KR20190019997A - Method of predicting a sintered density of a uranium oxide(UOx) pellet for the nuclear fuel by Spectrophotometer - Google Patents
Method of predicting a sintered density of a uranium oxide(UOx) pellet for the nuclear fuel by Spectrophotometer Download PDFInfo
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- 229910000439 uranium oxide Inorganic materials 0.000 title claims abstract description 74
- 238000000034 method Methods 0.000 title claims abstract description 34
- 239000003758 nuclear fuel Substances 0.000 title claims abstract description 9
- 239000008188 pellet Substances 0.000 title abstract 3
- WZECUPJJEIXUKY-UHFFFAOYSA-N [O-2].[O-2].[O-2].[U+6] Chemical compound [O-2].[O-2].[O-2].[U+6] WZECUPJJEIXUKY-UHFFFAOYSA-N 0.000 claims abstract description 36
- ZAASRHQPRFFWCS-UHFFFAOYSA-P diazanium;oxygen(2-);uranium Chemical compound [NH4+].[NH4+].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[U].[U] ZAASRHQPRFFWCS-UHFFFAOYSA-P 0.000 claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims description 31
- 239000002243 precursor Substances 0.000 claims description 5
- QIHQMTDZLVGHRM-UHFFFAOYSA-N N.[U+6] Chemical compound N.[U+6] QIHQMTDZLVGHRM-UHFFFAOYSA-N 0.000 claims 2
- 238000004458 analytical method Methods 0.000 abstract description 11
- 238000005245 sintering Methods 0.000 description 15
- 239000000446 fuel Substances 0.000 description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- 238000012887 quadratic function Methods 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- SANRKQGLYCLAFE-UHFFFAOYSA-H uranium hexafluoride Chemical compound F[U](F)(F)(F)(F)F SANRKQGLYCLAFE-UHFFFAOYSA-H 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 150000003671 uranium compounds Chemical class 0.000 description 2
- DSERHVOICOPXEJ-UHFFFAOYSA-L uranyl carbonate Chemical compound [U+2].[O-]C([O-])=O DSERHVOICOPXEJ-UHFFFAOYSA-L 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 229910052770 Uranium Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 238000001739 density measurement Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004148 unit process Methods 0.000 description 1
- DNYWZCXLKNTFFI-UHFFFAOYSA-N uranium Chemical compound [U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U] DNYWZCXLKNTFFI-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N9/00—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity
- G01N9/36—Analysing materials by measuring the density or specific gravity, e.g. determining quantity of moisture
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
- G01J3/28—Investigating the spectrum
- G01J3/42—Absorption spectrometry; Double beam spectrometry; Flicker spectrometry; Reflection spectrometry
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
- G01J3/46—Measurement of colour; Colour measuring devices, e.g. colorimeters
- G01J3/462—Computing operations in or between colour spaces; Colour management systems
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
- G01J3/28—Investigating the spectrum
- G01J3/2823—Imaging spectrometer
- G01J2003/2826—Multispectral imaging, e.g. filter imaging
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
- G01J3/46—Measurement of colour; Colour measuring devices, e.g. colorimeters
- G01J2003/466—Coded colour; Recognition of predetermined colour; Determining proximity to predetermined colour
Abstract
Description
본 발명은 핵연료 제조공정에 있어서, 우라늄산화물(UOx)의 전구체인 중우라늄산암모늄(ammonium diuranate)의 색도를 분광기(Spectrophotometer)로 측정함으로써 소결공정 전에 우라늄산화물(UOx)의 소결밀도를 예측 계산 또는 분석하는 방법에 관한 것이다.The present invention relates to a method for predicting or calculating the sintering density of uranium oxide (UOx) before sintering by measuring the chromaticity of ammonium diuranate, which is a precursor of uranium oxide (UOx), by a spectrophotometer And the like.
핵연료 제조공정은 육불화우라늄(UF6)으로부터 우라늄산화물(UOx) 분말을 제조한 후 이를 압분, 소결하여 생산된 소결체를 연료봉에 장입하고 조립하여 핵연료 집합체를 만드는 공정이다.The nuclear fuel fabrication process is a process to manufacture uranium oxide (UOx) powder from uranium hexafluoride (UF 6 ), compaction and sintering the powder, and charging the sintered product into the fuel rod and assembling the fuel assembly.
