JP3508008B2 - Method for producing Li2O microspheres for tritium breeding - Google Patents
Method for producing Li2O microspheres for tritium breedingInfo
- Publication number
- JP3508008B2 JP3508008B2 JP24034597A JP24034597A JP3508008B2 JP 3508008 B2 JP3508008 B2 JP 3508008B2 JP 24034597 A JP24034597 A JP 24034597A JP 24034597 A JP24034597 A JP 24034597A JP 3508008 B2 JP3508008 B2 JP 3508008B2
- Authority
- JP
- Japan
- Prior art keywords
- microspheres
- gel
- dropping
- solution
- producing
- 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
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
- Y02E30/10—Nuclear fusion reactors
-
- 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
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- Manufacturing Of Micro-Capsules (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Description
【０００１】[0001]
【発明の属する技術分野】本発明は核融合炉のトリチウ
ム増殖材であるＬｉ2 Ｏ微小球を、Ｌｉ2 ＣＯ3を原料
として湿式法により製造するＬｉ2 Ｏ微小球の製造方法
に関するものである。TECHNICAL FIELD The present invention relates to a Li 2 O microspheres is tritium breeder nuclear fusion reactor, a method of manufacturing a Li 2 O microspheres prepared by a wet method Li 2 CO 3 as a raw material .
【０００２】[0002]
【従来の技術】Ｌｉ2 ＣＯ3 を原料とした湿式法による
Ｌｉ2 Ｏ微小球の製造方法は、図３（ａ）〜（ｇ）に示
すように滴下原液調整から焼結に至る各工程により構成
されている。 2. Description of the Related Art A method of manufacturing Li 2 O microspheres by a wet method using Li 2 CO 3 as a raw material is carried out by each step from adjustment of a dropping stock solution to sintering as shown in FIGS. It is configured.
【０００３】かかる製造方法においては、図３（ａ）
（ｂ）に示すように、アセトン中でゲル化するポリビニ
ルアルコール等の高分子化合物の水溶液とＬｉ2 ＣＯ3
粉末とを混合して滴下原液を作製し、この滴下原液を同
図（ｃ）に示すように、アセトン中に滴下しゲル球を得
る。そして、同図（ｄ）の工程にて乾燥させた後、同図
（ｅ）に示すように、このゲル球を熱処理すると高分子
化合物は除去され、Ｌｉ2 ＣＯ3 微小球となる。つい
で、同図（ｆ）に示すように、このＬｉ2 ＣＯ3 微小球
を真空中で熱分解することによりＬｉ2 Ｏ微小球に変換
し、同図（ｇ）に示すようにさらに加熱を続けることに
よりＬｉ2 Ｏ微小球焼結体を得る。In such a manufacturing method, as shown in FIG.
As shown in (b), an aqueous solution of a polymer compound such as polyvinyl alcohol that gels in acetone and Li 2 CO 3
The powder and the powder are mixed to prepare a dropping stock solution, and the dropping stock solution is dropped into acetone to obtain gel spheres as shown in FIG. Then, after being dried in the step of FIG. 3D, as shown in FIG. 3E, the gel spheres are heat-treated to remove the polymer compound and become Li 2 CO 3 microspheres. Then, as shown in FIG. 6F, the Li 2 CO 3 microspheres are thermally decomposed in vacuum to be converted into Li 2 O microspheres, and further heating is continued as shown in FIG. Thus, a Li 2 O microsphere sintered body is obtained.
