the fluorescence information is converted into an energy spectrum for analysis by a digital multichannel spectrometer after being formed and amplified by a charge sensitive preamplifier and a pulse forming amplifier; the computer establishes a coupling model of a double detection structure by analyzing the distance information of the laser range finder and utilizing the detection response of different detectors to X fluorescence and the penetration capability of characteristic X fluorescence information with different energy, overcomes the influence of geometric effect caused by uneven surface of massive uranium ores on the characteristic X fluorescence intensity of multiple elements in a sample, and improves the analysis accuracy of the online X fluorescence analyzer.
The working principle of the massive uranium ore multi-element online X fluorescence analyzer with the double detection structure is as follows: the method comprises the steps that a double detection structure (a reflection type and a transmission type) is provided, a laser range finder is adopted for auxiliary judgment of geometric change of the bulk uranium ores, reflection type measurement is adopted when the geometric change of the bulk uranium ores is within 20mm, when X rays emitted by an X-ray tube irradiate on a bulk uranium ore sample, characteristic X fluorescence information of the uranium ores is excited, the fluorescence information is received by a silicon drift detector, and the fluorescence information is converted into an energy spectrum for analysis by a digital multichannel spectrometer after being formed and amplified by a charge sensitive preamplifier and a pulse forming amplifier; when the geometric variation range of the massive uranium ores is 20 mm-100 mm, the transmission type uranium ores play a main role, when X rays emitted by an X-ray tube irradiate on a massive uranium ore sample, characteristic X fluorescence information of the uranium ores is excited, the fluorescence information is received by a cadmium telluride detector, and the fluorescence information is converted into an energy spectrum for analysis by a digital multichannel spectrometer after being formed and amplified by a charge sensitive preamplifier and a pulse forming amplifier; the computer establishes a coupling model of a double detection structure by analyzing the distance information of the laser range finder and utilizing the detection response of different detectors to X fluorescence and the penetration capability of characteristic X fluorescence information with different energy, overcomes the influence of geometric effect caused by uneven surface of massive uranium ores on the characteristic X fluorescence intensity of multiple elements in a sample, and improves the analysis accuracy of the online X fluorescence analyzer.
Example 1:
1. the high voltage 2 of a silver target X light pipe 1,X light pipe of the Dandong east electron tube factory is set to be 80000V, so that the characteristic X-ray fluorescence of multiple elements in uranium ores can be effectively excited; the distance between the X-ray tube l and the surface of the sample 14 is 50 mm.
2. The SDD-123 silicon drift detector 3 of amptek company in USA is adopted to form an included angle of 90 degrees and a distance of 6 mm with the surface of the sample, and the included angle and the distance are used for ensuring that the analyzer obtains better resolution.
3. The cadmium telluride detector 7 from amptek, usa is used at an angle of 90 degrees and a distance of 6 mm from the sample surface, which are used to ensure good resolution of the analyzer.
4. An excitation light source, a detection system and a digital multichannel spectrometer 11 are fixed on a 5mm ship-shaped sled scraper, and a large bulk uranium ore sample is flattened by adopting the physical gravity principle.
5. The laser light source is LOD infrared laser of Shanghai Beile. The laser light source emits infrared light, the infrared light irradiates on the sample platform, and the surface change data of the sample are monitored in real time.
6. A 10kg uranium ore sample was prepared and measured for 100s.
7. The signal collected by the silicon drift detector 3 is amplified by the pulse shaping amplifier 6, then converted into an energy spectrum (as shown in fig. 2) for analysis by the digital multichannel spectrometer 11, and then processed by a computer to obtain the content of the low atomic number elements in the uranium mine.
8. Signals collected by the cadmium telluride detector 7 are amplified by the pulse shaping amplifier 6, then are converted into an energy spectrum diagram (as shown in fig. 3) which can be used for analysis through the digital multichannel spectrometer 11, and then data processing is carried out through a computer to obtain the content of the high atomic number elements in the uranium mine.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications can be made without departing from the principle of the present invention, and these modifications should also be regarded as the protection scope of the present invention.