이 공정 중에서, 육불화우라늄(UF6)으로부터 우라늄산화물(UOx) 분말을 제조하는 공정을 재변환공정이라 하는데, 이는 다시 건식 재변환공정과 습식 재변환공정으로 나눌 수 있다. 건식 재변환공정은 육불화우라늄(UF6)을 기체 상태에서 반응시켜 직접 우라늄산화물(UOx) 분말을 생산하며, 습식 재변환공정은 전구체인 중우라늄산암모늄(ammonium diuranate) 또는 탄산우라닐암모늄(ammonium uranyl carbonate)를 거쳐 우라늄산화물(UOx) 분말을 생산하는 과정상의 차이가 있다.Among these processes, the process of producing uranium oxide (UOx) powder from uranium hexafluoride (UF 6 ) is referred to as a re-conversion process, which can be divided into a dry recycling process and a wet recycling process. The dry recycle process produces uranium oxide (UOx) powder directly by reacting uranium hexafluoride (UF 6 ) in the gaseous state, and the wet recom- bination process is a process that uses the precursor, ammonium diuranate or ammonium uranyl carbonate ammonium uranyl carbonate) to produce uranium oxide (UOx) powder.
재변환공정을 통해 생산된 우라늄산화물(UOx)의 소결밀도 분석은 핵연료를 제조하는 과정에 있어서 필수적인 기술이다. 지금까지는 소결밀도의 분석을 우라늄산화물(UOx) 분말 상태에서 분석할 수 없었고, 소결공정까지 모두 거친 후 소결체 Sample을 제조하여 소결밀도를 측정하였다. 이렇게 할 경우 Electrical Balance 측정 장비를 이용하여 아래와 같은 식에 따라 소결밀도(Sintered Density)를 산출하였다.Analysis of the sintered density of uranium oxide (UOx) produced through the recycling process is an essential technique in the process of producing nuclear fuel. Until now, the analysis of sintering density has not been able to be carried out in the state of uranium oxide (UOx) powder. After all the sintering process has been carried out, a sintered sample is prepared and the sintered density is measured. In this case, the sintered density was calculated according to the following equation using an electrical balance measuring instrument.
하지만, 이러한 소결밀도 분석은 소결공정을 수행한 이후에 소결체의 품질 검사 차원에서 이루어지는 것이므로, 만약 소결밀도가 핵연료 제조의 시방범위에 포함되지 않는 값이 나오는 경우 다시 후속 처리공정을 거쳐야 한다는 위험요소를 지니고 있다. 추가로 이러한 측정 방법은 Electrical Balance와 물을 사용한 부피변화를 이용하는 밀도 측정 방법이므로 전후의 처리과정이 매우 번거로우며 분석자에 따라 오차발생률이 높을 수 있는 단점이 있었다. However, since the sintering density analysis is performed after the sintering process is performed to check the quality of the sintered body, if the sintering density is not included in the specification range of the nuclear fuel production, . In addition, since this measurement method is a density measurement method using the electrical balance and the volume change using water, the post-processing process is very troublesome and the error rate may be high according to the analyst.
본 발명자들은, 이러한 기존의 단점을 극복하여, 소결공정 전에 우라늄산화물(UOx)의 소결밀도를 예측 계산 또는 분석하는 방법을 고안하여, 실제로 측정할 수 있음을 확인하여 본 발명을 완성하였다.The inventors of the present invention completed the present invention by confirming that a method of predicting or analyzing the sintering density of uranium oxide (UOx) before and after the sintering process was devised and actually measured.
본 발명의 목적은, 핵연료용 우라늄산화물(UOx) 소결체용 분말 제조 과정에서, 우라늄산화물(UOx)의 소결밀도를 사전 예측 및 분석하는 간편하고 신뢰성이 높은 방법을 제공하고자 함에 있다.It is an object of the present invention to provide a simple and reliable method for predicting and analyzing the sintering density of uranium oxide (UOx) in the process of producing a powder for sintered uranium oxide (UOx) for nuclear fuel.
