CN113295675A - Novel uranium isotope ratio measuring device and method thereof - Google Patents
Novel uranium isotope ratio measuring device and method thereof Download PDFInfo
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- CN113295675A CN113295675A CN202110507109.4A CN202110507109A CN113295675A CN 113295675 A CN113295675 A CN 113295675A CN 202110507109 A CN202110507109 A CN 202110507109A CN 113295675 A CN113295675 A CN 113295675A
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Abstract
The invention discloses a novel uranium isotope ratio measuring device which mainly comprises a first detection laser, a second detection laser, a beam combiner, an ablation laser, a beam splitter, a first photoelectric detector, a second photoelectric detector, a data acquisition card and an industrial personal computer; the plasma is excited by irradiating the ablation laser emitted by the ablation laser on a sample in the ablation chamber through the second reflector, the laser emitted by the first detection laser passes through the first polaroid, the laser emitted by the second detection laser sequentially passes through the first reflector and the polaroid, two beams of laser pass through the plasma after being combined by the beam combining mirror, and are split to the first photoelectric detector and the second photoelectric detector again by the beam splitting mirror, and the data acquisition card acquires signals of the first photoelectric detector and the second photoelectric detector and transmits the signals to the industrial personal computer. A novel uranium isotope ratio measuring method is also disclosed. The invention provides a technology for measuring the ratio of uranium isotopes, which is portable, rapid, high in sensitivity and non-contact.
Description
Technical Field
The invention relates to the technical field of absorption spectroscopy, in particular to a novel uranium isotope ratio measuring device and a method thereof.
Background
Uranium is the most important nuclear fuel found in nature, and three uranium isotopes (uranium isotope)238U、235U and234U)，235the content of U in natural uranium ore is only 0.711%, and less than 0.006%234U, the remainder of more than 99.2% of the uranium being238U。235U is easy to be fissile under the action of neutrons, releases huge energy through chain reaction, and in practical production and use,235u abundance may reflect the production purpose and use of the nuclear material. Uranium is a strategic resource related to national security and national civilization, and high importance is attached to the collection and storage of nuclear materials in various countries, and the periodic development of extraction, concentration and purification of refined natural uranium products from uranium ores or seawater and the storage process thereof235U/238Measurement of the U isotope ratio.
In view of the great significance of uranium materials to the field of national defense and energy, people have been researching and developing the rapid and accurate measurement235U/238Method of U isotope ratio. For example, atomic emission spectrometry (ICP-AES) using inductively coupled plasma as an atomization and ionization source, a measurement method (ICP-MS) using inductively coupled plasma and mass spectrometry in combination, Thermal Ionization Mass Spectrometry (TIMS), Laser Induced Breakdown Spectroscopy (LIBS), and the like, fission track-thermal surface ionization mass spectrometry (FT-TIMS) and Secondary Ion Mass Spectrometry (SIMS) are mainly used for high-precision analysis of uranium isotope ratios in particulate matter. The measurement methods related to mass spectrometry have high accuracy, but the measurement methods are measurement work carried out in a laboratory, have high requirements on test environment, take time for preparing samples, have long lead cycle, are difficult to transport radioactive materials, have large volume of a measurement device, expensive instruments, time-consuming use and maintenance and are professional for testersThe technical capability requirement is high, so that the technology is difficult to meet the requirements of portable, rapid, online and high-sensitivity measurement of the uranium isotope ratio at the same time.
Therefore, it is of great significance to develop a technology which is portable, rapid, high in sensitivity and capable of carrying out uranium isotope ratio measurement through remote control.
Disclosure of Invention
The invention aims to solve the technical problem of providing a novel uranium isotope ratio measuring device and a method thereof, so that the spectrum detection technology is applied to the measurement of the uranium isotope ratio, the detection precision is further improved by using a difference technology, and the device has great technical advantages and wide application prospect.
