JP3836089B2 - Sample container for melting point measurement of MOX fuel - Google Patents
Sample container for melting point measurement of MOX fuel Download PDFInfo
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- JP3836089B2 JP3836089B2 JP2003173954A JP2003173954A JP3836089B2 JP 3836089 B2 JP3836089 B2 JP 3836089B2 JP 2003173954 A JP2003173954 A JP 2003173954A JP 2003173954 A JP2003173954 A JP 2003173954A JP 3836089 B2 JP3836089 B2 JP 3836089B2
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Description
【０００１】
【発明の属する技術分野】
本発明は、サーマルアレスト法によりＭＯＸ燃料の融点を測定するための耐熱試料容器に関し、更に詳しく述べると、全体がタングステン−レニウム合金からなる融点測定用試料容器に関するものである。本発明は、特に高Ｐｕ富化度で高Ｏ／ＭのＵ−Ｐｕ混合酸化物の融点測定に有用である。
【０００２】
【従来の技術】
【特許文献１】
特開２００２−２９６２０６号公報
【０００３】
高速増殖炉ではＭＯＸ燃料（ウラン−プルトニウム混合酸化物）が用いられている。これは、酸化ウラン（ＵＯ2 ）と酸化プルトニウム（ＰｕＯ2 ）の固溶体である。酸化ウラン（ＵＯ2 ）と酸化プルトニウム（ＰｕＯ2 ）は同じ結晶構造を持ち、全組成範囲にわたって固溶する。また、混合酸化物では、ＭＯ2±x （Ｍ＝Ｐｕ＋Ｕ）が可能であり、広い単相領域が存在する。ここで酸素と重金属の比はＯ／Ｍ（＝２±ｘ）と呼ばれており、化学量論比２．０からのずれの程度に依存して物性が変化する。ＭＯＸ燃料として用いられているのは、Ｏ／Ｍ＝１．９９〜１．９５が多いとされている。
【０００４】
ところで、酸化ウラン（ＵＯ2 ）の溶融温度は２８４０℃前後、酸化プルトニウム（ＰｕＯ2 ）の溶融温度は２３９０℃前後であり、混合酸化物の場合には組成に応じて両者の間の値をとる。またＯ／Ｍによっても溶融温度は変化する。更に、燃焼が進むと、核***生成物（ＦＰ）の蓄積に伴う融点の低下が生じる。このようなことから分かるように、融点の正確な測定は、核燃料の開発・製造に極めて重要である。
【０００５】
従来、核燃料物質の融点測定にはサーマルアレスト（熱停留）法が用いられている。これは、測定試料を封入した容器を加熱炉内に設置し、温度計測しながら試料を昇温していき、試料が溶融する際の潜熱（融解吸熱）により昇温が停滞する熱曲線の変化を読み取ることで試料の融点を求める方法である。変曲点の読み取り誤差を極力低く抑えるために、試料の温度計測と同時に試料容器の温度を計測し、容器温度データをリファレンスとして、リファレンスと試料温度データとの差分をプロットし、プロットした示差熱曲線の変曲点を読み取ることで試料の融点を求める方法も提案されている（特許文献１参照）。
【０００６】
ところで、融点を測定する試料となる核燃料物質の中には、前記のように、融点が２８００℃を超えるものもある。そのために試料容器としては、従来、タングステン製の容器が用いられている。
【０００７】
【発明が解決しようとする課題】
しかし、ＭＯＸ燃料について融点測定を行おうとすると、熱曲線の形状が非常に悪く不安定となり解析が困難になるという問題があった。特に、Ｐｕ濃度が約３０％のＭＯＸ燃料について、燃料設計等で必要となってくるＯ／Ｍ＝２．００〜１．９８付近では融点の測定を行っても、信頼性の高い正確なデータを得ることは困難であった。このように従来方法において、熱曲線の形状が非常に悪く不安定となり解析が困難になる原因については、解明されていなかった。
【０００８】