상기 목적을 달성하기 위하여, 본 발명은 핵연료용 우라늄산화물(UOx) 소결체용 분말 제조공정에 있어서, (1) 측정 대상인 중우라늄산암모늄(ammonium diuranate) 분말의 색도를 분광기(Spectrophotometer)로 측정하는 단계; (2) 상기 측정한 색도의 데이터값을, 표준 중우라늄산암모늄(ammonium diuranate) 분말의 색도 그래프의 값과 비교하는 단계; 및 (3) 상기 비교를 통해 측정 대상인 중우라늄산암모늄(ammonium diuranate) 분말의 예상 우라늄산화물(UOx) 소결밀도를 계산하여 얻는 단계;를 포함하는 핵연료용 우라늄산화물(UOx) 소결체용 분말의 소결밀도 계산 방법을 제공한다.In order to achieve the above object, the present invention provides a process for producing a powder for a uranium oxide (UOx) sintered body for nuclear fuel, comprising the steps of: (1) measuring the chromaticity of the ammonium diuranate powder to be measured with a spectrophotometer ; (2) comparing the measured data value of the chromaticity with the value of a chromaticity graph of a standard ammonium uranate powder; And (3) calculating the sintered density of the uranium oxide (UOx) of the ammonium diuranate powder to be measured through the comparison, thereby obtaining a sintered density of the powder for uranium oxide (UOx) sintered fuel for fuel. Provides a calculation method.
바람직하게는, 색도의 데이터값은 L* a* b* 표색계를 사용한다.Preferably, the L * a * b * color system is used as the data value of the chromaticity.
바람직하게는, 색도의 데이터값은 L* a* b* 표색계의 L*값을 사용한다.Preferably, the L * value of the L * a * b * color system is used as the data value of the chromaticity.
상기와 같은 본 발명에 따르면, 종래 분석방법의 문제점인 소결체로 생산된 제품에 대해서만 분석이 가능하며 분석 결과에 따라 후속처리공정을 거쳐야 한다는 위험요소를 제거할 수 있다. 이와 더불어, 우라늄산화물(UOx) 분말을 제조하기 전에 전구체인 중우라늄산암모늄(ammonium diuranate)의 색도를 분광기(Spectrophotometer)로 측정하여 이후 제조될 우라늄산화물(UOx)의 소결밀도를 예측함에 따라, 평균 분석 시간을 기존 방법의 13시간(소결체 제조공정 포함)대비 약 2.5% 수준인 20분 내외로 단축시키는 효과가 있다.According to the present invention as described above, it is possible to analyze only the products produced by the sintered body, which is a problem of the conventional analysis method, and eliminate the risk factor that the subsequent processing process must be performed according to the analysis result. In addition, the chromaticity of the ammonium diuranate precursor, uranium oxide (UOx) powder, was measured by a spectrophotometer to predict the sintered density of uranium oxide (UOx) The analysis time is reduced to about 20 minutes, which is about 2.5% of the conventional method (including the sintering process).
따라서, 본 발명에 의해 도출된 분석 데이터는 소결체 제조공정의 모든 단계에서 소결밀도를 분석 및 예측함으로써 최상의 소결체를 제조하는데 기여할 수 있다.Therefore, the analytical data derived by the present invention can contribute to the manufacture of the best sintered body by analyzing and predicting the sintered density at every stage of the sintered body manufacturing process.
도 1은 우라늄산화물(UOx) 분말의 소결밀도 계산 과정 흐름도이다.
도 2는 A) 우라늄산암모늄(Ammonium diuranate)와 B) 우라늄산화물(UOx) 분말의 사진이다.
도 3은 분광기로 측정한 색도값 L*과 소결밀도 간 상관관계 그래프이다.
도 4는 분광기로 측정한 색도값 a*과 소결밀도 간 상관관계 그래프이다.
도 5는 분광기로 측정한 색도값 b*과 소결밀도 간 상관관계 그래프이다.
도 6은 분광기로 측정한 색도값과 소결밀도 간 상관관계를 이용하여, 소결밀도를 예측하는 그래프 모습이다.FIG. 1 is a flow chart for calculating the sintering density of uranium oxide (UOx) powder.
