JPH0827228B2 - Method for measuring sinterability of uranium dioxide powder - Google Patents
Method for measuring sinterability of uranium dioxide powderInfo
- Publication number
- JPH0827228B2 JPH0827228B2 JP1049514A JP4951489A JPH0827228B2 JP H0827228 B2 JPH0827228 B2 JP H0827228B2 JP 1049514 A JP1049514 A JP 1049514A JP 4951489 A JP4951489 A JP 4951489A JP H0827228 B2 JPH0827228 B2 JP H0827228B2
- Authority
- JP
- Japan
- Prior art keywords
- dioxide powder
- uranium dioxide
- sinterability
- measuring
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- 239000000843 powder Substances 0.000 title claims description 42
- OOAWCECZEHPMBX-UHFFFAOYSA-N oxygen(2-);uranium(4+) Chemical compound [O-2].[O-2].[U+4] OOAWCECZEHPMBX-UHFFFAOYSA-N 0.000 title claims description 31
- FCTBKIHDJGHPPO-UHFFFAOYSA-N uranium dioxide Inorganic materials O=[U]=O FCTBKIHDJGHPPO-UHFFFAOYSA-N 0.000 title claims description 31
- 238000000034 method Methods 0.000 title claims description 10
- 238000007254 oxidation reaction Methods 0.000 claims description 19
- 230000003647 oxidation Effects 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000008188 pellet Substances 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000000977 initiatory effect Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 238000004438 BET method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
Classifications
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
Landscapes
- Monitoring And Testing Of Nuclear Reactors (AREA)
Description
【発明の詳細な説明】 （産業分野） 本発明は二酸化ウラン粉末の焼結性を測定する方法に
関する。TECHNICAL FIELD The present invention relates to a method for measuring the sinterability of uranium dioxide powder.
（従来技術とその問題点） 二酸化ウラン粉末の物性、特に焼結性を測定する方法
として、従来平均粒径（Fsss法等）及び比表面積（BET
法等）を測定する方法があつたが、粉末の重量を正確に
一定量秤量する必要がある等、自動化及びオンラインで
の測定には不適であつた。(Prior art and its problems) As a method for measuring the physical properties of uranium dioxide powder, particularly the sinterability, conventional average particle size (Fsss method, etc.) and specific surface area (BET
Method, etc.), but it was not suitable for automation and on-line measurement because it was necessary to accurately weigh a certain amount of powder.
また、これらの物性値は焼結性とある程度の相関はあ
るものの、これだけでは不充分であり、より相関性のあ
る指標が求められていた。Further, although these physical property values have a certain degree of correlation with the sinterability, this is not sufficient alone, and a more correlated index has been sought.
（発明の目的） 本発明者らは上記の従来方法の問題点を解決すべく、
種々検討した結果、一定条件下で加熱昇温した場合の二
酸化ウラン粉末の酸化開始温度が粉末の焼結性と極めて
良い相関にあることを見出し、この知見に基づいて本発
明を完成するに到つた。(Object of the Invention) In order to solve the above problems of the conventional method, the present inventors
As a result of various studies, it was found that the oxidation start temperature of the uranium dioxide powder when heated and heated under a certain condition has an extremely good correlation with the sinterability of the powder, and the present invention was completed based on this finding. Ivy.
（発明の構成） すなわち、本発明によれば、二酸化ウラン粉末を天び
ん上の耐熱耐酸化性皿に一様に載せ、該二酸化ウラン粉
末の上方から0.2〜5.0℃/mmの昇温速度に制御されたヒ
ーターで一様に該二酸化ウラン粉末を加熱し、二酸化ウ
ラン粉末の重量変化量を天びんで検知し、二酸化ウラン
粉末における単位時間あたりの重量増加量が規定値を超
えた時点の温度を読みとり、この温度に基づいて、二酸
化ウラン粉末の焼結性を測定する、二酸化ウラン粉末の
焼結性測定方法に構成されている。(Structure of the Invention) That is, according to the present invention, the uranium dioxide powder is uniformly placed on a heat-resistant and oxidation-resistant dish on a balance, and the temperature rising rate is controlled from above the uranium dioxide powder to 0.2 to 5.0 ° C / mm. The uranium dioxide powder is uniformly heated by the heater provided, the weight change amount of the uranium dioxide powder is detected by the balance, and the temperature at the time when the weight increase amount of the uranium dioxide powder per unit time exceeds the specified value is read. The method for measuring the sinterability of uranium dioxide powder is based on this temperature.
ここで、前記規定値とは、二酸化ウラン粉末の酸化が
開始されたと判断することができる値であり、この値
は、予め実験的に確認されている。本明細書において
は、二酸化ウラン粉末における単位時間あたり重量増加
量が前記規定値を超えた時点の温度を酸化開始温度と称
する。Here, the specified value is a value with which it can be determined that the oxidation of the uranium dioxide powder has started, and this value has been experimentally confirmed in advance. In the present specification, the temperature at which the weight increase amount of the uranium dioxide powder per unit time exceeds the specified value is referred to as the oxidation start temperature.