【０００４】[0004]
【発明が解決しようとする課題】しかしながら、上記従
来の熱分解工程では、微小球表層が始めに熱分解され、
熱分解後も加熱を受け続けることになるため、熱分解に
より生じた微小球表層部のＬｉ2 Ｏ粒子同士の結合が進
み、微小球表面の開口部は狭小化あるいは減少する。ま
た、熱分解が進行するにつれて、熱分解反応部は微小球
中心部へと移行していくため、反応部から発生したＣＯ
2 は次第に微小球外部へ抜け出にくくなってゆき、その
結果、上記従来の熱分解方法では熱分解完了までに６０
時間以上の長時間を要していた。すなわち、この従来の
長時間の熱分解は、熱分解生成物であるＬｉ2 Ｏのその
後の焼結特性を低下させ、また製造コストを増加させる
という問題がある。However, in the above conventional thermal decomposition step, the surface of the microspheres is first thermally decomposed,
Since the particles continue to be heated even after pyrolysis, the Li 2 O particles in the surface layer of the microspheres produced by the pyrolysis are bonded to each other, and the openings on the surface of the microspheres are narrowed or reduced. Further, as the thermal decomposition progresses, the thermal decomposition reaction part moves to the central part of the microsphere, so that the CO generated from the reaction part
2 gradually became difficult to escape to the outside of the microsphere, and as a result, the above-mentioned conventional thermal decomposition method resulted in 60
It took a long time, more than an hour. That is, this conventional long-time thermal decomposition has a problem that the subsequent sintering characteristics of Li 2 O, which is a thermal decomposition product, deteriorates and the manufacturing cost increases.
【０００５】本発明は叙上の如き実状に対処し、上記熱
分解工程時間を短縮することにより、上記Ｌｉ2 Ｏ微小
球の焼結特性の向上を図ると共に、製造コストを低減す
ることを目的とするものである。The present invention aims to improve the sintering characteristics of the Li 2 O microspheres and reduce the manufacturing cost by coping with the actual situation as described above and shortening the time for the thermal decomposition process. It is what
【０００６】[0006]
【課題を解決するための手段】すなわち、上記目的に適
合する本発明のトリチウム増殖用Ｌｉ2 Ｏ微小球の製造
方法は、ポリビニルアルコール等のゲル媒体の水溶液中
にＬｉ2 ＣＯ3 の粉末を混合して滴下原液を作製し、こ
の滴下原液をアセトン等のゲル化材の液中に滴下し上記
Ｌｉ2 ＣＯ3 を含有するゲル球を得、このＬｉ2 ＣＯ3
を含有するゲル球から上記ゲル媒体を除去してＬｉ2 Ｃ
Ｏ3 の微小球となし、このＬｉ2 ＣＯ3の微小球を熱分
解することによりＬｉ2 Ｏの微小球を得るＬｉ2 Ｏ微小
球の製造方法において、上記滴下原液中に加熱により蒸
発飛散する多数の微細な繊維状化合物を添加して均一分
散させる一方、この滴下原液によって上記Ｌｉ2 ＣＯ3
を含有するゲル球を作製し、このＬｉ2 ＣＯ3 を含有す
るゲル球を熱処理することにより上記ゲル媒体と繊維状
化合物とを蒸発飛散させてＬｉ2 ＣＯ3 の微小球を形成
すると共に、この繊維化合物の蒸発飛散により上記Ｌｉ
2 ＣＯ3 微小球に、球の表面を介し内部から外部に連通
する細孔を形成せしめ、この細孔を有するＬｉ2 ＣＯ3
微小球を熱分解することにより上記Ｌｉ2 Ｏの微小球を
得ることを特徴とする。また、上記繊維状化合物として
は、直径１０〜１００μｍ、長さ１０〜１０００μｍの
ものが適当である。[Means for Solving the Problems] That is, the method for producing Li 2 O microspheres for tritium breeding according to the present invention, which is suitable for the above object, comprises mixing Li 2 CO 3 powder into an aqueous solution of a gel medium such as polyvinyl alcohol. to prepare a dropping stock, the dropping stock obtain a gel spheres containing the Li 2 CO 3 was added dropwise into the liquid gelling materials such as acetone, the Li 2 CO 3
And removing the gel medium from the gel spheres containing Li 2 C
O 3 microspheres and without, in the manufacturing method of the Li 2 O microspheres to obtain a Li 2 O of microspheres by pyrolysis of microspheres of the Li 2 CO 3, evaporated scattered by heating during the dropping stock While a large number of fine fibrous compounds were added and uniformly dispersed, the above-mentioned Li 2 CO 3 was added by this dropping stock solution.
The gel spheres containing Li 2 CO 3 are prepared, and the gel spheres containing Li 2 CO 3 are heat-treated to evaporate and disperse the gel medium and the fibrous compound to form Li 2 CO 3 microspheres. Due to the evaporation and scattering of the fiber compound, the above Li
2 CO 3 microspheres are formed with pores communicating from the inside to the outside through the surface of the sphere, and the Li 2 CO 3 having the pores is formed.