Figure 2 is a photograph of A) Ammonium diuranate and B) Uranium oxide (UOx) powder.
3 is a graph showing a correlation between the chromaticity value L * and the sintered density measured with a spectroscope.
4 is a graph showing a correlation between a chromaticity value a * measured by a spectroscope and a sintered density.
5 is a graph showing a correlation between the chromaticity value b * measured by a spectroscope and sintered density.
FIG. 6 is a graph showing the sintered density predicted using the correlation between the chromaticity value measured by the spectroscope and the sintered density.
이하, 본 발명을 상세히 설명한다.Hereinafter, the present invention will be described in detail.
기존 방법의 문제점을 해결하기 위하여, 본 발명은 습식 재변환공정 중 침전/여과/건조 공정에서 생성된 중우라늄산암모늄(ammonium diuranate)의 색도를 분광기(Spectrophotometer)로 측정함으로써, 소결체 제조공정에 투입되기 전에 우라늄산화물(UOx)의 소결밀도를 분광기를 이용하여 예측 계산 및 분석하였고, 이러한 방법의 예측력이 뛰어남을 확인하였다.In order to solve the problems of the conventional method, the present invention is characterized in that the chromaticity of ammonium diuranate produced in the precipitation / filtration / drying process during the wet recycle process is measured by a spectrophotometer, (UOx) sintered density was estimated and analyzed using a spectrometer, and it was confirmed that this method has excellent predictive power.
본 발명에서 활용한 분광기(Spectrophotometer) 분석은 최근 화학, 생명과학, 환경, 제약 분야 등에서 가장 많이 활용하고 있는 분석 방법이다. 이 원리는 물질 종류에 따라 빛 에너지를 흡수하여 전자전이 및 회전과 같은 여러 가지 분자운동을 일으키면서 나타나는 고유의 흡수 스펙트럼을 측정하는 것이다. 이때 물질마다 발생하는 흡수 스펙트럼 및 에너지 값의 차이는 L* a* b* 표색계로 표현된다. 이러한 분광기(Spectrophotometer)를 활용한 분석방법은 유기 또는 무기 화합물의 정량, 정성분석에까지 광범위하게 활용되고 있다.The spectrophotometer analysis utilized in the present invention is the most widely used analytical method in the fields of chemistry, life sciences, environment, and pharmaceuticals. This principle is to measure the intrinsic absorption spectrum of various kinds of molecules, such as electron transfer and rotation, by absorbing light energy according to the kind of substance. The difference between the absorption spectra and the energy values generated for each material is represented by the L * a * b * color system. These spectrophotometer-based analytical methods are widely used for quantitative and qualitative analysis of organic or inorganic compounds.
구체적으로는, 핵연료용 우라늄산화물(UOx) 소결체용 분말 제조공정에 있어서, (1) 측정 대상인 중우라늄산암모늄(ammonium diuranate) 분말의 색도를 분광기(Spectrophotometer)로 측정하는 단계; (2) 상기 측정한 색도의 데이터값을, 표준 중우라늄산암모늄(ammonium diuranate) 분말의 색도 그래프의 값과 비교하는 단계; 및 (3) 상기 비교를 통해 측정 대상인 중우라늄산암모늄(ammonium diuranate) 분말의 예상 우라늄산화물(UOx) 소결밀도를 계산하여 얻는 단계;를 포함하는 핵연료용 우라늄산화물(UOx) 소결체용 분말의 소결밀도 계산 방법을 제공한다.Specifically, in the process for producing powders for uranium oxide (UOx) sintered fuel for nuclear fuel, (1) measuring the chromaticity of the ammonium diuranate powder to be measured with a spectrophotometer; (2) comparing the measured data value of the chromaticity with the value of a chromaticity graph of a standard ammonium uranate powder; And (3) calculating the sintered density of the uranium oxide (UOx) of the ammonium diuranate powder to be measured through the comparison, thereby obtaining a sintered density of the powder for uranium oxide (UOx) sintered fuel for fuel. Provides a calculation method.
상기 색도의 데이터값은 L* a* b* 표색계를 사용하는 것이 바람직하다.It is preferable that the data value of the chromaticity be an L * a * b * color system.