本発明の目的は、ＭＯＸ燃料中の酸素と試料容器との反応を抑え、昇温停滞時の熱曲線の不安定性を低減させてＭＯＸ燃料の融点測定に対する信頼性を向上させることができる融点測定用試料容器を提供することである。本発明の他の目的は、特に燃料設計等の観点から重要性の高いＰｕ濃度が３０％以下のＭＯＸ燃料において、Ｏ／Ｍ＝２．００〜１．９８付近のＵ−Ｐｕ混合酸化物の融点の正確な信頼性の高い測定が行える融点測定用試料容器を提供することである。
【０００９】
【課題を解決するための手段】
タングステン製試料容器にＭＯＸ燃料（Ｕ−Ｐｕ混合酸化物）を封入して、サーマルアレスト法によって融点測定を行った後、試料の金相観察を行った結果、試料中にタングステンが多く混入していることが判明した。試料中にタングステンが混入する原因は、ＭＯＸ燃料中に含まれる酸素と試料容器の構成材であるタングステンとが反応するためであり、ＭＯＸ燃料とタングステン製試料容器の酸素ポテンシャル（酸化のし易さの目安）がタングステン製試料容器の方が高いために起こるものと考えられる。
【００１０】
このようなＭＯＸ燃料と試料容器構成材であるタングステンとにおける酸素のやりとりが測定に影響している可能性があり、これが測定の不安定性を大きくしていたものと推測された。そこで鋭意研究を続けた結果、本発明者等は、従来技術において熱曲線の形状が非常に悪く解析が困難になってしまう原因は、Ｕ−Ｐｕ混合酸化物中に含まれる酸素と試料容器の構成材であるタングステンとが反応し、その反応の際に発生する熱が、試料溶融の際の融解吸熱と同時に起こることによって昇温停滞の熱曲線が不安定なものになってしまうためであることを見出した。これはタングステン製試料容器を使用してＰｕ濃度が約３０％でＯ／Ｍが２．００付近のＵ−Ｐｕ混合酸化物の融点測定を行う場合に必ず生じる現象である。本発明は、かかる熱曲線形状悪化のメカニズムの知得に基づきなされたものである。
【００１１】
Ｕ−Ｐｕ混合酸化物中の酸素とタングステン製試料容器との反応は、Ｏ／Ｍを下げることにより低減できることが分かっている。具体的には、Ｐｕ濃度が約３０％のＵ−Ｐｕ混合酸化物において、上記の現象が見られなくなるＯ／Ｍはおおよそ１．９４以下である。しかし、それでは燃料設計等で必要となってくるＯ／Ｍ＝２．００〜１．９８付近の融点の予測は不可能である。そのため、何らかの対策が必要となる。
【００１２】
このような課題を解決できる本発明は、ＭＯＸ燃料を封入してサーマルアレスト法により融点を測定するための試料容器であって、全体がタングステン−レニウム合金からなるＭＯＸ燃料の融点測定用試料容器である。ここで典型的には、測定試料となるＭＯＸ燃料はＰｕ濃度が約３０％（例えば３０〜２９％程度）でＯ／Ｍ＝２．００〜１．９５のＵ−Ｐｕ混合酸化物であり、容器構成材であるタングステン−レニウム合金はタングステン９０％−レニウム１０％からなる。一般的にはＰｕ濃度３０〜０％を測定範囲としており、それに応じて本発明は３０％Ｐｕ以下のＭＯＸ燃料の融点測定に使用できる。
【００１３】
【発明の実施の形態】
融点の測定方法は、基本的には従来技術と同様であってよく、測定試料を封入した容器を加熱炉内に設置し、温度計測しながら試料を昇温していき、試料が溶融する際の潜熱（融解吸熱）により昇温が停滞し、溶融が終了した時点で再び昇温が継続される熱曲線を得て、この熱曲線の解析から試料の融点を求めるサーマルアレスト法である。
【００１４】
酸化ウラン（ＵＯ2 ）をタングステン製試料容器に封入して測定した結果の一例を図１に示す。酸化ウランの場合には、容器構成材であるタングステンとの反応は生じない。また、酸化ウランの場合には、固相温度と液相温度が１点（同一の温度）として観測されるため、昇温の停滞を明確に認定することができる。従って、模式的には図２に示すような熱曲線が得られる。具体的な解析法は、サーマルアレスト開始直前までの熱曲線とサーマルアレストが現れている間の熱曲線の交点を求め、それを融点とする。
【００１５】
ところが、ＭＯＸ燃料の場合、固相温度と液相温度とが２点（異なる温度）として観測されるため、昇温の停滞は必ずしも明確であるとは限らない。理想的な場合の熱曲線を模式的に表したのが図３である。従って、このような場合も、基本的には熱曲線の変曲点から融点を求めることができる。
【００１６】
【実施例】
図４は本発明に係る融点測定用試料容器の一実施例を示す断面図である。試料容器は、円筒部１０の下端に底蓋１２を嵌め込み、所定量の試料を入れ、上端に上蓋１４を嵌め込み、溶接等により封入する構造である。なお、底蓋中央の凹部１６は放射温度計の測定部分である。本発明では、これら円筒部１０、底蓋１２、及び上蓋１４の全てがタングステン−レニウム合金によって製作されており、その点に特徴がある。典型的な組成は、タングステン９０％−レニウム１０％である。