It is characterized in that the above-mentioned Li 2 O microspheres are obtained by thermally decomposing the microspheres. As the fibrous compound, those having a diameter of 10 to 100 μm and a length of 10 to 1000 μm are suitable.
【０００７】[0007]
【作用】Ｌｉ2 Ｏ微小球の製造において、熱分解反応を
速やかに進行させるためには、熱分解により発生する気
体、すなわちＣＯ2 の除去を円滑に行う必要がある。す
なわち、上記本発明のＬｉ2 Ｏ微小球の製造方法におい
ては、熱分解の前工程である仮焼工程でＬｉ2 ＣＯ3 微
小球の内部から表面まで繋がる細孔を形成させ、熱分解
により発生気体であるＣＯ2 を、この細孔を通じて速や
かに微小球外部に流出させることが可能であり、これに
より上記熱分解反応を速やかに進行させて熱分解時間を
短縮し、Ｌｉ2 Ｏ微小球の焼結特性の向上と製造コスト
の低減とを併せて実現することが可能である。In the production of Li 2 O microspheres, it is necessary to smoothly remove the gas generated by thermal decomposition, that is, CO 2 in order to promote the thermal decomposition reaction quickly. That is, in the above-described method for producing Li 2 O microspheres of the present invention, pores that connect from the inside to the surface of the Li 2 CO 3 microspheres are formed in the calcination step that is a pre-step of thermal decomposition, and are generated by thermal decomposition. the CO 2 is a gas, it is possible to quickly flow out in microspheres outside through the pores, thereby promptly proceeded the pyrolysis reaction reduces the cracking time, the Li 2 O microspheres It is possible to realize both improvement of sintering characteristics and reduction of manufacturing cost.
【０００８】[0008]
【発明の実施の形態】以下さらに添付図面を参照して、
本発明の実施の形態を説明する。BEST MODE FOR CARRYING OUT THE INVENTION With reference to the accompanying drawings,
An embodiment of the present invention will be described.
【０００９】図１は本発明実施形態のトリチウム増殖用
Ｌｉ2 Ｏ微小球の製造方法を示すチャート図である。す
なわち、上記本発明実施形態のＬｉ2 Ｏ微小球の製造方
法は、同図（ａ）〜（ｇ）に示すように滴下原液調整か
ら焼結に至る各工程により構成される。FIG. 1 is a chart showing the method for producing tritium breeding Li 2 O microspheres according to an embodiment of the present invention. That is, the method for producing Li 2 O microspheres of the above-described embodiment of the present invention is configured by the steps from the preparation of the dropping stock solution to the sintering, as shown in FIGS.
【００１０】かかる製造方法においては、まず同図
（ａ）（ｂ）に示すように、ゲル化材であるアセトン中
でゲル化するゲル媒体、すなわちポリビニルアルコール
等高分子化合物の水溶液と、Ｌｉ2 ＣＯ3 の粉末とを混
合して滴下原液を作製する。次いで、この滴下原液を同
図（ｃ）に示すように、振動ノズルにより上記アセトン
中に滴下し、同図（ｄ）の乾燥工程を経てＬｉ2 ＣＯ3
を含有するゲル球を得る。In such a manufacturing method, first, as shown in FIGS. 3A and 3B, a gel medium that gels in acetone, which is a gelling material, that is, an aqueous solution of a polymer compound such as polyvinyl alcohol, and Li 2 A CO 3 powder is mixed to prepare a stock solution for dropping. Then, as shown the dropping stock in FIG (c), the vibrating nozzle and dropped into the acetone, Li 2 CO 3 with a drying step in the (d) of FIG
To obtain gel spheres containing
【００１１】この場合、本発明では図１（ｂ）に示すよ
うに、上記滴下原液中に、２００℃〜５００℃程度の加
熱により蒸発飛散する多数の微細な繊維状化合物を添加
して均一に分散させると共に、この滴下原液によって上
記Ｌｉ2 ＣＯ3 を含有するゲル球を作製し、このＬｉ2
ＣＯ3 を含有するゲル球を同図（ｅ）に示すように熱処
理（仮焼）することにより上記ゲル媒体と繊維状化合物
とを蒸発飛散させてＬｉ2 ＣＯ3 の微小球を形成する。In this case, according to the present invention, as shown in FIG. 1 (b), a large number of fine fibrous compounds which evaporate and scatter by heating at about 200 ° C. to 500 ° C. are added to the above undiluted stock solution to make it uniform. with disperse, to prepare a gel spheres containing the Li 2 CO 3 by the dropwise stock, the Li 2
The gel spheres containing CO 3 are heat-treated (calcined) as shown in FIG. 3E to evaporate and scatter the gel medium and the fibrous compound to form Li 2 CO 3 microspheres.