In order to solve the technical problems, the invention adopts a technical scheme that: the novel uranium isotope ratio measuring device mainly comprises a first detection laser, a second detection laser, a beam combiner, an ablation laser, a beam splitter, a first photoelectric detector, a second photoelectric detector, a data acquisition card and an industrial personal computer;
the plasma is excited by irradiating the ablation laser emitted by the ablation laser on a sample in the ablation chamber through the second reflector, the laser emitted by the first detection laser passes through the first polaroid, the laser emitted by the second detection laser sequentially passes through the first reflector and the polaroid, two beams of laser pass through the plasma after being combined by the beam combining mirror, and are split to the first photoelectric detector and the second photoelectric detector again by the beam splitting mirror, and the data acquisition card acquires signals of the first photoelectric detector and the second photoelectric detector and transmits the signals to the industrial personal computer.
In a preferred embodiment of the present invention, the ablation laser is a pulsed laser.
In a preferred embodiment of the invention, the first detection laser is measured by scanning a wavelength in the range 394.4850-394.4950 nm235U and238u atoms absorb the signal and the second detection laser measures the background noise signal at 394.5000nm by scanning a fixed wavelength.
In a preferred embodiment of the present invention, the laser beams emitted by the first detection laser and the second detection laser form vertically polarized light through the first polarizer, the first mirror and the second polarizer, respectively.
In a preferred embodiment of the present invention, the laser beam combined by the beam combiner is input to the ablation chamber after the beam quality optimization is performed on the laser beam by the spatial filter.
Furthermore, the air inlet end of the ablation chamber is connected with a pressure controller, buffer gas is filled in the ablation chamber, and the air outlet end of the ablation chamber is connected with a vacuum pump to maintain a pressure environment of 10 Kpa.
Furthermore, a three-axis displacement platform is arranged at the lower part of the ablation chamber and connected with an industrial personal computer, so that the spatial position of the ablation chamber is controllable, and laser horizontally penetrates through plasma.
In order to solve the technical problem, the invention adopts another technical scheme that: the novel uranium isotope ratio measuring method comprises the following steps:
s1: by utilizing the novel uranium isotope ratio measuring device, a standard uranium isotope ratio sample is obtained through the beer Lambert law235U and238a U absorption signal spectrum and a background noise absorption signal spectrum;
s2: by using a difference method, will235U and238subtracting the spectrum of the background noise signal from the spectrum of the U absorption signal to obtain the spectrum without the background noise235U and238u absorbs the signal spectrum;
s3: obtained according to step S2235U and238determining a standard sample by combining the absorption signal spectrum of U and the beer Lambert law235U content and corresponding absorption strength;
s4: repeating the steps, measuring multiple groups of known uranium isotope ratio standard samples, and obtaining multiple groups of data235Determining a uranium isotope ratio calibration curve by the U content and the corresponding absorption intensity;
s5: utilizing novel uranium isotope ratio measuring device repeats steps S1-S3, measures unknown isotope ratio sample, obtains the sample that awaits measuring235The absorption strength of U;
s6: the sample to be tested obtained in the step S5235The absorption intensity of U and that obtained in step S4And comparing the uranium isotope ratio calibration curves to obtain the isotope ratio of the sample to be detected.
The invention has the beneficial effects that:
(1) the invention can carry out the isotope ratio measurement on site without sample preparation or only a small amount of samples, and has the characteristics of portability, rapidness, high sensitivity and capability of carrying out the isotope ratio measurement through remote control;
(2) the invention provides a pair of235U/238The U isotope ratio realizes a portable, rapid and online analysis technology with high detection sensitivity, so that the spectrum detection technology is applied to the measurement of the uranium isotope ratio, the detection precision is further improved by using a differential technology, and the method has great technical advantages and wide application prospect.
Drawings
FIG. 1 is a schematic structural diagram of a preferred embodiment of the novel uranium isotope ratio measuring device of the present invention;
FIG. 2 is a flow chart of the novel uranium isotope ratio measurement method;
figure 3 is a schematic diagram of a calibration curve for the novel uranium isotope ratio measurement.
