[보고서]조사핵연료 고체화학 특성 규명 연구

임상호

보고서 정보

주관연구기관

한국원자력연구원
Korea Atomic Energy Research Institute

연구책임자

임상호

참여연구자

한선호 , 최광순 , 하영경 , 차완식 , 박재일 , 김준혁 , 이광은 , 박정미 , 김정석 , 송규석 , 김종윤 , 배상은 , 이정묵 , 이신경 , 김종구 , 박서현

보고서유형

최종보고서

발행국가

대한민국

언어

한국어

발행년월

2018-11

과제시작연도

2018

주관부처

과학기술정보통신부
Ministry of Science and ICT

연구관리전문기관

한국연구재단
National Research Foundation of Korea

등록번호

TRKO201900019630

과제고유번호

1711064928

사업명

원자력기술개발사업(R&D)

DB 구축일자

2020-04-11

키워드

조사핵연료.국부핵종분포.고체화학.고온화학거동.계면화학거동.Irradiated fuel.Local nuclide distribution.Solid-state Chemistry.High temperature Chemical behavior.Interfacial chemical behavior.

표 (top, left and right) Overview of old ICP-MS system. (bottom, left) Disassembly of old ICP-MS system. (bottom, right) Temporary storage of old ICP system in empty space
표 Preparation of space for new HR(high resolution)-ICP-MS installation
표 Installation of 440V power supply
표 HR-ICP-MS and additional equipments transfer
표 Installation of HR-ICP-MS, glove box and DUP exhaust line
표 (left) Operation of plasma in HR-ICP-MS. (right) Plasma inside torch box seen through window indicated by arrow
표 Connection of Ar gas line and sample gas line between HR-ICP-MS and LA instrument
표 Tuning of operation condition of HR-ICP-MS
표 Comparison of sensitivity for In-115 (1 ppb) at old ICP-MS and new HR-ICP-MS
표 Optimized measurement conditions for LA instrument
표 (top) Microscope image of SRM-612 glass with laser ablated craters. (bottom) Intensity of 86Sr, 88Sr, 139La,232Th and 358U measured by LA-ICP-MS
표 (top, left) 86Sr/238U ratio, (top, right) 88Sr/238U ratio, (bottom, left) 139La/238U ratio and (bottom, right) 232Th/235U ratio measured by LA-ICP-MS (straight/dotted red lines indicate the average/standard deviation value, respectively)
표 Layout for shielded glovebox
표 Glovebox without shielding equipment
표 New layout for shielded glovebox
표 Complete installation of shielded glovebox
표 The principle of the desolvator. Sweep gas (Ar) removes solvent vapor while the analyte transport efficiency remains high
표 (left) Installation of APEX Omega HF with plasma of ICP-MS. (right) Inside of APEX Omega HF
표 Control software of APEX Omega HF
표 Optimized measurement conditions for APEX Omega HF
표 Comparison of measured intensity with and without desolvator (APEX Omega HF) for In-115 (left) and U-238 (right)
표 Comparison of measured stability for In-115 and U-238 with (left) and without desolvator (APEX Omega HF) (right)
표 Aligned laser path from Nd:YAG Inlite II to shielded LA glovebox
표 Software interface of Nd:YAG Inlite II
표 Laser ablation system in shielded LA glovebox
표 Software interface of laser ablation system and CCD image of sample
표 Laser ablation mass spectra of Th-232 and U-238 from line scans of SRM-612 with a 20μm s-1 scan rate. Certificated and experimental values of Th232/U238 are 1.045 and 1.064, respectively
표 Sample Chamber of shielded LA-ICP-MS for high-level radioactive materials including irradiated nuclear fuels
표 Specification of HTK 16N and HTK 2000N high temperature analysis system
표 (a) Shipped box and (b) part box pictures
표 (a) High temperature sample stage, (b) turbo and rotary pumps, and (c) temperature controller
표 (a) Original XRD system and (b-c) XRD system equipped with high temperature sample stage (b) with cover and (c) without cover
표 (a) Original XRD system and (b) XRD system installed with high temperature controller