【００１２】そして、この繊維状化合物の蒸発飛散によ
り上記Ｌｉ2 ＣＯ3 微小球に、球の表面を介し内部から
外部に連通する複数の細孔を形成せしめ、この細孔を有
するＬｉ2 ＣＯ3 微小球を同図（ｆ）に示すように熱分
解することにより上記Ｌｉ2Ｏの微小球を得る。さら
に、このＬｉ2 Ｏの微小球を、同図（ｇ）に示すように
焼結することによりＬｉ2 Ｏ粒子を得る。By vaporizing and scattering the fibrous compound, the Li 2 CO 3 microspheres are formed with a plurality of pores communicating from the inside to the outside through the surface of the sphere, and the Li 2 CO 3 having the pores is formed. The Li 2 O microspheres are obtained by thermally decomposing the microspheres as shown in FIG. Further, the Li 2 O microspheres are sintered as shown in FIG. 3G to obtain Li 2 O particles.
【００１３】上記加熱により蒸発飛散する微細な繊維状
化合物としては、下記の〜の全ての条件を満たすも
のが好適である。As the fine fibrous compound which evaporates and scatters upon heating, those which satisfy all of the following conditions (1) to (4) are suitable.
【００１４】 主構成元素がＣ、Ｈ、Ｏであり、その
他の元素としてはＬｉ以外含まない化合物、あるいは化
合物自体および熱処理による生成物がＬｉ2 ＣＯ3 やＬ
ｉ2 Ｏと反応せず、熱処理により容易に蒸発飛散するも
の。
形状は、直径が約１０〜１００μｍ、長さが約１０
〜１０００μｍであること。
アセトン中でゲル化する高分子化合物水溶液とＬｉ
2 ＣＯ3 粉末との混合液、およびアセトンに対してほと
んど溶解しない、あるいは分解しない性質を有するこ
と。
この繊維状化合物の具体例としては、セルロース繊維や
ビニロン繊維等がある。Compounds whose main constituent elements are C, H, and O and other elements other than Li, or the compounds themselves and the products of the heat treatment are Li 2 CO 3 and L
Those that do not react with i 2 O and easily evaporate and scatter by heat treatment. The shape is about 10 to 100 μm in diameter and about 10 in length.
~ 1000 μm. Aqueous solution of polymer compound that gels in acetone and Li
2 It has the property of being hardly dissolved or decomposed in a mixed solution with 2 CO 3 powder and acetone. Specific examples of the fibrous compound include cellulose fiber and vinylon fiber.
【００１５】このように、本発明実施形態の製造方法に
おいては、前記滴下原液中に上記繊維状化合物を添加す
ることにより乾燥ゲル球を熱処理（仮焼）し、高分子化
合物および繊維状化合物をＬｉ2 ＣＯ3 微小球から除去
した際に形成される空間部分によってＬｉ2 ＣＯ3 微小
球表面から中心部を繋ぐ直径数十μｍほどの細孔ができ
るようにしたものである。As described above, in the production method of the embodiment of the present invention, the dried gel spheres are heat-treated (calcined) by adding the above-mentioned fibrous compound to the above-mentioned dropping stock solution to remove the polymer compound and the fibrous compound. The space formed when the Li 2 CO 3 microspheres are removed forms pores with a diameter of several tens of μm that connect the surface of the Li 2 CO 3 microspheres to the center.
