JPS63103858A - Manufacture of lithium oxide sintered body - Google Patents
Manufacture of lithium oxide sintered bodyInfo
- Publication number
- JPS63103858A JPS63103858A JP61251203A JP25120386A JPS63103858A JP S63103858 A JPS63103858 A JP S63103858A JP 61251203 A JP61251203 A JP 61251203A JP 25120386 A JP25120386 A JP 25120386A JP S63103858 A JPS63103858 A JP S63103858A
- Authority
- JP
- Japan
- Prior art keywords
- sintered body
- sintering
- li2o
- compact
- powder
- 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.)
- Pending
Links
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 title claims description 23
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 229910001947 lithium oxide Inorganic materials 0.000 title claims description 6
- 239000000843 powder Substances 0.000 claims description 23
- 238000005245 sintering Methods 0.000 claims description 17
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 16
- 239000011261 inert gas Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 description 20
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 description 17
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 9
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 239000011888 foil Substances 0.000 description 7
- 239000007789 gas Substances 0.000 description 7
- 229910052715 tantalum Inorganic materials 0.000 description 7
- 229910052697 platinum Inorganic materials 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 230000004927 fusion Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 3
- 229910052808 lithium carbonate Inorganic materials 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- YZCKVEUIGOORGS-NJFSPNSNSA-N Tritium Chemical compound [3H] YZCKVEUIGOORGS-NJFSPNSNSA-N 0.000 description 2
- 229910052722 tritium Inorganic materials 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- YQNQTEBHHUSESQ-UHFFFAOYSA-N lithium aluminate Chemical compound [Li+].[O-][Al]=O YQNQTEBHHUSESQ-UHFFFAOYSA-N 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 238000010186 staining Methods 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Abstract
(57)【要約】本公報は電子出願前の出願データであるた
め要約のデータは記録されません。(57) [Abstract] This bulletin contains application data before electronic filing, so abstract data is not recorded.
Description
【発明の詳細な説明】
〔発明の属する技術分野〕
この発明は、核融合炉のブランケット材等に用いられる
酸化リチウム焼結体の輿遣方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Technical field to which the invention pertains] The present invention relates to a method for transporting a sintered lithium oxide body used as a blanket material for a nuclear fusion reactor.
核融合炉のブランケット材の有力な候補である酸化リチ
ウム（以下の本文ではＬｉ２Ｏとする）は、通常Ｌｉ
２０の粉末を加圧成形し、それを焼結することによって
得られる。そして、トリチウムの増殖作用を高める観点
からはＬｉ ２０焼結体はできる限り密度が高く、表面
の清浄性（着色、汚損、不純物の付着などがないこと）
に優れたものが要求される。従来、検討されているＬｉ
２０圧粉体の焼結方法の特徴と、その問題点などは以
下の通りである。Lithium oxide (referred to as Li2O in the following text), which is a promising candidate for blanket material in fusion reactors, is usually Li
It is obtained by compacting a powder of No. 20 and sintering it. From the perspective of enhancing the multiplication effect of tritium, the Li 20 sintered body must have as high a density as possible, and the surface must be clean (no coloring, staining, adhesion of impurities, etc.).
excellence is required. Previously studied Li
The characteristics and problems of the sintering method for 20 green compacts are as follows.
（１，１Ｌｉ２０圧粉体をアルミナ基板などの上に載置
し、これをアルゴンガス雰囲気中で９０００〜１２００
”Ｃの温度で１〜４時間焼結する方法（焼結条件は以下
全て同様とする）：この方法は簡便であるが、焼結密度
の上昇が少なく、かつガス雰囲気中の不純物などの付着
により焼結体の表面が変色しやすいという問題がある。(Place a 1,1Li20 powder compact on an alumina substrate, etc., and heat it to a temperature of 9000 to 1200 in an argon gas atmosphere.