【００１７】
このようなタングステン−レニウム合金製試料容器を用いたＵ−Ｐｕ混合酸化物の熱曲線の一例を図５に示す。試料のＰｕ濃度は２９．９％、Ｏ／Ｍ＝２．００である。また比較のために、従来のタングステン製試料容器を用いたＵ−Ｐｕ混合酸化物の熱曲線の例を図６に示す。試料のＰｕ濃度は２９．５％、Ｏ／Ｍ＝２．００である。
【００１８】
両者を対比すると、明らかな相違が認められる。Ｕ−Ｐｕ混合酸化物では、前述のように（図３参照）固相温度と液相温度の２点がある。まず固相温度に着目すると、図５のタングステン−レニウム合金製試料容器（本発明品）を用いての測定では変曲点が分かるが、図６のタングステン製試料容器（従来品）を用いての測定では、固相温度が本当にあるのかどうかが分からないほど微妙な変化となっている。また液相温度については、図５のタングステン−レニウム合金製試料容器（本発明品）での測定の方が４０℃程度低く液相温度が観測されており、これも試料容器の構成材を変更し試料容器との反応による熱曲線変化を除去した成果である。
【００１９】
融点測定後の試料の金相観察結果を図７に示す。Ａはタングステン−レニウム合金製試料容器（本発明品）による融点測定試料であり、Ｂはタングステン製試料容器（従来品）による融点測定試料である。白色の部分が反応により容器構成材が混入した箇所を示している。明らかにタングステン−レニウム合金製試料容器（本発明品）を用いた場合は試料容器構成材の混入が殆ど生じていないことが分かる。
【００２０】
本発明で用いるタングステン−レニウム合金は、従来用いられていたタングステンよりも若干融点が低いが、Ｕ−Ｐｕ混合酸化物を測定する上では、タングステン９０％−レニウム１０％であれば特に問題はない。なお、本発明に係る試料容器は、Ｕ−Ｐｕ混合酸化物（Ｐｕ濃度が３０％程度のもの）と同程度以上の酸化力のある高融点材料の融点測定にも使用可能であることはいうまでもない。また、タングステン−レニウム合金製試料容器はタングステン製試料容器に比べて高価であるから、試料の性状に応じて使い分けることが望ましい。
【００２１】
【発明の効果】
本発明は上記のように、タングステン−レニウム合金製の融点測定用試料容器であるから、試料がＵ−Ｐｕ混合酸化物（例えばＰｕ濃度：３０％程度、Ｏ／Ｍ：２．００付近）であっても、容器構成材との酸化反応が低減し、そのため熱曲線の形状が安定化し且つ良好になり、熱曲線の解析が行い易くなる。その結果、燃料設計の観点から重要性の高いＯ／Ｍ＝２．００〜１．９８付近の融点の従来方法よりも正確な信頼性の高い測定が可能となる。
【図面の簡単な説明】
【図１】酸化ウランのサーマルアレスト法による測定結果の一例を示すグラフ。
【図２】酸化ウランを試料とする場合の理想的な熱曲線を示す模式図。
【図３】Ｕ−Ｐｕ混合酸化物を試料とする場合の理想的な熱曲線を示す模式図。
【図４】融点測定用試料容器の一例を示す断面図。
【図５】本発明品を用いたＵ−Ｐｕ混合酸化物の熱曲線を示すグラフ。
【図６】従来品を用いたＵ−Ｐｕ混合酸化物の熱曲線を示すグラフ。
【図７】融点測定後の試料の金相観察結果を示す図。
【符号の説明】
１０ 円筒部
１２ 底蓋
１４ 上蓋
１６ 凹部[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a heat-resistant sample container for measuring the melting point of MOX fuel by a thermal arrest method. More specifically, the present invention relates to a melting point measurement sample container made entirely of a tungsten-rhenium alloy. The present invention is particularly useful for measuring the melting point of U-Pu mixed oxides with high Pu enrichment and high O / M.