以下、本発明において、酸化開始温度に基づいて二酸
化ウラン粉末の焼結性を測定する構成とした理由を説明
する。The reason why the present invention is configured to measure the sinterability of the uranium dioxide powder based on the oxidation start temperature will be described below.
二酸化ウラン粉末を一定昇温速度で加熱する場合、第
１図に示すような重量変化を示すことが知られている。
第１図において、40〜80℃での微量な重量減少は、二酸
化ウラン粉末に吸着している水分の蒸発（脱着）による
ためであり、更に第二図に示すように100〜140℃付近で
の急激な重量増加は、二酸化ウラン粉末が空気中の酸素
と反応し、酸化が起こつているためである。したがっ
て、二酸化ウラン粉末における単位時間あたりの重量変
化量が規定値を超える程に急激であることをもって、二
酸化ウラン粉末の酸化が開始されたと判断することがで
きる。この酸化反応によりUO2粉末はU4O9又はU3O7のよ
うに高次の酸化物に移行する。本発明者らはこのときの
酸化開始温度は粉末により異なり、UO2ペレツトを製造
するときの焼結性と極めて良い相関にあることを発見し
たのである。It is known that when the uranium dioxide powder is heated at a constant heating rate, the weight change as shown in FIG. 1 is exhibited.
In Fig. 1, the slight weight loss at 40 to 80 ° C is due to the evaporation (desorption) of the water adsorbed on the uranium dioxide powder. The rapid increase in the weight is due to the fact that the uranium dioxide powder reacts with oxygen in the air to cause oxidation. Therefore, when the amount of change in weight of the uranium dioxide powder per unit time is so rapid as to exceed the specified value, it can be determined that the oxidation of the uranium dioxide powder has started. By this oxidation reaction, the UO 2 powder is transformed into a higher-order oxide such as U 4 O 9 or U 3 O 7 . The present inventors have found that the oxidation initiation temperature at this time varies depending on the powder and has a very good correlation with the sinterability when producing UO 2 pellets.
このように、酸化開始温度を測定する本発明方法で
は、第３図に示すように、まずUO2粉末を１〜200g天び
ん上の例えば、ステンレス製皿に一様に載せる。このと
き、UO2粉末は正確に一定量をとる必要がなく、おおよ
その量でよく、好ましくは10〜30gが適当である。重量
が多過ぎても、少な過ぎても再現性の点で問題となる。Thus, in the method of the present invention for measuring the oxidation start temperature, as shown in FIG. 3, first, UO 2 powder is evenly placed on, for example, a stainless steel dish on a balance of 1 to 200 g. At this time, the UO 2 powder does not have to be taken in an exact fixed amount, and may be an approximate amount, preferably 10 to 30 g. If the weight is too large or too small, reproducibility becomes a problem.
次に、点びん上の二酸化ウラン粉末を上方からできる
だけ一様に加熱できるセラミツクヒーターで、0.2〜5.0
℃/mの一定昇温速度で加熱する。一定昇温速度が0.2℃/
mm未満の場合には、測定時間が長くなる等の問題があ
り、また一定昇温速度が5.0℃/mmを超えた場合には酸化
開始温度の再現性の点で問題となる。好ましくは1.5〜
2.5℃/mmの間の一定昇温速度で加熱するのが適当であ
る。Next, with a ceramic heater that can heat the uranium dioxide powder on the point bottle as evenly as possible from above, 0.2 ~ 5.0
Heat at a constant rate of temperature rise of ° C / m. Constant heating rate of 0.2 ° C /
When it is less than mm, there is a problem that the measurement time becomes long, and when the constant heating rate exceeds 5.0 ° C./mm, there is a problem in reproducibility of the oxidation start temperature. Preferably 1.5 to
It is suitable to heat at a constant heating rate between 2.5 ° C / mm.
このような本発明方法で測定された二酸化ウラン粉末
の酸化開始温度は、第２図に示すように、UO2ペレツト
の焼結性と極めて良い相関がみられ、従来の平均粒径と
焼結性又は比表面積と焼結性の相関よりはさらに良い相
関性が得られている。The oxidation initiation temperature of the uranium dioxide powder measured by the method of the present invention has a very good correlation with the sinterability of UO 2 pellets as shown in FIG. A better correlation is obtained than the correlation between the property or the specific surface area and the sinterability.
次に本発明を実施例により具体的に説明するが、以下
の実施例によつて本発明の範囲は限定されるものではな
い。Next, the present invention will be specifically described by way of examples, but the scope of the present invention is not limited by the following examples.
実施例 焼結性の異なる６種類のUO2粉末について、次の方法
でそれぞれ酸化開始温度を測定した。Example The oxidation start temperature was measured for each of six types of UO 2 powders having different sinterability by the following method.