【００１６】図２に熱分解工程における微小球断面の模
式図を示す。図２（ａ）は従来の場合を、同図（ｂ）は
本発明による場合を表している。図２中の斜線部は熱分
解雰囲気（真空）との接触領域を、また図２（ｂ）の点
線で囲まれた部分は微小球に形成された細孔を示す。FIG. 2 shows a schematic view of a cross section of microspheres in the thermal decomposition step. FIG. 2A shows a conventional case, and FIG. 2B shows a case according to the present invention. The shaded area in FIG. 2 indicates the contact area with the pyrolysis atmosphere (vacuum), and the area surrounded by the dotted line in FIG. 2 (b) indicates the pores formed in the microsphere.
【００１７】上記本発明のように内部に細孔を形成した
Ｌｉ2 ＣＯ3 仮焼球を熱分解してＬｉ2 Ｏ微小球を作製
する場合、内部まで繋がった細孔よりＣＯ2 が除去され
るため短時間で熱分解が進むようになる。つまり図２の
（ａ）と（ｂ）を比較すると、本発明の（ｂ）の方が真
空との接触領域が広いため、細孔におけるＣＯ2 の移動
速度は従来の（ａ）に比べＬｉ2Ｏ粒子間を拡散してい
くよりも格段に速く、速やかに微小球外部へと除去され
る。したがって上記本発明の（ｂ）の方が熱分解反領域
が広く、単位時間の熱分解量が多くなることになる。When Li 2 CO 3 calcined spheres having pores formed therein are pyrolyzed to produce Li 2 O microspheres as in the present invention, CO 2 is removed from the pores connected to the inside. Therefore, thermal decomposition proceeds in a short time. In other words, comparing (a) and (b) of FIG. 2, since the contact area with the vacuum is wider in (b) of the present invention, the moving speed of CO 2 in the pores is lower than that in the conventional (a). It is much faster than the diffusion between 2 O particles and is rapidly removed to the outside of the microsphere. Therefore, the above-mentioned (b) of the present invention has a wider thermal decomposition reaction range, and the amount of thermal decomposition per unit time increases.
【００１８】また熱分解が進行するにしたがい斜線部で
囲まれた白色領域（未熱分解領域）からもＣＯ2 が発生
するが、従来の（ａ）よりも本発明の（ｂ）の方が一つ
一つの白色領域が小さく、白色領域中心から真空領域ま
での距離が短いため、熱分解により発生したＣＯ2 の真
空領域への移動は短時間になる。As the thermal decomposition progresses, CO 2 is also generated from the white area surrounded by the shaded area (non-thermally decomposed area). In the present invention (b), however, the CO 2 is generated rather than the conventional (a). Since each white region is small and the distance from the center of the white region to the vacuum region is short, the CO 2 generated by thermal decomposition moves to the vacuum region in a short time.
【００１９】このように本発明においては、微小球内部
における熱分解反応面の増加および熱分解時の生成気体
（ＣＯ2 ）の微小球外部への除去が容易になり、従来よ
りも短時間に熱分解反応を終了させることが可能であ
る。As described above, in the present invention, the increase of the thermal decomposition reaction surface inside the microspheres and the removal of the gas (CO 2 ) generated during the thermal decomposition to the outside of the microspheres are facilitated, and the time is shorter than before. It is possible to terminate the thermal decomposition reaction.
【００２０】（実施例１）以下に内部に細孔を形成した
Ｌｉ2 Ｏ微小球焼結体の作製実施例を示す。Example 1 An example of producing a Li 2 O microsphere sintered body having pores formed therein will be shown below.
【００２１】 原料にはＬｉ2 ＣＯ3 粉末、ポリビニ
ルアルコール、純水を用いた。またポリビニルアルコー
ルのゲル化材としてアセトンを使用した。繊維状化合物
にはセルロース繊維（直径３０μｍ、長さ８００μｍ）
を使用した。Li 2 CO 3 powder, polyvinyl alcohol, and pure water were used as raw materials. Acetone was used as a gelling agent for polyvinyl alcohol. Cellulose fiber (diameter 30 μm, length 800 μm) as fibrous compound
It was used.