표 (a) Original XRD system and (b) XRD system equipped with high temperature analysis system
표 in-situ XRD spectra obtained from MgO sample at each temperature
표 Visualization of peak intensities acquired from in-situ annealing of MgO sample
표 (a) Original XRD system and (b) XRD system after eliminating sample stage
표 Installation of HTK 2000N with chiller line, vacuum line and several connections
표 Opening of two chiller valves with proper pressure
표 Temperature controller with green light on cooling panel, indicating normal operating of chiller
표 Rotary and turbo pump controller with pressure gauge
표 Change of blank to absorber Cu 99.9 % for the protection of XRD detector during z axis alignment
표 Several setting values for starting z axis alignment
표 Method to find the optimum z axis height using z axis alignment
표 Programming with slit size, temperature and heating rate for operating of high temperature XRD
표 Programming of delay time, start 2θ and stop 2θ values at each measured temperature for operating of high temperature XRD
표 in-situ high temperature XRD results obtained from MgO sample at each temperature during heating and cooling
표 Two dimensional view of in-situ high temperature XRD spectra obtained from MgO sample at each temperature
표 Two dimensional view of in-situ high temperature XRD spectra depending on interval range (temperature per step) obtained from Zr metal sample
표 Monitoring the heating process performed in heating chamber
표 Two dimensional view of in-situ high temperature XRD spectra obtained from Zr metal sample during heating
표 Two dimensional view of in-situ high temperature XRD spectra obtained from Zr metal sample during cooling
표 Two dimensional view of in-situ high temperature XRD spectra obtained from only W heating strip during heating
표 Two dimensional view of in-situ high temperature XRD spectra obtained from only W heating strip during cooling
표 Photographs of side view on UO2 and (UNd)O2 pellets as increasing Nd(III) contents
표 XRD spectra of un-doped UO2 and doped with 10 mol% trivalent dopants on UO2-x, and/or tetravalent-dopants on UO2
표 Lattice parameters of un-doped UO2 and doped with 10 mol% trivalent-, and/or tetravalent-dopants on UO2 matrices
표 lattice parameters and contraction factors of un-doped UO2 and doped with 10 mol% trivalent-, and/or tetravalent-dopants on UO2 matrices. Also, ionic radius of dopants and U(IV, V)* are presented
표 Comparing the domain structures on the surfaces of un-doped UO2-x and UO2 matrices, and doped with trivalent-, and/or tetravalent-dopants on matrices, respectively. Magnification of all images is ×3000, and scale bars in images indicate 5 ㎛ length
표 4-point probe analytical system for measuring the electrical conductivity of un-doped-, and doped pellets with 10 mol% trivalent-, and/or tetravalent-dopants
표 Electrical conductivity of un-doped UO2 and doped with 10 mol% trivalent-, and/or tetravalent-dopants on UO2 matrices
표 Raman spectroscopy system. (left) SR500i spectrometer, (middle) microscopic Raman chmber, (right) opitcs and 633 nm He-Ne laser
표 Raman spectra of UO2, U0.9Th0.1O2, U0.9Zr0.1O2, U0.9Nd0.1O2 and U0.9Gd0.1O2 from bottom to top
표 Raman spectra of metal doped CeO2 and descriptions of oxygen vacancies and MO8-type complex [J. Phys. Chem. A 2011, 115, 7972–7977]
표 Deconvoluted Raman spectra of U0.9Nd0.1O2 (bottom) and U0.9Gd0.1O2 (top)
표 RDE (Rotating disk electrode) analytical system