The parts in the drawings are numbered as follows: 1. the device comprises a first detection laser, a second detection laser, a first ablation laser, a second ablation laser, a first polaroid, a second polaroid, a beam combiner, a beam splitter, a spatial filter, a 9 ablation chamber, a third-axis displacement platform, a first photoelectric detector, a second photoelectric detector, a third photoelectric detector, a fourth photoelectric detector, a fifth photoelectric detector, a sixth photoelectric detector, a fifth photoelectric detector, a sixth photoelectric detector, a fourth photoelectric detector, a fifth photoelectric detector, a sixth photoelectric detector, a fourth photoelectric detector, a fifth photoelectric detector, a sixth photoelectric detector, a data acquisition card, a fourth photoelectric detector, a sixth photoelectric detector, a fourth photoelectric detector, a sixth photoelectric detector, a data acquisition card, a 16, an industrial personal computer, a 17, a pressure controller, a 18 and a vacuum pump.
Detailed Description
The following detailed description of the preferred embodiments of the present invention, taken in conjunction with the accompanying drawings, will make the advantages and features of the invention easier to understand by those skilled in the art, and thus will clearly and clearly define the scope of the invention.
Referring to fig. 1, an embodiment of the present invention includes:
a novel uranium isotope ratio measuring device mainly comprises a first detection laser 1, a second detection laser 2, a beam combining mirror 6, a first polaroid 4, a second polaroid 5, a first reflector 13, an ablation laser 3, a second reflector 14, a beam splitter 7, a first photoelectric detector 11, a second photoelectric detector 12, a data acquisition card 15 and an industrial personal computer 16. The ablation laser emitted by the ablation laser 3 irradiates a sample in the ablation chamber 9 through a second reflecting mirror 14 to excite plasma, the laser emitted by a first detection laser 1 passes through a first polaroid 4, the laser emitted by a second detection laser 2 sequentially passes through a first reflecting mirror 13 and a second polaroid 5, two beams of laser pass through the plasma after being combined by a beam combining mirror 6 and then are split to a first photoelectric detector 11 and a second photoelectric detector 12 again by a beam splitting mirror 7, and a data acquisition card 15 acquires signals of the first photoelectric detector 11 and the second photoelectric detector 12 and transmits the signals to an industrial personal computer.
Preferably, the ablation laser 3 is a 1064nm high-energy pulse laser, the pulse frequency is set to 5 or 10Hz, the energy is set to 50mJ, and the energy density is about 4J/cm2. The first detection laser 1 measures by scanning the wavelength in the range of 394.4850-394.4950 nm235U and238u atoms absorb the signal and the second detection laser 2 measures the background noise signal by scanning a fixed wavelength at 394.5000 nm.
Further, a spatial filter 8 is connected between the beam combiner 6 and the ablation chamber 9, and the laser beam combined by the beam combiner 6 is input to the ablation chamber 9 after being subjected to beam quality optimization through the spatial filter 8.
Furthermore, the air inlet end of the ablation chamber 9 is connected with a pressure controller 17, helium with high ionization potential energy is filled as buffer gas to slow down the expansion speed of the plasma, and nitrogen, argon and the like can be filled as buffer gas; the air outlet end of the ablation chamber 9 is connected with a vacuum pump 18, and the pressure environment of 10Kpa is maintained. The lower part of the ablation chamber 9 is also provided with a three-axis displacement platform 10, and the three-axis displacement platform 10 is connected with an industrial personal computer 16, so that the spatial position of the ablation chamber 9 can be controlled, and laser horizontally penetrates through plasma.
Preferably, the data acquisition card 15 is connected to the industrial personal computer 16, and acquires signals at a high sampling rate of 10 MHz.