A method of sintering at a temperature of 1 to 4 hours at a temperature of There is a problem in that the surface of the sintered body tends to discolor due to this.
（２）！空中（１０〜１０ｔｏｒｒ）テ焼結ヲ行つ方法
：この方法によれば高い焼結密度が得られ、表面の清浄
性も向上する。しかし、真空中であるとＬｉ２Ｏ圧粉体
のＬｉが蒸発して重量減が生ずるとともに、Ｌｉ２Ｏに
含有される水酸化リチウム（ＬｉＯＨ）、 炭酸リチ
ウム（Ｌｉ２ＣＯ５）などが揮発して炉内を汚染すると
いう欠点がある。また、この方法は量産性の面で劣って
いる。(2)! Method of performing sintering in air (10 to 10 torr): This method provides a high sintering density and improves surface cleanliness. However, in a vacuum, Li in the Li2O powder compact evaporates, resulting in weight loss, and lithium hydroxide (LiOH), lithium carbonate (Li2CO5), etc. contained in Li2O volatilize and contaminate the inside of the furnace. There is a drawback. Moreover, this method is inferior in terms of mass productivity.
（３）白金（Ｐｔ）、 タンタル（Ｔａ）、＝、ケル
（Ｎｉ）。(3) Platinum (Pt), tantalum (Ta), Kel (Ni).
モリブデン（Ｍｏ）、 タングステン（Ｗ）の容器にＬ
ｉ２Ｏ圧粉体を収容し、これを密閉状態にしてアルゴン
ガスもしくは真空穴囲気で焼結する方法：Ｐｔ 、 Ｔ
ａ 容器を用い、密閉状態が完全であるならば、良好
なＬ ｉ ｚ Ｏ焼結体を得ることができる。しかし、
ともに高価な材料であり、容器の製作費も高くて経済的
に劣ることかつＴａはＬｉ２Ｏ中にご（わずかに含有さ
れるＬｉ ＯＨ，Ｌｉ ２ ＣＯ３によって激しい腐食
をうけ容器を繰返し使用することは不可能である。Ｎｉ
、Ｍｏ、ＷはＰｔ 、 Ｔａ より安価であるが、そ
れぞれＬｉｚＯと反応を起こし、清浄な表面を有する焼
結体を得ることは困難である。L in molybdenum (Mo) and tungsten (W) containers
A method of storing an i2O powder compact, sealing it, and sintering it in an argon gas or vacuum hole environment: Pt, T
If a container is used and the container is completely sealed, a good L iz O sintered body can be obtained. but,
Both are expensive materials, and the manufacturing cost of the container is high, making them economically inferior. Ta also suffers from severe corrosion due to the small amounts of LiOH and Li 2 CO3 contained in Li2O, making it difficult to use the container repeatedly. It's impossible.Ni
, Mo, and W are cheaper than Pt and Ta, but each reacts with LizO, making it difficult to obtain a sintered body with a clean surface.
ｆ４１ Ｐｔ 、 Ｔａの箔でＬｉ ｚ□圧粉体を完全
に覆い、それを密閉状態の容器に収容して焼結する方法
：この方法によれば極めて良好な特性を有するＬｉ２Ｏ
焼結体が得られる。しかし、前項（３）と同様の欠点を
有し、さらに異形の圧粉体ではこの方法の採用が困難で
ある。f41 A method of completely covering the Li z□ compact with Pt, Ta foil, storing it in a sealed container, and sintering it: This method produces Li2O, which has extremely good properties.
A sintered body is obtained. However, it has the same drawbacks as in the previous item (3), and furthermore, it is difficult to employ this method for irregularly shaped powder compacts.
この発明は、核融合炉のブランケット材として必要とさ
れる焼結密度と表面性状を容易に得ることができ、量産
性、経済性に優れたＬｉ２Ｏ焼結体の製造方法を提供す
ることを目的とする。The purpose of this invention is to provide a method for manufacturing a Li2O sintered body that can easily obtain the sintered density and surface texture required as a blanket material for a nuclear fusion reactor, and is excellent in mass production and economy. shall be.