표 Detachable working electrode and its design patent for RDE (Rotating disk electrode) analytical system
표 Cyclic voltammograms of UO2 in (a) 0.1 M NaClO4(aq) and (b) 0.1 M NaClO4(aq) containing 0.01 M CO32-/HCO-. The pH of both solutions are adjusted to at 9.0. Scan rate is 0.05 V/sec
표 Cyclic voltammograms of doped pellets with (a) trivalent dopants(Nd3+, Gd3+) on UO2-x and (b) tetravalent dopants (Zr4+, Th4+) on UO2 in 0.1 M NaClO4(aq) containing 0.01 M CO32-/HCO- at pH 9, respectively. Scan rate is 0.05 V/sec
표 Steady-state current density of surface oxidation (at –0.25 V) and dissolutive oxidation (at 0.20 V) on undoped- and/or doped with trivalent or tetravalent dopants on matrix, respectively
표 Optical images of (a) UO2, (b) U0.98Nd0.02O2, and (c) U0.94Nd0.06O2 pellets
표 Alumina tube furnace for the sintering of U1-yNdyO2 pellets
$Lattice parameters for UO2, U0.98Nd0.02O2, and U0.94Nd0.06O2 pellets as a function of the molar fraction of Nd (y). Black line represents fitting curve evaluated from calculated lattice parameters$ 표 Lattice parameters for UO2, U0.98Nd0.02O2, and U0.94Nd0.06O2 pellets as a function of the molar fraction of Nd (y). Black line represents fitting curve evaluated from calculated lattice parameters
표 Raman spectra of UO2, U0.98Nd0.02O2, and U0.94Nd0.06O2 pellets
표 SEM images (×3,000) of (a) UO2, (b) U0.98Nd0.02O2, and (c) U0.94Nd0.06O2 pellets
표 SEM images (×1,000) and EDS mapping data of uranium, oxygen, and neodymium elements obtained from (a) UO2, (b) U0.98Nd0.02O2, and (c) U0.94Nd0.06O2 pellets
표 Optical image of Zr sample
표 XRD spectrum of Zr sample
표 Raman spectrum of Zr sample
표 SEM image (×1,000) and EDS mapping data of zirconium element obtained from Zr sample
표 Schematic illustration of U1-yNdyO2/Zr sample
표 Optical images of samples after annealing of (a) UO2 with (d) Zr, (b) U0.98Nd0.02O2, with (e) Zr, and (c) U0.94Nd0.06O2, with (f) Zr at 1200℃
표 Optical images of samples after annealing of (a) UO2/Zr, (b) U0.98Nd0.02O2, with (d) Zr, and (c) U0.94Nd0.06O2, with (e) Zr at 1450℃
표 XRD spectra of UO2, U0.98Nd0.02O2, and U0.94Nd0.06O2 pellets after annealing of U1-yNdyO2/Zr samples at 1200℃
표 Fig. 3-15. XRD spectra of U0.98Nd0.02O2 and U0.94Nd0.06O2 pellets after annealing of U1-yNdyO2/Zr samples at 1450℃
표 XRD spectra of Zr samples after annealing of U1-yNdyO2/Zr samples at 1200℃
표 XRD spectra of Zr samples after annealing of U1-yNdyO2/Zr samples at 1450℃
표 Raman spectra of UO2, U0.98Nd0.02O2, and U0.94Nd0.06O2 pellets after annealing of U1-yNdyO2/Zr samples at 1200℃
표 Raman spectra of U0.98Nd0.02O2 and U0.94Nd0.06O2 pellets after annealing of U1-yNdyO2/Zr samples at 1450℃
표 Raman spectra of Zr samples after annealing of U1-yNdyO2/Zr samples at 1200℃
표 Raman spectra of Zr samples after annealing of U1-yNdyO2/Zr samples at 1450℃
표 SEM images (×1,000) and EDS mapping data of uranium, oxygen, and neodymium elements obtained from (a) UO2, (b) U0.98Nd0.02O2, and (c) U0.94Nd0.06O2 pellets after annealing with Zr at 1200 ℃
표 SEM images (×1,000) and EDS mapping data of uranium, oxygen, zirconium, and neodymium elements obtained from (a) U0.98Nd0.02O2, and (b) U0.94Nd0.06O2 pellets after annealing with Zr at 1450 ℃
표 SEM images (×1,000) and EDS mapping data of zirconium element obtained from Zr samples after annealing with (a) UO2, (b) U0.98Nd0.02O2, and (c) U0.94Nd0.06O2 pellets at 1200 ℃
표 SEM images (×1,000) and EDS mapping data of zirconium element obtained from Zr samples after annealing with (a) U0.98Nd0.02O2 and (b) U0.94Nd0.06O2 pellets at 1450 ℃