約20gのUO2粉末を天びん上のステンレス製皿に一様に
載せ、上方よりセラミツクヒーターを用い、２℃/mmの
昇温速度でUO2粉末を一様に加熱した。１分間当たりの
重量増加が2mgを越えた時点の温度をそれぞれ酸化開始
温度とし、このときの粉末の温度を読みとつた。About 20 g of UO 2 powder was evenly placed on a stainless steel dish on a balance, and the ceramic heater was used to uniformly heat the UO 2 powder at a temperature rising rate of 2 ° C./mm. The temperature at which the weight increase per minute exceeded 2 mg was defined as the oxidation start temperature, and the temperature of the powder at this time was read.
このようにして得られた酸化開始温度と一定条件下で
製造したUO2ペレツトの焼結密度を第１表に示す。ま
た、これをグラフ化したものが第２図である。Table 1 shows the oxidation start temperature thus obtained and the sintering density of UO 2 pellets produced under certain conditions. Further, FIG. 2 is a graph of this.
（発明の効果） 本発明は上記構成をとることによつて次の効果を示
す。 (Effects of the Invention) The present invention has the following effects due to the above configuration.
（１） 二酸化ウラン粉末の酸化開始温度の測定が比較
的簡便にできるため、自動化が可能であり、UO2粉末製
造ラインでの工程管理に利用できる。(1) Since the oxidation start temperature of uranium dioxide powder can be measured relatively easily, it can be automated and can be used for process control in the UO 2 powder production line.
（２） UO2ペレツトには焼結密度の厳しい仕様（95±
1.5％）が定められているため、UO2ペレツトの焼結性と
極めて良い相関がみられる二酸化ウラン粉末の酸化開始
温度はUO2ペレツト製造上重要な特性値となりうる。(2) For UO 2 pellets, specifications with severe sintering density (95 ±
Since 1.5%) is defined, the oxidation start temperature of the uranium dioxide powder very good correlation with the sintering of UO 2 Peretsuto is observed can be a UO 2 Peretsuto producing important characteristic values.
第１図は昇温速度２℃/mmの一定条件で加熱したときの
温度と二酸化ウラン粉末（約20g）の重量変化量（ΔＧ
・ｇ）の関係を示すグラフ図、第２図は二酸化ウラン粉
末の酸化開始温度と焼結密度の関係を示すグラフ図、第
３図は本発明測定方法の装置概略図の１例図である。Figure 1 shows the temperature change and the weight change of uranium dioxide powder (about 20g) (ΔG
.G) is a graph showing the relationship, FIG. 2 is a graph showing the relationship between the oxidation start temperature of the uranium dioxide powder and the sintering density, and FIG. 3 is an example of an apparatus schematic view of the measuring method of the present invention. .
Claims (1)
性皿に一様に載せ、該二酸化ウラン粉末の上方から0.2
〜5.0℃/minの昇温速度に制御されたヒーターで一様に
該二酸化ウラン粉末を加熱し、該二酸化ウラン粉末の重
量変化量を天びんで検知し、該二酸化ウラン粉末におけ
る単位時間あたりの重量増加量が規定値を超えた時点の
温度を読みとり、この温度に基づいて、該二酸化ウラン
粉末の焼結性を測定することを特徴とする二酸化ウラン
粉末の焼結性測定方法。1. Uranium dioxide powder is evenly placed on a heat-resistant and oxidation-resistant dish on a balance, and 0.2% from above the uranium dioxide powder.
~ 5.0 ℃ / min heating the uranium dioxide powder uniformly with a heater controlled, the weight change amount of the uranium dioxide powder is detected by a balance, the weight of the uranium dioxide powder per unit time A method for measuring the sinterability of uranium dioxide powder, which comprises reading the temperature at the time when the amount of increase exceeds a specified value and measuring the sinterability of the uranium dioxide powder based on this temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1049514A JPH0827228B2 (en) | 1989-03-01 | 1989-03-01 | Method for measuring sinterability of uranium dioxide powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1049514A JPH0827228B2 (en) | 1989-03-01 | 1989-03-01 | Method for measuring sinterability of uranium dioxide powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02228592A JPH02228592A (en) | 1990-09-11 |
| JPH0827228B2 true JPH0827228B2 (en) | 1996-03-21 |
Family
ID=12833240
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1049514A Expired - Lifetime JPH0827228B2 (en) | 1989-03-01 | 1989-03-01 | Method for measuring sinterability of uranium dioxide powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0827228B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5251824B2 (en) * | 2009-10-22 | 2013-07-31 | 株式会社村田製作所 | Management method of sintered density of ceramic sintered body |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6142213B2 (en) | 2013-07-11 | 2017-06-07 | 株式会社Ｊｏｌｅｄ | ORGANIC EL ELEMENT AND METHOD FOR PRODUCING ORGANIC EL ELEMENT |
-
1989
- 1989-03-01 JP JP1049514A patent/JPH0827228B2/en not_active Expired - Lifetime
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6142213B2 (en) | 2013-07-11 | 2017-06-07 | 株式会社Ｊｏｌｅｄ | ORGANIC EL ELEMENT AND METHOD FOR PRODUCING ORGANIC EL ELEMENT |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH02228592A (en) | 1990-09-11 |
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