상기 색도의 데이터값은 L* a* b* 표색계의 L*값을 사용하는 것이 바람직하다.The data value of the chromaticity is preferably the L * value of the L * a * b * colorimetric system.
이하, 실시예를 통하여 본 발명을 더욱 상세히 설명하고자 한다. 이들 실험예는 오로지 본 발명을 예시하기 위한 것으로서, 본 발명의 범위가 이들 실험예에 의해 제한되는 것으로 해석되지는 않는 것은 당업계에서 통상의 지식을 가진 자에게 있어서 자명할 것이다.Hereinafter, the present invention will be described in more detail with reference to Examples. It will be apparent to those skilled in the art that these examples are for illustrative purposes only and that the scope of the present invention is not construed as being limited by these examples.
실시예 1. 표준 중우라늄산암모늄(ammonium diuranate) 분말의 색도 그래프 결정Example 1 Determination of Chromatogram of Ammonium Diuranate Powder in Standards
우라늄산화물(UOx)의 전구체인 중우라늄산암모늄(ammonium diuranate) 분말 샘플의 색도 값을 Spectrophotometer로 측정하여 우라늄산화물(UOx)의 소결밀도를 예측 계산 및 분석하기 위해서는 먼저 표준 데이터에 의한 그래프를 결정하는 것이 필요하다.In order to predict and calculate the sintered density of uranium oxide (UOx) by measuring the chromaticity value of a sample of ammonium diuranate powder, which is a precursor of uranium oxide (UOx), by a spectrophotometer, It is necessary.
실험에 따르면, 습식 재변환공정 중, 중우라늄산암모늄(ammonium diuranate)을 제조하는 단계인 침전 단위공정에서, 일부 조업변수인 pH 및 NH3/Air 비율이 우라늄산화물(UOx)의 소결밀도와 관련되며, 또한 이 조업변수가 중우라늄산암모늄(ammonium diuranate)의 색도(본원의 실험에서는 L*a*b* 표색계로 표현)와도 관련이 있는 것으로 나타났다.Experiments have shown that in the sedimentation unit process, which is the step of preparing ammonium diuranate during the wet recycle process, some operating parameters, pH and NH3 / Air ratio, are related to the sintered density of uranium oxide (UOx) , And this operating parameter is also related to the chromaticity of ammonium diuranate (expressed in L * a * b * colorimetry in our experiments).
이에 따라, 다른 변인을 통제하고 해당 조업변수를 달리하여, 충분한 수의 중우라늄산암모늄(ammonium diuranate) 분말 샘플을 제조하고, 각각의 샘플 색도를 측정한 다음, 이를 동일 조건에서 배소/환원하여 우라늄산화물(UOx) 분말을 제조한 후 다시 각각의 소결밀도를 측정하면 실제 공정 운영중 사용할 수 있는 표준 데이터에 의한 그래프를 얻을 수 있으며, 이를 도식화 또는 수식화하면 이후에 측정하는 샘플에 대해서도 사용할 수 있게 된다.Accordingly, a sufficient number of ammonium diuranate powder samples were prepared by controlling other variables and operating variables, and the chromaticity of each sample was measured and then roasted / reduced under the same conditions to produce uranium After the oxide (UOx) powders are prepared, the sintered density of each of them can be measured again to obtain a graph based on standard data that can be used during actual process operation. .
(도 2)와 같은 모습의 우라늄산암모늄(Ammonium diuranate)과 우라늄산화물(UOx) 분말을, 침전/여과/건조과정의 조업변수인 최종 pH와 NH3/Air 비율을 다르게 하여 제조하고, 우라늄산암모늄(Ammonium diuranate)의 측정 색도값 L*, a*, b*와 소결밀도 간 상관관계 수식을 그래프를 이용하여 구한다.Ammonium diuranate and uranium oxide (UOx) powders of the same form as in Example 1 (FIG. 2) were prepared by varying the final pH and NH 3 / air ratio, which are operating parameters of the precipitation / filtration / The relationship between measured chromaticity values L *, a *, b * and sintered density of ammonium diuranate is obtained using a graph.