【００２２】 はじめに純水とポリビニルアルコール
を混合、加熱溶解しポリビニルアルコール１０ｗｔ％水
溶液を調整した。次にこのポリビニルアルコール水溶液
とＬｉ2 ＣＯ3 粉末と純水を攪拌混合し滴下原液を調整
した。滴下原液の組成はＬｉ2ＣＯ3 ２６ｗｔ％、ポリ
ビニルアルコール５ｗｔ％とした。さらに滴下原液の２
ｖｏｌ％のセルロース繊維を滴下原液に添加し攪拌混合
した。First, pure water and polyvinyl alcohol were mixed and dissolved by heating to prepare a 10 wt% polyvinyl alcohol aqueous solution. Next, this polyvinyl alcohol aqueous solution, Li 2 CO 3 powder and pure water were stirred and mixed to prepare a dropping stock solution. The composition of the dropping stock solution was Li 2 CO 3 26 wt% and polyvinyl alcohol 5 wt%. Furthermore, 2 of undiluted solution
Vol% cellulose fiber was added to the dropping stock solution and mixed with stirring.
【００２３】 組成調整した滴下原液を温度−２０℃
のアセトンへ滴下した。アセトン中で滴下原液に含まれ
るポリビニルアルコールはゲル化し、その内部にＬｉ2
ＣＯ3粉末およびセルロース繊維が分散したゲル球が作
製される。ゲル球は滴下後アセトン（液温−２０℃）中
に１時間静置して熟成させた。
熟成後、ゲル球をアセトンから取り出し、大気中、
室温で、２４時間乾燥させて乾燥ゲル球とした。The composition of the stock solution for dropping was adjusted to a temperature of −20 ° C.
Was added dropwise to acetone. The polyvinyl alcohol contained in the undiluted solution in acetone gelled, and Li 2
Gel spheres are produced in which CO 3 powder and cellulose fibers are dispersed. After dropping, the gel spheres were left to stand in acetone (liquid temperature −20 ° C.) for 1 hour for aging. After aging, remove the gel spheres from acetone, and in the air,
It was dried at room temperature for 24 hours to give dried gel spheres.
【００２４】 乾燥ゲル球を大気中、４００℃、６時
間仮焼した。仮焼によりゲル球からポリビニルアルコー
ルおよびセルロースが除去され、Ｌｉ2 ＣＯ3 粉末より
構成される仮焼球となった。仮焼球内部には細孔が形成
されていた。
仮焼球を真空中、７００℃で３０時間加熱してＬｉ
2 ＣＯ3 を熱分解した。圧力は１０-2Ｔｏｒｒ以下とし
た。得られた熱分解球の相同定をＸＲＤにて実施したこ
とろＬｉ2 Ｏであることを確認した。
最後に熱分解球を真空中、１１００℃、４時間焼結
して直径１ｍｍのＬｉ2Ｏ微小球焼結体が得られた。The dried gel spheres were calcined in air at 400 ° C. for 6 hours. By calcination, polyvinyl alcohol and cellulose were removed from the gel spheres to obtain calcined spheres composed of Li 2 CO 3 powder. Pores were formed inside the calcined ball. The calcined ball is heated in vacuum at 700 ° C. for 30 hours to obtain Li.
2 CO 3 was pyrolyzed. The pressure was 10 -2 Torr or less. The phase of the resulting pyrolyzed sphere was identified by XRD, which confirmed that it was Li 2 O. Finally, the pyrolyzed spheres were sintered in vacuum at 1100 ° C. for 4 hours to obtain Li 2 O microsphere sintered bodies with a diameter of 1 mm.