The optical path principle of the measuring device is as follows: the working current and temperature of the first detection laser 1 and the second detection laser 2 are set, so that the wavelength of the first detection laser 1 is scanned within 394.4850-394.4950 nm, and the wavelength of the second detection laser 2 is fixed at 394.5000nm where no uranium atoms are absorbed. The laser of the first detection laser 1 passes through the first polaroid 4, the laser of the second detection laser 2 passes through the second polaroid 5 after being emitted by the first reflector 13, two beams of laser form vertical polarized light, laser beam combination is carried out by using the beam combining mirror 6 with high transmittance and high reflectivity for the polarized light, the combined laser is subjected to plasma excited by the laser 3 through ablation, and then is re-divided into two beams of detection laser by the beam splitting mirror 7, the laser emitted by the first detection laser 1 is input into the first photoelectric detector 11, the laser emitted by the second detection laser 2 is input into the second photoelectric detector 12, the data acquisition card 15 acquires signals of the first photoelectric detector 11 and the second photoelectric detector 12 and inputs the signals into the industrial personal computer 16, and the industrial personal computer 16 carries out concentration inversion on the spectral signals acquired by the data acquisition card 15, so that the isotope ratio of uranium can be acquired.
Referring to fig. 2, an embodiment of the present invention further provides a novel uranium isotope ratio measurement method, including the following steps:
s1: by utilizing the novel uranium isotope ratio measuring device, a standard uranium isotope ratio sample is obtained through the beer Lambert law235U and238a U absorption signal spectrum and a background noise absorption signal spectrum;
s2: by using a difference method, will235U and238subtracting the spectrum of the background noise signal from the spectrum of the U absorption signal to obtain the spectrum without the background noise235U and238u absorbs the signal spectrum;
s3: obtained according to step S2235U and238determining a standard sample by combining the absorption signal spectrum of U and the beer Lambert law235U content and corresponding absorption strength;
s4: repeating the steps, measuring multiple groups of known uranium isotope ratio standard samples, and obtaining multiple groups of data235The U content and the corresponding absorption intensity determine the calibration curve for the uranium isotope ratio, as shown in figure 3,235the U content and the absorption strength have good linearity;
s5: utilizing novel uranium isotope ratio measuring device repeats steps S1-S3, measures unknown isotope ratio sample, obtains the sample that awaits measuring235The absorption strength of U;
s6: the sample to be tested obtained in the step S5235And comparing the absorption intensity of the U with the uranium isotope ratio calibration curve obtained in the step S4 to obtain the isotope ratio of the sample to be detected.
The principle of the uranium isotope ratio measuring method is as follows:
the basic principle of the spectral detection of trace components is the Beer-Lambert (Beer-Lambert) absorption law. During measurement, laser passes through a sample to be measured, and the absorption of a specific component on a given absorption path is measured. The exit light intensity It (v) of the direct absorption spectrum is expressed by Beer-Lambert's law as:
It(v)＝I0(v)e-α(v)L (1)
wherein ν is the frequency of the laser, α (v) is the absorption coefficient of the sample gas, which is used to characterize the absorption of a certain gaseous substance to the light with a certain wavelength, and the above formula can also be expressed as:
n is per cm3The atomic number of the absorbing atoms in the gas volume, σ (v) is the absorption cross section, S is the spectral line absorption intensity,
is a normalized spectral absorption profile. Since the gas absorbs the light, the intensity of the emergent light is changed into It(v), recording I with a highly sensitive detector0(v) and ItAnd (v) obtaining the absorption spectrum of the gas to be measured by the formula (2) according to the light intensity change of the wavelength within the range of 394.4850-394.4950 nm.
From the above, the sample with known standard abundance can be scanned235U/238The U absorption line obtains the spectrum C1, fixed235U/238U no uranium atom absorption line a background noise spectrum C2 was obtained, the spectrum of the non-absorption (no uranium atom absorption) line was subtracted from the spectrum of the absorption line scan:
C3＝C1-C2 (3)
and determining a linear calibration curve by the absorption spectral lines of a plurality of groups of standard abundance samples, and determining the abundance of the current sample by the calibration curve and the absorption spectral lines of the unknown abundance samples.