표 XRD patterns of UO2 (black) and U1-yZryO2 pellets with y = 0.02 (red), 0.06 (blue), and 0.1 (green) from bottom to top
표 Lattice parameters obtained from XRD patterns of UO2 and U1-yNdyO2 pellets with increasing Nd content
표 XRD patterns of UO2 (black) and U1-yThyO2 pellets with y = 0.01 (red), 0.05 (blue), and 0.1 (green) from top to bottom
표 Lattice parameters obtained from XRD patterns of UO2 and U1-yThyO2 pellets with increasing Th content
$XRD patterns of UO2 (black) and U1-yZryO2 pellets with y = 0.01 (red), 0.03 (blue), 0.05 (magenta), and 0.1 (green) from bottom to top. The diffraction patterns of UO2 (PDF#05-0550), monoclinic ZrO2 (m-ZrO2; PDF#07-0343), and tetragonal ZrO2 (t-ZrO2; PDF#02-0733) in the bottom panels were obtained from the PDF-2 database$ 표 XRD patterns of UO2 (black) and U1-yZryO2 pellets with y = 0.01 (red), 0.03 (blue), 0.05 (magenta), and 0.1 (green) from bottom to top. The diffraction patterns of UO2 (PDF#05-0550), monoclinic ZrO2 (m-ZrO2; PDF#07-0343), and tetragonal ZrO2 (t-ZrO2; PDF#02-0733) in the bottom panels were obtained from the PDF-2 database
표 Lattice parameters obtained from XRD patterns of UO2 and U1-yZryO2 pellets with increasing Zr content
표 Comparing the domain structures on the surfaces of (U,Gd)O2, (U,Nd)O2, (U,Th)O2 and (U,Zr)O2 from top to bottom. Doping level increases from left to right. Magnification of all images is ×3000, and scale bars in images indicate 5 ㎛ length
표 Electrical conductivity of (U,Gd)O2, (U,Nd)O2, (U,Th)O2 and (U,Zr)O2 with various doping level
표 Raman spectra of UO2 (black) and U1-yNdyO2 pellets with y = 0.02 (red), 0.06 (blue), and 0.1 (green) from top to bottom
표 Deconvoluted Raman spectra of U0.99Nd0.01O2 (up) and U0.95Nd0.05O2 (bottom) pellets with Lorentzian peaks at ~445, ~535, ~575 and ~630 cm-1. Open circles and orange continuous line indicate the experimental data and fitted line using Lorentzian peaks, respectively
표 Area ratio between peaks at ~445 and ~535 cm-1 as a function of Nd content in U1-yNdyO2 pellets
표 Raman spectra of UO2 (black) and U1-yThyO2 pellets with y = 0.01 (red), 0.05 (blue), and 0.1 (green) from top to bottom
표 Raman spectra of UO2 (black) and U1-yZryO2 pellets with y = 0.01 (red), 0.03 (blue), 0.05 (magenta), and 0.1 (green). The shift and decrease in intensity of the T2g band and development of a peak at 598 cm-1 with increasing Zr content are shown in the inset
표 Comparison fo Raman spectra of U0.9Zr0.1O2 with those of monoclinic-ZrO2 and tetragonal-ZrO2
표 (a) T2g band position of UO2 and U1-yZryO2 pellets and (b) intensity ratio of the peak at 598 cm-1 to T2g band (I598/IT2g) as a function of Zr content(y)
표 (a) Vibrational frequencies of U1-yZryO2 as a function of Zr content (y). (b) The simulated intensities and Raman frequencies of U0.87Zr0.13O2. Normal modes of the peaks at (c) 466.82 cm-1 and (d) 596.15 cm-1. The yellow, green and red spheres represent U, Zr and O atoms, respectively
표 Cyclic voltammograms recorded on U1-yGdyO2 (left, up), U1-yZryO2 (right, up), U1-yNdyO2 (left, bottom), and U1-yThyO2 (right, bottom) electrodes in a 0.1 M NaClO4 solution containing [HCO3-/CO32-]=0.01 M, pH=9at pH 8.9, respectively. Scan rate was 50 mV/s
표 Raman spectra of hyper-stoichiometric UO2+x (black line) and U1-yThyO2+x pellets with y = 0.01 (red line), 0.05 (blue line), and 0.1 (green line) as shown from top to bottom