以上の目的は、金属もしくはセラミック與の容器を使用
し、該容器中に純度９９％以上のアルミナ粉末（ＡＪｚ
Ｏｓ ）でＬｉ ２０圧粉体を埋設し、不活性ガスもし
くは真空中にて焼結することにより達成できる。For the above purpose, a metal or ceramic container is used, and alumina powder (AJz) with a purity of 99% or more is placed in the container.
This can be achieved by embedding a Li 20 green compact in an inert gas or vacuum.
本発明者らは、Ｌｉ ２０焼結体の表面に発生する着色
、汚点１重金属の付着などは、雰囲気ガス中の不純物お
よびＬｉ ２０圧粉体に微量含有されるＬｉＯＨ。The present inventors believe that the discoloration and stains that occur on the surface of the Li 20 sintered body and the adhesion of heavy metals are caused by impurities in the atmospheric gas and LiOH contained in trace amounts in the Li 20 compact.
Ｌｉ２ＣＯ３の浸み出しなどがその原因になるものと考
えた。そして、ＰｔおよびＴａ箔でＬｉ ２０圧粉体を
完全に覆って焼結した場合、良好な表面性状をもつ焼結
体になるのは、これら箔の存在で雰囲気ガス中の不純物
と圧粉体の反応が防止され、かつＰｔとＴａがＬｉ Ｏ
Ｈ、Ｌｉ ２ ＣＯ３を吸収するためであろうと判断し
た。しかし、ｐｔとＴａを用いた場合は前述の欠点を有
している。そこで、発明者らはＬｉ２Ｑ圧粉体と雰囲気
ガスとの反応を防止でき、かつＬＩ ＯＨ、Ｌｉ ２
ＣＯ３を吸収できる微細な粉末を用い、この粉末中にＬ
ｉ２Ｏ圧粉体を埋設して焼結すれば、本発明の目的を達
成できるのではないかと発想し、この粉末として純度四
％以上のアルミナ粉末を選定することによって本発明を
完結した。本発明で、アルミナ粉末の純度を９９％以上
としたのは、これ以下であるとアルミナに含有される酸
化マグネシア、酸化けい素およびアルカリ分（Ｎａ２Ｏ
、Ｋ２Ｏなど）などが多くなって、これらがＬｉ２Ｏと
反応し、Ｌｉ２Ｏ圧粉体の表面にガラス層を形成するこ
とを実験的に確認したためである。また、アルミナが良
好な結果を示すのは、このアルミナがＬｉ２Ｏの１、ｉ
０Ｈ、Ｌｉ ２ ＣＯ３を吸収してリチウムアルミネ
ートに変化するためであろうと推定した。It was thought that seepage of Li2CO3 was the cause. When a Li 20 green compact is completely covered with Pt and Ta foils and sintered, the sintered body has good surface properties because of the presence of these foils, which prevent impurities in the atmospheric gas from forming on the green compact. reaction is prevented, and Pt and Ta are LiO
It was determined that this was probably to absorb H, Li 2 CO 3 . However, the use of pt and Ta has the above-mentioned drawbacks. Therefore, the inventors were able to prevent the reaction between the Li2Q powder compact and the atmospheric gas, and to
A fine powder that can absorb CO3 is used, and L is contained in this powder.
The present invention was completed based on the idea that the object of the present invention could be achieved by embedding and sintering an i2O green compact, and by selecting alumina powder with a purity of 4% or more as the powder. In the present invention, the purity of the alumina powder is set to 99% or more because if the purity is less than 99%, the magnesia oxide, silicon oxide, and alkali content (Na2O
This is because it has been experimentally confirmed that a large amount of Li2O (K2O, etc.) reacts with Li2O to form a glass layer on the surface of the Li2O powder compact. In addition, the reason why alumina shows good results is that this alumina has 1, i of Li2O.