【００２５】[0025]
【発明の効果】以上説明したように、本発明のトリチウ
ム増殖用Ｌｉ2 Ｏ微小球の製造方法は、ゲル媒体にＬｉ
2 ＣＯ3 粉末を混合した滴下原液中に、加熱により蒸発
飛散する多数の微細な繊維状化合物を添加して均一分散
させる一方、この滴下原液によって上記Ｌｉ2 ＣＯ3 を
含有するゲル球を作製し、このＬｉ2 ＣＯ3 を含有する
ゲル球を熱処理することにより上記ゲル媒体と繊維状化
合物とを蒸発飛散させてＬｉ2 ＣＯ3 の微小球を形成す
ると共に、この繊維状化合物の蒸発飛散により上記Ｌｉ
2 ＣＯ3 微小球に、球の表面を介し内部から外部に連通
する細孔を形成せしめ、この細孔を有するＬｉ2 ＣＯ3
微小球を熱分解することにより上記Ｌｉ2Ｏの微小球を
得るものであり、熱分解の前工程である仮焼工程でＬｉ
2 ＣＯ3 微小球の内部から表面まで繋がる細孔を形成さ
せ、熱分解による発生気体であるＣＯ2 を、この細孔を
通じて速やかに微小球外部に流出させることが可能であ
り、これにより上記熱分解反応を速やかに進行させて熱
分解時間を短縮し、Ｌｉ2 Ｏが受ける熱量を減少せしめ
てＬｉ2 Ｏ微小球の焼結特性の低下を抑制すると共に、
上記熱分解時間を短縮することにより製造コストの低減
を併せて実現するとの顕著な効果を奏するものである。As described above, the method for producing Li 2 O microspheres for breeding tritium according to the present invention uses Li as a gel medium.
A large number of fine fibrous compounds that evaporate and scatter by heating are added to a dropping stock solution mixed with 2 CO 3 powder to uniformly disperse the gel, and a gel sphere containing Li 2 CO 3 is prepared by the dropping stock solution. The gel spheres containing Li 2 CO 3 are heat-treated to evaporate and scatter the gel medium and the fibrous compound to form Li 2 CO 3 microspheres. Li
2 CO 3 microspheres are formed with pores communicating from the inside to the outside through the surface of the sphere, and the Li 2 CO 3 having the pores is formed.
The microspheres of Li 2 O are obtained by thermally decomposing the microspheres.
It is possible to form pores connecting from the inside of 2 CO 3 microspheres to the surface thereof, and to allow CO 2 which is a gas generated by thermal decomposition to quickly flow out of the microspheres through these pores. the decomposition reaction rapidly proceeded to reduce the thermal decomposition time, with and caused to decrease the amount of heat Li 2 O is subjected to suppress a decrease in the sintering characteristics of the Li 2 O microspheres,
By shortening the thermal decomposition time, it is possible to achieve a remarkable effect that the manufacturing cost is also reduced.
【図１】湿式造粒方による本発明実施形態のトリチウム
増殖用Ｌｉ2 Ｏ微小球の製造方法を示すチャート図であ
る。FIG. 1 is a chart showing a method for producing Li 2 O microspheres for tritium breeding according to an embodiment of the present invention by a wet granulation method.
【図２】熱分解工程における微小球断面の模式図であ
り、（ａ）は従来の場合を、（ｂ）は本発明による場合
を示している。FIG. 2 is a schematic view of a cross section of a microsphere in a thermal decomposition step, (a) showing a conventional case and (b) showing a case according to the present invention.
【図３】湿式造粒法による従来のＬｉ2 Ｏ微小球の製造
方法を示すチャート図である。FIG. 3 is a chart showing a conventional method for producing Li 2 O microspheres by a wet granulation method.