표 Deconvoluted Raman spectra of hyper-stoichiometric UO2+x and U1-yThyO2+x pellets with Lorentzian peaks at ~ 445 (black), 470 (red), 570 (blue) and 630 (green) cm-1. Black circles and magenta lines represent the experimental data and fitted lines, respectively
표 Intensity ratios of peaks at ~ 470 (black squares, I470/I445), 570 (red circles, I570/I445), and 630 (blue diamonds, I630/I445) cm-1 relative to the peak at ~ 445 cm-1 with a y value of U1-yThyO2+x
표 Optical images of (a) UO2, (b) U0.98Gd0.02O2, (c) U0.94Gd0.06O2, and (d) U0.90Gd0.10O2 pellets
표 XRD spectra of UO2, U0.98Gd0.02O2, U0.94Gd0.06O2, and U0.90Gd0.10O2 pellets
$Lattice parameters for UO2, U0.98Gd0.02O2, U0.94Gd0.06O2, and U0.90Gd0.10O2 pellets as a function of the molar fraction of Gd (y). Black line represents fitting curve evaluated from calculated lattice parameters$ 표 Lattice parameters for UO2, U0.98Gd0.02O2, U0.94Gd0.06O2, and U0.90Gd0.10O2 pellets as a function of the molar fraction of Gd (y). Black line represents fitting curve evaluated from calculated lattice parameters
표 Raman spectra of UO2, U0.98Gd0.02O2, U0.94Gd0.06O2, and U0.90Gd0.10O2 pellets
표 SEM images (×2,000) of (a) UO2, (b) U0.98Gd0.02O2, (c) U0.94Gd0.06O2, and (d) U0.90Gd0.06O2 pellets before polishing
표 SEM images (×2,000) and EDS mapping data of uranium, oxygen, and gadolinium elements obtained from (a) UO2, (b) U0.98Gd0.02O2, (c) U0.94Gd0.06O2, and (d) U0.90Gd0.10O2 pellets after polishing
표 Raman spectrum of polished Zr sample
표 SEM image (×2,000) obtained from polished Zr sample
표 Optical images of U1-yGdyO2/Zr samples, which are physically contacted between U1-yGdyO2 pelltes and Zr samples
표 High temperature chamber for heating of U1-yGdyO2/Zr samples
표 Optical images of samples after annealing of (a) UO2 with (e) Zr, (b) U0.98Gd0.02O2, with (f) Zr, and (c) U0.94Gd0.06O2, with (g) Zr and (d) U0.90Gd0.10O2, with (h) Zr at 300℃
표 Optical images of samples after annealing of (a) UO2 with (c) Zr and (b) U0.90Gd0.10O2, with (d) Zr at 1200℃
$Lattice parameters for U1-yGdyO2 pellets after annealing of U1-yGdyO2/Zr samples at 300, 700, and 1200 ℃ as a function of the molar fraction of Gd (y). Black line represents fitting curve evaluated from calculated lattice parameters$ 표 Lattice parameters for U1-yGdyO2 pellets after annealing of U1-yGdyO2/Zr samples at 300, 700, and 1200 ℃ as a function of the molar fraction of Gd (y). Black line represents fitting curve evaluated from calculated lattice parameters
표 Raman spectra of U1-yGdyO2 pellets after annealing of U1-yGdyO2/Zr samples at 300, 700, and 1200 ℃
표 Raman spectra of Zr samples after annealing of U1-yGdyO2/Zr samples at 300, 700, and 1200 ℃
표 SEM images (×2,000) obtained from U1-yGdyO2 pellets after annealing of U1-yGdyO2/Zr samples at 300, 700, and 1200 ℃
표 SEM images (×2,000) obtained from Zr samples after annealing of U1-yGdyO2/Zr samples at 300, 700, and 1200 ℃

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[국가R&D연구보고서] 조사핵연료 고체화학 특성 규명 연구
Research on the solid chemical characteristics and behavior of irradiated fuels 원문보기

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[국가R&D연구보고서] 조사핵연료 고체화학 특성 규명 연구 Research on the solid chemical characteristics and behavior of irradiated fuels 원문보기

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[국가R&D연구보고서] 조사핵연료 고체화학 특성 규명 연구
Research on the solid chemical characteristics and behavior of irradiated fuels 원문보기

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