It is presumed that this is because it absorbs 0H and Li 2 CO 3 and changes into lithium aluminate.
以下に実施例に基づき本発明の詳細な説明する。 The present invention will be described in detail below based on Examples.
市販のＬｉ２Ｏ粉末を、圧力５４３／（Ｍｌで形状４９
龍×４９Ｉｌｌ ｘ ２５ ａｍ厚の圧粉体に成形した
。この圧粉体の理論密度比は７３％であった。Ｌｉ２Ｏ
圧粉体の焼結は第１図の方法にて行った。第１図は、Ｌ
ｉｚＯ圧粉体１を板厚Ｑ、 ５ ＩＩＩの５ＵＳ３０４
ステンレスを用いて表作した容器２に収容し、その周囲
をアルミナ粉末３で満たし、さらにＳ Ｕ Ｓ ３０４
ステンレスの蓋４で密閉した状態を示している。この後
、第１図の状態の容器を焼結炉に挿入し、アルゴンガス
中で１２００”Ｃｘ２Ｈの条件で焼結を行った。Commercially available Li2O powder was prepared under pressure 543/(form 49 in Ml).
It was molded into a green compact of 49mm x 25mm thick. The theoretical density ratio of this compact was 73%. Li2O
The green compact was sintered by the method shown in FIG. Figure 1 shows L
izO powder compact 1 with plate thickness Q, 5 III 5US304
It is housed in a container 2 whose surface is made of stainless steel, and its surroundings are filled with alumina powder 3, and then SUS 304
It is shown in a state where it is sealed with a stainless steel lid 4. Thereafter, the container in the state shown in FIG. 1 was inserted into a sintering furnace, and sintering was performed in argon gas under the conditions of 1200"Cx2H.
本発明の方法に対する比較例としては、Ｌｉ２Ｏ圧粉体
をアルミナ基板上に直置きし、それを炉内に配設して前
記と同様の条件で焼結するものと、Ｌｉ２Ｏ圧粉体を厚
さＱ、 １１１ｍのＴａ箔で完全に覆いを行いそれをＴ
ａ容器に収容して焼結するものの二つについて実験を行
った。以上の実験結果を整理すると第１表のようになる
。As a comparative example for the method of the present invention, a method in which a Li2O green compact is placed directly on an alumina substrate, placed in a furnace, and sintered under the same conditions as above, and a method in which a Li2O green compact is placed directly on an alumina substrate, and a SaQ, completely covered with 111m of Ta foil and then
Experiments were conducted on two samples that were housed in a container and sintered. Table 1 summarizes the above experimental results.
第 １ 表
第１表より、Ｌｉ２Ｏ焼結体の理論密度比すなわち焼結
性は圧粉体をＴａ箔で覆った場合が最も優れているが、
アルミナ粉末で埋設して焼結した場合でもその理論密度
比は８６，５％となり、取扱上およびトリチウムの増殖
効率の観点からも問題のない値であった。焼結体の表面
性状においては、アルミナ基板上に直置きして焼結した
場合は満足する結果は得られないが、他の二つの方法で
は清浄な表面が得られた。一方、箔と容器の損傷および
炉内の汚染状況をみると、本発明の方法ではこれらが皆
無であり、容器を繰返し使用することが可能であった。Table 1 From Table 1, the theoretical density ratio, or sinterability, of the Li2O sintered body is best when the compact is covered with Ta foil, but
Even when it was embedded with alumina powder and sintered, the theoretical density ratio was 86.5%, which was a value that caused no problems from the viewpoint of handling and tritium multiplication efficiency. Regarding the surface quality of the sintered body, when the sintered body was placed directly on an alumina substrate and sintered, satisfactory results were not obtained, but a clean surface was obtained using the other two methods. On the other hand, when looking at damage to the foil and container and contamination inside the furnace, there was no such damage in the method of the present invention, and the container could be used repeatedly.