Claims (9)

1. The utility model provides a cubic uranium ore multielement on-line X fluorescence analysis appearance of two detection structures which characterized in that: this analysis appearance includes excitation light source, two detection analytical equipment, transmission band (13), auxiliary assembly, the excitation light source includes X light pipe (1), X light pipe high pressure (2), and auxiliary assembly includes ship type sled scraper blade (15) and laser range finder (12), and the fixed top of establishing in transmission band (13) of ship type sled scraper blade (15) is established in one side of ship type sled scraper blade (15) in laser range finder (12), and X light pipe (1) and X light pipe high pressure (2) are established on ship type sled scraper blade, two detection analytical equipment include two detection systems: the device comprises a reflective detection system and a transmissive detection system, wherein the reflective detection system comprises a silicon drift detector (3), a detector high voltage (4), a charge sensitive preamplifier (5) connected with the silicon drift detector (3), a pulse forming amplifier (6) connected with the charge sensitive preamplifier (5) and a digital multichannel spectrometer (11) connected with the pulse forming amplifier (6), and the silicon drift detector (3) is arranged on one side of an X light pipe (1); the transmission type detection system comprises a cadmium telluride detector (7), a detector high voltage (8), a charge sensitive preamplifier (9) connected with the cadmium telluride detector (7), a pulse shaping amplifier (10) connected with the charge sensitive preamplifier (9) and a digital multichannel spectrometer (11) connected with the pulse shaping amplifier (10), wherein the cadmium telluride detector (7) is arranged below a conveying belt (13); the energy spectrum information collected by the double detection systems is converted into an energy spectrum for analysis and is subjected to data processing control by a computer (16); the conveying belt (13) is used for conveying blocky uranium ore samples (14) on line; the ship-shaped sled scraper (15) flattens large blocky uranium ore samples (14) by adopting a physical gravity principle, and the laser range finder is used for assisting in judging geometric changes of blocky uranium ores and providing judgment bases for different detection systems; the method comprises the steps that a reflection type detection system and a transmission type detection system are adopted, a laser range finder (12) is adopted to assist in judging geometric change of a blocky uranium ore (14), reflection type measurement is adopted when the geometric change of the blocky uranium ore is within 20mm, when X-rays emitted by an X-ray tube irradiate on a blocky uranium ore sample, characteristic X fluorescence information of the uranium ore is excited, the fluorescence information is received by a silicon drift detector (3), and the fluorescence information is converted into an energy spectrum for analysis through a digital multichannel spectrometer (11) after being subjected to forming amplification by a charge sensitive preamplifier (5) and a pulse forming amplifier (6); when the geometric change range of the lumpy uranium ore is 20 mm-100 mm, the transmission type uranium ore plays a role, when X rays emitted by an X-ray tube irradiate on a lumpy uranium ore sample, the characteristic X fluorescence information of the uranium ore is excited, the fluorescence information is received by a cadmium telluride detector (7), and is converted into an energy spectrum for analysis by a digital multichannel spectrometer (11) after being shaped and amplified by a charge sensitive preamplifier (9) and a pulse shaping amplifier (10); the computer (16) establishes a coupling model of a double detection structure by analyzing the distance information of the laser range finder and utilizing the detection response of different detectors to X fluorescence and the penetration capability of characteristic X fluorescence information with different energy, overcomes the influence of geometric effect caused by uneven surface of the massive uranium ore on the characteristic X fluorescence intensity of multiple elements in the sample, and improves the analysis accuracy of the online X fluorescence analyzer.
2. The multi-element online X-ray fluorescence analyzer for bulk uranium ores with dual detection structures according to claim 1, wherein: the beryllium window of the silicon drift detector (3) is 0.4 mm, and the detection range is 1-30keV.
3. The multi-element online X-ray fluorescence analyzer for bulk uranium ores with dual detection structures according to claim 1, wherein: the beryllium window of the cadmium telluride detector (7) is 0.5 mm, and the detection range is 20-100keV.
4. The multi-element online X-ray fluorescence analyzer for bulk uranium ores with dual detection structures according to claim 1, wherein: the laser range finder (12) range is 0-100 mm, and the precision is 0.07mm, fixes on ship type sled scraper (15) and carries out the supplementary cubic uranium ore geometric variation that judges, provides the basis of judging for different detecting systems.
5. The multi-element online X-ray fluorescence analyzer for bulk uranium ores with dual detection structures according to claim 1, wherein: the high voltage of the X-ray tube (1) is 80000V.
6. The multi-element online X-ray fluorescence analyzer for bulk uranium ores with dual detection structures, according to claim 2, wherein: the distance between the silicon drift detector (3) and the massive uranium ore sample (14) is 6 millimeters, and the included angle is 90 degrees.
7. The multi-element online X-ray fluorescence analyzer for bulk uranium ores with dual detection structures, according to claim 3, wherein: the distance between the cadmium telluride detector (7) and the massive uranium ore sample (14) is 5mm, and the included angle is 90 degrees.
8. The multi-element online X-ray fluorescence analyzer for bulk uranium ores with dual detection structures according to claim 4, wherein: the boat-shaped sled scraper (15) is made of a steel plate with the thickness of 5mm, and the weight of the boat-shaped sled scraper is more than or equal to 100kg.
9. The multi-element online X-ray fluorescence analyzer for bulk uranium ores with dual detection structures according to claim 1, wherein: the thickness of the transmission belt (13) is 5mm.
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