[0002]
[Prior art]
[Patent Document 1]
Japanese Patent Laid-Open No. 2002-296206
MOX fuel (uranium-plutonium mixed oxide) is used in the fast breeder reactor. This is a solid solution of uranium oxide (UO 2 ) and plutonium oxide (PuO 2 ). Uranium oxide (UO 2 ) and plutonium oxide (PuO 2 ) have the same crystal structure and are dissolved in the entire composition range. In the mixed oxide, MO 2 ± x (M = Pu + U) is possible, and a wide single-phase region exists. Here, the ratio of oxygen to heavy metal is called O / M (= 2 ± x), and the physical properties change depending on the degree of deviation from the stoichiometric ratio of 2.0. It is said that O / M = 1.99 to 1.95 is often used as the MOX fuel.
[0004]
By the way, the melting temperature of uranium oxide (UO 2 ) is around 2840 ° C., the melting temperature of plutonium oxide (PuO 2 ) is around 2390 ° C., and in the case of a mixed oxide, it takes a value between the two depending on the composition. . Also, the melting temperature varies depending on O / M. Furthermore, as the combustion proceeds, the melting point decreases with the accumulation of fission products (FP). As can be seen from the above, accurate measurement of the melting point is extremely important for the development and production of nuclear fuel.
[0005]
Conventionally, the thermal arrest method has been used to measure the melting point of nuclear fuel materials. This is a change in the thermal curve in which the temperature rises stagnate due to the latent heat (melting endotherm) when the sample is melted by placing the container enclosing the measurement sample in the heating furnace and heating the sample while measuring the temperature. Is a method for obtaining the melting point of the sample by reading. To keep the inflection point reading error as low as possible, measure the temperature of the sample container at the same time as measuring the temperature of the sample, plot the difference between the reference and sample temperature data using the container temperature data as a reference, and plot the differential heat A method for obtaining the melting point of a sample by reading the inflection point of the curve has also been proposed (see Patent Document 1).
[0006]
By the way, as described above, some nuclear fuel materials serving as samples for measuring the melting point have melting points exceeding 2800 ° C. Therefore, a tungsten container is conventionally used as a sample container.
[0007]
[Problems to be solved by the invention]
However, when attempting to measure the melting point of MOX fuel, there is a problem that the shape of the heat curve is very bad and unstable, making analysis difficult. In particular, for MOX fuel with a Pu concentration of about 30%, accurate data with high reliability is obtained even when the melting point is measured in the vicinity of O / M = 2.00 to 1.98, which is required for fuel design. It was difficult to get. As described above, in the conventional method, the reason why the shape of the heat curve is very bad and unstable and the analysis becomes difficult has not been elucidated.
[0008]
It is an object of the present invention to suppress the reaction between oxygen in the MOX fuel and the sample container, to reduce the instability of the thermal curve when the temperature rise is stagnated, and to improve the reliability of the melting point measurement of the MOX fuel. A sample container is provided. Another object of the present invention is to provide a U-Pu mixed oxide of O / M = 2.00 to 1.98 in a MOX fuel having a Pu concentration of 30% or less, which is particularly important from the viewpoint of fuel design. An object of the present invention is to provide a melting point measurement sample container capable of accurately measuring the melting point with high reliability.