したがって、Ｌｉ２Ｕ圧粉体の焼結方法を経済性、量産
性および焼結体の品質特性などの面から総合的に評価す
ると本発明の優位性が明らかである。Therefore, when the method for sintering the Li2U green compact is comprehensively evaluated from the viewpoints of economy, mass production, quality characteristics of the sintered body, etc., the superiority of the present invention becomes clear.
なお、Ｌｉ２Ｏ圧粉体をアルミナ粉末中に埋設して焼結
する場合は、焼結体の表面性状に対し容器材質および容
器の蓋の有無はほとんど影響がなく、蓋をしな（ても実
用上問題のないことが実験的に確認した。一方、本実施
例ではアルゴンガス雰囲気で焼結する例を説明したが、
真空雰囲気でも同様の効果が得られることは当然であり
、焼結時の温度と時間も１２００℃×２）１に限定され
るものではなく、９００°〜１２００℃で１〜４時間の
範囲であれば良好な性状をもつＬｉｚＯ焼結体を得るこ
とができる。When sintering a Li2O compact by embedding it in alumina powder, the material of the container and the presence or absence of a lid on the container have almost no effect on the surface properties of the sintered body. It was experimentally confirmed that there were no problems.On the other hand, in this example, an example of sintering in an argon gas atmosphere was explained.
It is natural that the same effect can be obtained in a vacuum atmosphere, and the temperature and time during sintering are not limited to 1200 ° C If so, a LizO sintered body with good properties can be obtained.
以上説明したごと（、本発明によればＬ１２０圧粉体を
アルミナ粉末中に埋設して不活性ガスもしくは真空雰囲
気中で焼結することにより、高価なＰｔ 、 Ｔａの箔
と容器を使用することなく、かつ炉内も汚染せず、高密
度で表面性状の良好なＬｉｚＯ焼結体を得ることが可能
で、経済性ｐｉｔ産性などに優れたＬｉｚＯ焼結体の製
造方法を提供できるという効果を有する。As explained above (according to the present invention, expensive Pt and Ta foils and containers can be used by embedding the L120 green compact in alumina powder and sintering it in an inert gas or vacuum atmosphere). The effect is that it is possible to obtain a LizO sintered body with high density and good surface quality without contaminating the inside of the furnace, and it is possible to provide a method for manufacturing a LizO sintered body that is excellent in economy and pit productivity. has.
第１図は本発明の゛焼結方法を示したものでＬｉ２Ｏ圧
粉体をアルミナ粉末中に埋設した状態の側断面図である
。
１：酸化リチウム圧粉体、２ニーステンレス容器、３：
アルミナ粉末。FIG. 1 shows the sintering method of the present invention, and is a side sectional view of a Li2O powder compact embedded in alumina powder. 1: Lithium oxide compact, 2-knee stainless steel container, 3:
Alumina powder.
Claims (1)
粉末中に埋設し、不活性ガスもしくは真空中において焼
結することを特徴とする酸化リチウム焼結体の製造方法
。1) A method for producing a lithium oxide sintered body, which comprises embedding a lithium oxide compact in alumina powder with a purity of 99% or more and sintering it in an inert gas or vacuum.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61251203A JPS63103858A (en) | 1986-10-22 | 1986-10-22 | Manufacture of lithium oxide sintered body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61251203A JPS63103858A (en) | 1986-10-22 | 1986-10-22 | Manufacture of lithium oxide sintered body |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS63103858A true JPS63103858A (en) | 1988-05-09 |
Family
ID=17219223
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61251203A Pending JPS63103858A (en) | 1986-10-22 | 1986-10-22 | Manufacture of lithium oxide sintered body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63103858A (en) |
-
1986
- 1986-10-22 JP JP61251203A patent/JPS63103858A/en active Pending
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