フロントページの続き (58)調査した分野(Int.Cl.7，ＤＢ名) G21B 1/00 Continuation of front page (58) Fields surveyed (Int.Cl. 7 , DB name) G21B 1/00
Claims (2)
溶液中にＬｉ2 ＣＯ3 の粉末を混合して滴下原液を作製
し、この滴下原液をアセトン等のゲル化材の液中に滴下
し上記Ｌｉ2 ＣＯ3 を含有するゲル球を得、このＬｉ2
ＣＯ3 を含有するゲル球から上記ゲル媒体を除去してＬ
ｉ2 ＣＯ3 の微小球となし、このＬｉ2 ＣＯ3 の微小球
を熱分解することによりＬｉ2 Ｏの微小球を得るＬｉ2
Ｏ微小球の製造方法において、上記滴下原液中に加熱に
より蒸発飛散する多数の微細な繊維状化合物を添加して
均一分散させる一方、この滴下原液によって上記Ｌｉ2
ＣＯ3 を含有するゲル球を作製し、このＬｉ2 ＣＯ3 を
含有するゲル球を熱処理することにより上記ゲル媒体と
繊維状化合物とを蒸発飛散させてＬｉ2 ＣＯ3 を含有す
る微小球を形成すると共に、この繊維化合物の蒸発飛散
により上記Ｌｉ2ＣＯ3 微小球に、球の表面を介し内部
から外部に連通する細孔を形成せしめ、この細孔を有す
るＬｉ2 ＣＯ3 微小球を熱分解することにより上記Ｌｉ
2 Ｏの微小球を得ることを特徴とするトリチウム増殖用
Ｌｉ2 Ｏ微小球の製造方法。1. A liquid solution of Li 2 CO 3 is mixed with an aqueous solution of a gel medium such as polyvinyl alcohol to prepare a stock solution for dropping, and the stock solution for dropping is dropped into a solution of a gelling agent such as acetone to prepare the above Li 2 solution. A gel sphere containing CO 3 is obtained, which Li 2
Removing the gel medium from gel spheres containing CO 3
i 2 CO 3 microsphere and without, obtain Li 2 O of microspheres by pyrolysis of microspheres of the Li 2 CO 3 Li 2
The method of manufacturing a O microspheres, while uniformly dispersed by adding a large number of fine fibrous compounds that evaporate scattered by heating during the dropping stock, the Li 2 This dropping stock
A gel sphere containing CO 3 is produced, and the gel sphere containing Li 2 CO 3 is heat-treated to evaporate and disperse the gel medium and the fibrous compound to form a microsphere containing Li 2 CO 3. At the same time, by vaporizing and scattering the fiber compound, the Li 2 CO 3 microspheres are formed with pores communicating from the inside to the outside through the surface of the sphere, and the Li 2 CO 3 microspheres having the pores are thermally decomposed. By doing the above
A method for producing Li 2 O microspheres for breeding tritium, which comprises obtaining 2 O microspheres.
ｍ、長さ１０〜１０００μｍのものからなる請求項１記
載のトリチウム増殖用Ｌｉ2 Ｏ微小球の製造方法。2. The fibrous compound has a diameter of 10 to 100 μm.
The method for producing Li 2 O microspheres for tritium breeding according to claim 1, wherein the method comprises m and a length of 10 to 1000 μm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24034597A JP3508008B2 (en) | 1997-08-20 | 1997-08-20 | Method for producing Li2O microspheres for tritium breeding |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24034597A JP3508008B2 (en) | 1997-08-20 | 1997-08-20 | Method for producing Li2O microspheres for tritium breeding |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH1164556A JPH1164556A (en) | 1999-03-05 |
| JP3508008B2 true JP3508008B2 (en) | 2004-03-22 |
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ID=17058114
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP24034597A Expired - Lifetime JP3508008B2 (en) | 1997-08-20 | 1997-08-20 | Method for producing Li2O microspheres for tritium breeding |
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| Country | Link |
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| CA3200272A1 (en) | 2015-12-16 | 2017-06-22 | 6K Inc. | Spheroidal dehydrogenated metals and metal alloy particles |
| AU2020264446A1 (en) | 2019-04-30 | 2021-11-18 | 6K Inc. | Mechanically alloyed powder feedstock |
| CA3153254A1 (en) | 2019-11-18 | 2021-06-17 | 6K Inc. | Unique feedstocks for spherical powders and methods of manufacturing |
| US11590568B2 (en) | 2019-12-19 | 2023-02-28 | 6K Inc. | Process for producing spheroidized powder from feedstock materials |
| KR20230029836A (en) | 2020-06-25 | 2023-03-03 | 6케이 인크. | Microcomposite alloy structure |
| KR20230073182A (en) | 2020-09-24 | 2023-05-25 | 6케이 인크. | Systems, devices and methods for initiating plasma |
| US11919071B2 (en) | 2020-10-30 | 2024-03-05 | 6K Inc. | Systems and methods for synthesis of spheroidized metal powders |
| US12040162B2 (en) | 2022-06-09 | 2024-07-16 | 6K Inc. | Plasma apparatus and methods for processing feed material utilizing an upstream swirl module and composite gas flows |
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