[0009]
[Means for Solving the Problems]
After the MOX fuel (U-Pu mixed oxide) was sealed in a tungsten sample container and the melting point was measured by the thermal arrest method, the gold phase of the sample was observed. As a result, a lot of tungsten was mixed in the sample. Turned out to be. The reason why tungsten is mixed in the sample is that oxygen contained in the MOX fuel reacts with tungsten, which is a constituent material of the sample container, and the oxygen potential (ease of oxidation) of the MOX fuel and the tungsten sample container. This is probably because the tungsten sample container is higher.
[0010]
The exchange of oxygen between the MOX fuel and tungsten, which is a sample container constituent material, may have an influence on the measurement, and it was speculated that this increased measurement instability. As a result of intensive research, the present inventors have found that the reason why the shape of the heat curve is very poor and the analysis becomes difficult in the prior art is that the oxygen contained in the U-Pu mixed oxide and the sample container This is because the component tungsten reacts and the heat generated during the reaction occurs simultaneously with the melting endotherm during the melting of the sample, resulting in an unstable heating curve. I found out. This is a phenomenon that always occurs when a tungsten sample container is used to measure the melting point of a U-Pu mixed oxide having a Pu concentration of about 30% and an O / M of around 2.00. The present invention has been made based on the knowledge of the mechanism for the deterioration of the heat curve shape.
[0011]
It has been found that the reaction between oxygen in the U-Pu mixed oxide and the tungsten sample container can be reduced by lowering the O / M. Specifically, in the U-Pu mixed oxide having a Pu concentration of about 30%, the O / M at which the above phenomenon is not observed is approximately 1.94 or less. However, it is impossible to predict the melting point in the vicinity of O / M = 2.00 to 1.98, which is necessary for fuel design and the like. Therefore, some countermeasure is required.
[0012]
The present invention, which can solve such problems, is a sample container for enclosing MOX fuel and measuring the melting point by the thermal arrest method, and is a sample container for measuring the melting point of MOX fuel made entirely of a tungsten-rhenium alloy. is there. Typically, the MOX fuel as a measurement sample is a U-Pu mixed oxide having a Pu concentration of about 30% (for example, about 30 to 29%) and O / M = 2.00 to 1.95. The container-constituting tungsten-rhenium alloy is composed of 90% tungsten-10% rhenium. In general, the Pu concentration is 30 to 0%, and the present invention can be used to measure the melting point of MOX fuel with 30% Pu or less.
[0013]
DETAILED DESCRIPTION OF THE INVENTION
The method for measuring the melting point may be basically the same as that of the prior art. When the sample is melted by placing the container enclosing the measurement sample in a heating furnace and raising the temperature while measuring the temperature, This is a thermal arrest method in which the temperature rise is stagnated due to the latent heat (melting endotherm) and the temperature rises again when melting is completed, and the melting point of the sample is obtained from the analysis of the heat curve.
[0014]
FIG. 1 shows an example of the results obtained by measuring uranium oxide (UO 2 ) in a tungsten sample container. In the case of uranium oxide, there is no reaction with tungsten as the container constituent material. In the case of uranium oxide, since the solid phase temperature and the liquid phase temperature are observed as one point (the same temperature), the stagnation of the temperature rise can be clearly identified. Therefore, a thermal curve as schematically shown in FIG. 2 is obtained. A specific analysis method obtains the intersection of the thermal curve immediately before the start of thermal arrest and the thermal curve while the thermal arrest appears, and uses it as the melting point.
[0015]
However, in the case of MOX fuel, since the solid phase temperature and the liquid phase temperature are observed as two points (different temperatures), the stagnation of the temperature rise is not necessarily clear. FIG. 3 schematically shows a heat curve in an ideal case. Therefore, in such a case as well, the melting point can basically be obtained from the inflection point of the thermal curve.