구체적으로는, 다섯 개의 우라늄화합물(Ammonium diuranate)을 각 Glass cell에 적당량 넣은 후, Spectrophotometer로 Calibration을 실시하고 표준 Sample들을 측정한다. 이때 측정 색도값으로 표현되는 L*(또는 a*, b*) 표색계 데이터와 실제 소결체의 소결밀도 데이터를 바탕으로 다섯 개의 표준 Sample간의 추세선(X축 : L* 또는 a* 또는 b*, Y축 : 소결밀도)을 도출하여 우라늄화합물(Ammonium diuranate)에 대한 표준 Sample 공식을 얻는다.Specifically, add the appropriate amount of five uranium compounds (Ammonium diuranate) to each glass cell, calibrate with a spectrophotometer, and measure standard samples. Based on the L * (or a *, b *) colorimetric data represented by the measured chromaticity values and the sintered density data of the actual sintered body, a trend line (X axis: L * or a * or b * : Sintered density) to obtain a standard Sample formula for the uranium compound (Ammonium diuranate).
좀 더 구체적으로는, 아래 표와 같은 값들을 얻었다.More specifically, the values shown in the table below were obtained.
(도 3)에서 보듯이, L* 값과 소결밀도는 일정한 곡선(2차 함수로 표현될 수 있음)의 수식으로 나타낼 수 있음을 확인하였다. R2 값은 0.9618로 신뢰성이 높음을 확인하였다.(FIG. 3), it was confirmed that the L * value and the sintered density can be expressed by a constant curve (which can be expressed by a quadratic function). R2 value was 0.9618, confirming high reliability.
이에 비해 (도 4)에서 보듯이, a*값과 소결밀도도 일정한 곡선(2차 함수로 표현될 수 있음)의 수식으로 나타낼 수 있지만, R2 값은 0.4034로 신뢰성이 높지 않음을 확인하였다. (도 5)에서 보듯이, b*값과 소결밀도도 일정한 곡선(2차 함수로 표현될 수 있음)의 수식으로 나타낼 수 있지만, R2 값은 0.6374로 신뢰성이 높지 않음을 확인하였다.On the other hand, as shown in FIG. 4, the a * value and the sintered density can also be expressed by a constant curve (which can be expressed by a quadratic function), but the R2 value is 0.4034, indicating that the reliability is not high. As can be seen from FIG. 5, the b * value and the sintered density can also be represented by a constant curve (which can be expressed as a quadratic function), but the R2 value is 0.6374, indicating that the reliability is not high.
결국 L* 값을 기준으로 소결밀도를 높은 신뢰성으로 산출할 수 있음을 확인하였다.As a result, it was confirmed that the sintered density can be calculated with high reliability based on the L * value.
실시예 2. 측정 대상인 중우라늄산암모늄(ammonium diuranate) 분말의 색도 측정과 소결 밀도 계산Example 2. Measurement of chromaticity and sintering density of ammonium diuranate powder to be measured
실제 우라늄산화물(UOx) 소결체용 분말 제조 공정 운영중에는, 제조된 중우라늄산암모늄(ammonium diuranate) 분말의 샘플을 채취하여 Glass cell에 적당량 넣은 후, 분광기(Spectrophotometer)로 Calibration을 실시하고 측정하여 이런 과정을 통해 색도값으로 L* a* b* 표색계를 사용하는 데이터를 얻는다(도 1의 S100 단계).During operation of the UOx powder manufacturing process, a sample of the prepared ammonium diuranate powder is sampled and placed in a glass cell in an appropriate amount, followed by calibrating with a spectrophotometer, To obtain data using the L * a * b * colorimetric system as the chromaticity value (step S100 of FIG. 1).
그리고 나서, 실시예 1.에서 얻은 표준 색도 그래프의 값과 비교(도 1의 S200 단계)하고 L*값을 기준으로 공식에 넣어 답을 구하면, 해당 샘플이 우라늄산화물(UOx) 소결체가 되었을 때의 소결밀도 값을 예측 계산 및 분석(도 1의 S300 단계)할 수 있다.Then, the value is compared with the value of the standard chromaticity graph obtained in Example 1 (step S200 in FIG. 1), and the formula is added to the formula based on the L * value. If the sample is a uranium oxide (UOx) sintered body The sintered density value can be predictively calculated and analyzed (step S300 in FIG. 1).