The invention can carry out the isotope ratio measurement on site without sample preparation or only a small amount of samples, and has the characteristics of portability, rapidness, high sensitivity and capability of carrying out the isotope ratio measurement through remote control.
The invention provides a pair of235U/238The U isotope ratio realizes a portable, rapid and online analysis technology with high detection sensitivity, so that the spectrum detection technology is applied to the measurement of the uranium isotope ratio, the detection precision is further improved by using a differential technology, and the method has great technical advantages and wide application prospect.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes performed by the present specification and drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (8)
1. A novel uranium isotope ratio measuring device is characterized by mainly comprising a first detection laser, a second detection laser, a beam combiner, an ablation laser, a beam splitter, a first photoelectric detector, a second photoelectric detector, a data acquisition card and an industrial personal computer;
the plasma is excited by irradiating the ablation laser emitted by the ablation laser on a sample in the ablation chamber through the second reflector, the laser emitted by the first detection laser passes through the first polaroid, the laser emitted by the second detection laser sequentially passes through the first reflector and the polaroid, two beams of laser pass through the plasma after being combined by the beam combining mirror, and are split to the first photoelectric detector and the second photoelectric detector again by the beam splitting mirror, and the data acquisition card acquires signals of the first photoelectric detector and the second photoelectric detector and transmits the signals to the industrial personal computer.
2. A novel uranium isotope ratio measuring device according to claim 1, wherein the ablation laser is a pulsed laser.
3. A novel uranium isotope ratio measuring apparatus according to claim 1, wherein the first probe laser measures by scanning a wavelength in a range of 394.4850-394.4950 nm235U and238u atoms absorb the signal and the second detection laser measures the background noise signal at 394.5000nm by scanning a fixed wavelength.
4. A novel uranium isotope ratio measuring device according to claim 1, wherein the laser light emitted by the first detection laser and the laser light emitted by the second detection laser form vertically polarized light by a first polarizing plate, a first reflecting mirror and a second polarizing plate, respectively.
5. A novel uranium isotope ratio measuring device according to claim 1, wherein the laser beam combined by the beam combining mirror is subjected to beam quality optimization by a spatial filter and then input to an ablation chamber.
6. A novel uranium isotope ratio measuring device according to claim 1 or 5, wherein the gas inlet end of the ablation chamber is connected with a pressure controller, buffer gas is injected, and the gas outlet end of the ablation chamber is connected with a vacuum pump, so as to maintain a pressure environment of 10 Kpa.
7. A novel uranium isotope ratio measuring device according to claim 1 or 5, wherein a triaxial displacement platform is arranged at the lower part of the ablation chamber and is connected with an industrial personal computer, so that the spatial position of the ablation chamber can be controlled, and laser can horizontally pass through plasma.
8. A novel uranium isotope ratio measuring method is characterized by comprising the following steps:
s1: by utilizing the novel uranium isotope ratio measuring device, a standard uranium isotope ratio sample is obtained through the beer Lambert law235U and238a U absorption signal spectrum and a background noise absorption signal spectrum;
s2: by using a difference method, will235U and238subtracting the spectrum of the background noise signal from the spectrum of the U absorption signal to obtain the spectrum without the background noise235U and238u absorbs the signal spectrum;
s3: obtained according to step S2235U and238determining a standard sample by combining the absorption signal spectrum of U and the beer Lambert law235U content and corresponding absorption strength;
s4: repeating the steps, measuring multiple groups of known uranium isotope ratio standard samples, and obtaining multiple groups of data235Determining a uranium isotope ratio calibration curve by the U content and the corresponding absorption intensity;
s5: utilizing novel uranium isotope ratio measuring device repeats steps S1-S3, measures unknown isotope ratio sample, obtains the sample that awaits measuring235The absorption strength of U;
s6: the sample to be tested obtained in the step S5235And comparing the absorption intensity of the U with the uranium isotope ratio calibration curve obtained in the step S4 to obtain the isotope ratio of the sample to be detected.
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