[0016]
【Example】
FIG. 4 is a cross-sectional view showing an embodiment of a sample container for melting point measurement according to the present invention. The sample container has a structure in which a
[0017]
An example of the thermal curve of the U-Pu mixed oxide using such a sample container made of tungsten-rhenium alloy is shown in FIG. The Pu concentration of the sample is 29.9% and O / M = 2.00. For comparison, FIG. 6 shows an example of a thermal curve of a U-Pu mixed oxide using a conventional tungsten sample container. The Pu concentration of the sample is 29.5% and O / M = 2.00.
[0018]
When the two are contrasted, a clear difference is observed. In the U-Pu mixed oxide, as described above (see FIG. 3), there are two points: a solid phase temperature and a liquid phase temperature. First, paying attention to the solid phase temperature, the inflection point can be found in the measurement using the tungsten-rhenium alloy sample container (product of the present invention) in FIG. 5, but using the tungsten sample container (conventional product) in FIG. In this measurement, the change is so subtle that it is unknown whether the solid phase temperature really exists. As for the liquid phase temperature, the liquid phase temperature was observed to be lower by about 40 ° C. in the tungsten-rhenium alloy sample container (product of the present invention) in FIG. 5, and this also changed the constituent materials of the sample container. This is the result of removing the heat curve change due to the reaction with the sample container.
[0019]
The gold phase observation result of the sample after melting | fusing point measurement is shown in FIG. A is a melting point measurement sample using a tungsten-rhenium alloy sample container (product of the present invention), and B is a melting point measurement sample using a tungsten sample container (conventional product). The white part has shown the location where the container constituent material mixed by reaction. Obviously, when a sample container made of tungsten-rhenium alloy (product of the present invention) is used, the sample container constituent material is hardly mixed.
[0020]
The tungsten-rhenium alloy used in the present invention has a slightly lower melting point than that of conventionally used tungsten. However, when measuring U-Pu mixed oxide, there is no particular problem if tungsten is 90% -
[0021]
【The invention's effect】
Since the present invention is a sample container for measuring the melting point made of a tungsten-rhenium alloy as described above, the sample is a U-Pu mixed oxide (for example, Pu concentration: about 30%, O / M: around 2.00). Even if it exists, the oxidation reaction with the container constituent material is reduced, so that the shape of the heat curve is stabilized and improved, and the analysis of the heat curve is facilitated. As a result, more accurate and reliable measurement of the melting point near O / M = 2.00 to 1.98, which is highly important from the viewpoint of fuel design, is possible.
[Brief description of the drawings]
FIG. 1 is a graph showing an example of a measurement result of uranium oxide by a thermal arrest method.
FIG. 2 is a schematic diagram showing an ideal thermal curve when uranium oxide is used as a sample.
FIG. 3 is a schematic diagram showing an ideal thermal curve when a U-Pu mixed oxide is used as a sample.
FIG. 4 is a sectional view showing an example of a melting point measurement sample container.
FIG. 5 is a graph showing a thermal curve of a U-Pu mixed oxide using the product of the present invention.
FIG. 6 is a graph showing a thermal curve of a U-Pu mixed oxide using a conventional product.
FIG. 7 is a view showing a gold phase observation result of a sample after melting point measurement.
[Explanation of symbols]
10
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| JP2003173954A JP3836089B2 (en) | 2003-06-18 | 2003-06-18 | Sample container for melting point measurement of MOX fuel |
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| JP2003173954A JP3836089B2 (en) | 2003-06-18 | 2003-06-18 | Sample container for melting point measurement of MOX fuel |
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| CN108318367A (en) * | 2017-12-29 | 2018-07-24 | 中核四0四有限公司 | In a kind of MOX pellets oxygen metallic atom than analysis method |
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| JP4604154B2 (en) * | 2007-01-11 | 2010-12-22 | 独立行政法人 日本原子力研究開発機構 | MOX fuel melting point measurement sample |
| DE102013102088B3 (en) * | 2013-03-04 | 2014-07-17 | Netzsch-Gerätebau GmbH | Method and device for material analysis |
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