(도 6)에서 L*값을 기반으로 소결밀도를 계산하는 사례를 볼 수 있다. L*값이 79이므로, 소결밀도 예측값은 10.35가 되고, 실제 소결 후의 측정값과 동일한 것을 확인하였다.(FIG. 6), an example of calculating the sintered density based on the L * value can be seen. Since the L * value is 79, the sintered density predicted value is 10.35, which is the same as the measured value after the actual sintering.
이상, 본 발명내용의 특정한 부분을 상세히 기술하였는바, 당업계의 통상의 지식을 가진 자에게 있어서, 이러한 구체적인 기술은 단지 바람직한 실시양태일 뿐이며, 이에 의해 본 발명의 범위가 제한되는 것이 아닌 점은 명백할 것이다. 따라서 본 발명의 실질적인 범위는 첨부된 청구항들과 그것들의 등가물에 의해 정의된다고 할 것이다. Having described specific portions of the present invention in detail, those skilled in the art will appreciate that these specific embodiments are merely preferred embodiments and that the scope of the present invention is not limited thereby. something to do. Accordingly, the actual scope of the present invention will be defined by the appended claims and their equivalents.
Claims (1)
(1) 샘플 우라늄산화물(UOx) 소결체와, 이 샘플 우라늄산화물 소결체의 전구체인 샘플 중우라늄암모늄(ammonium diuranate) 분말을 측정하여 중우라늄암모늄 분말의 색도 값에 대한 우라늄산화물 소결체의 소결 밀도를 포함하는 표준 데이터를 얻는 단계;
(2) 분광기를 이용하여 표적 우리늄산화물 소결체의 제조 공정에서 표적 중우라늄암모늄 분말의 색도 값을 측정하는 단계;
(3) 상기 표준 데이터에서 표적 중우라늄암모늄 분말의 색도 값에 대응하는 색도 값을 구하는 단계; 및
(4) 대응하는 색도 값에 대해 표준 데이터로부터 소결밀도를 구하여 표적 우라늄 산화물 (UOx) 소결체의 소결밀도를 예측하는 단계;를 포함하는 핵연료용 우라늄산화물(UOx) 소결체용 분말의 소결밀도 예측 방법.
In a method for predicting sintered density of uranium oxide (UOx) sintered body for nuclear fuel,
(1) A method for producing a uranium oxide (UOx) sintered body, comprising the steps of: measuring a sample uranium oxide (UOx) sintered body and ammonium diuranate powder as a precursor of the sample uranium oxide sintered body, Obtaining standard data;
(2) measuring the chromaticity value of the uranium ammonium powder in the target in the manufacturing process of the target uranium oxide sintered body using the spectroscope;
(3) obtaining a chromaticity value corresponding to the chromaticity value of the uranium ammonium powder in the target from the standard data; And
(4) determining the sintered density of the sintered uranium oxide (UOx) sintered body by determining the sintered density from the standard data for the corresponding chromaticity value, and predicting the sintered density of the sintered uranium oxide (UOx) sintered body.
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| JP2502150B2 (en) * | 1989-06-08 | 1996-05-29 | 三菱原子燃料株式会社 | Method for measuring sinterability of uranium dioxide powder |
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| JP2502150B2 (en) * | 1989-06-08 | 1996-05-29 | 三菱原子燃料株式会社 | Method for measuring sinterability of uranium dioxide powder |
| US5602646A (en) * | 1992-12-29 | 1997-02-11 | Societe Franco-Belge De Fabrication De Combustibles | Optical method and device for automatically classifying cylindrical nuclear-fuel pellets |
| JP2003513273A (en) * | 1999-11-03 | 2003-04-08 | コミツサリア タ レネルジー アトミーク | Elemental analyzer by optical emission spectrometry for laser-produced plasma |
| KR20110124854A (en) * | 2010-05-12 | 2011-11-18 | 삼성코닝정밀소재 주식회사 | Sputtering target based zinc oxide contained aluminum and method deciding the faluty performance of the same |
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