JPH01176207A - Production of oxide superconducting powder - Google Patents
Production of oxide superconducting powderInfo
- Publication number
- JPH01176207A JPH01176207A JP62335981A JP33598187A JPH01176207A JP H01176207 A JPH01176207 A JP H01176207A JP 62335981 A JP62335981 A JP 62335981A JP 33598187 A JP33598187 A JP 33598187A JP H01176207 A JPH01176207 A JP H01176207A
- Authority
- JP
- Japan
- Prior art keywords
- raw material
- solution
- oxide
- atomized
- container
- 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
- 239000000843 powder Substances 0.000 title claims abstract description 54
- 238000004519 manufacturing process Methods 0.000 title claims description 11
- 239000002994 raw material Substances 0.000 claims abstract description 64
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- 239000002887 superconductor Substances 0.000 claims abstract description 6
- 230000001590 oxidative effect Effects 0.000 claims abstract description 4
- 239000007789 gas Substances 0.000 claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 239000003595 mist Substances 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 4
- 239000002245 particle Substances 0.000 abstract description 37
- 239000000243 solution Substances 0.000 abstract description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 9
- PXBRQCKWGAHEHS-UHFFFAOYSA-N dichlorodifluoromethane Chemical compound FC(F)(Cl)Cl PXBRQCKWGAHEHS-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052802 copper Inorganic materials 0.000 abstract description 4
- 150000002823 nitrates Chemical class 0.000 abstract description 3
- 239000007864 aqueous solution Substances 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- 238000000034 method Methods 0.000 description 9
- 239000010949 copper Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 230000007423 decrease Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000000889 atomisation Methods 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 239000005457 ice water Substances 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910017610 Cu(NO3) Inorganic materials 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- AFYPFACVUDMOHA-UHFFFAOYSA-N chlorotrifluoromethane Chemical compound FC(F)(F)Cl AFYPFACVUDMOHA-UHFFFAOYSA-N 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification 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
- Y02E40/00—Technologies for an efficient electrical power generation, transmission or distribution
- Y02E40/60—Superconducting electric elements or equipment; Power systems integrating superconducting elements or equipment
Landscapes
- Oxygen, Ozone, And Oxides In General (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Superconductor Devices And Manufacturing Methods Thereof (AREA)
- Superconductors And Manufacturing Methods Therefor (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は所望の球径で均質性の高い粒度を持つ（粒子径
の均一な）酸化物超電導粉体の製造方法に関するもので
ある。DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a method for producing oxide superconducting powder having a desired spherical diameter and highly homogeneous particle size (uniform particle size).
（従来技術）
アルカリ土金属、島土類元素、銅及び酸素からなる酸化
物系超電導粉体を製造する方法として本件出願人は先に
次のような方法を特許出願した。(Prior Art) The applicant previously filed a patent application for the following method as a method for producing oxide-based superconducting powder consisting of alkaline earth metals, island earth elements, copper, and oxygen.
これは酸化物系超電導粉体を構成する各々の原料を溶媒
に溶かして溶液としたのち、これらを所望の組成比とな
るように混合して均一な混合溶液とした後、該混合溶液
を第３図の霧化袋ｇ１３の周波数０．７〜３ Ｍ Ｈ７
の超音波振動子にて霧化し、この霧化原料の粒子を粒子
分級器５において所望の粒子径に分級し、これを流量コ
ントローラー１から供給される搬送用ガスにより第３図
Ｃブロックに搬送する０次にこの霧状原料６を０．２気
圧以上の酸素分圧を有する酸素雰囲気中で加熱炉７によ
り７００〜１１００℃に加熱して酸化物系超電導粉体９
とし、この酸化物系超電導粉体９を第３図Ｃブロックの
容器１０に導入する。この容器１０は冷媒１２よって冷
却されており、同容器１０内において酸化物系超電導粉
体に残存している溶媒を回収すると同時に分級する。こ
のようにして得られた酸化物系超電導粉体を第３図Ｃブ
ロックの攪拌羽根１９で攪拌しながら１ｏｏｏ〜６００
０ｖの直流電圧により該粉体に荷電して補集板１６に補
集するようにしたものである。この方法によると平均粒
径で０．８ｇｍ、標準偏差０．３５ｐｍの酸化物系超電
導体粉末が製作できるものであった。This involves dissolving each of the raw materials constituting the oxide-based superconducting powder in a solvent to form a solution, and then mixing these to a desired composition ratio to make a uniform mixed solution. Frequency of atomization bag g13 in Figure 3: 0.7 to 3 MH7
The particles of this atomized raw material are classified into desired particle diameters by a particle classifier 5, and are transported to block C in FIG. 3 by a transport gas supplied from a flow controller 1. Next, this atomized raw material 6 is heated to 700 to 1100° C. in a heating furnace 7 in an oxygen atmosphere having an oxygen partial pressure of 0.2 atmospheres or more to form an oxide-based superconducting powder 9.
Then, this oxide-based superconducting powder 9 is introduced into the container 10 of block C in FIG. 3. This container 10 is cooled by a refrigerant 12, and the solvent remaining in the oxide-based superconducting powder is recovered and classified at the same time in the container 10. The oxide-based superconducting powder thus obtained was stirred with the stirring blade 19 of block C in FIG.
The powder is charged with a DC voltage of 0V and collected on a collection plate 16. According to this method, oxide-based superconductor powder with an average particle size of 0.8 gm and a standard deviation of 0.35 pm could be produced.
（従来技術の問題点） 前記従来方法では次のような課題が残されている。(Problems with conventional technology) The following problems remain in the conventional method.
（１）超音波素子により原料液体を霧化する工程におい
て、超音波素子と接触している原料液体２の温度が運転
時間の経過とともに上昇し、霧化した原料液体６の粒子
系が大きくなる。(1) In the process of atomizing the raw material liquid by an ultrasonic element, the temperature of the raw material liquid 2 in contact with the ultrasonic element increases with the passage of operating time, and the particle system of the atomized raw material liquid 6 becomes larger. .
（２）霧化された霧状原料６が分級器５等を通過して加
熱炉７に入るまでの間に温度変化があると（例えば温度
上昇する々）、霧状原料６の濃度が蒸発により濃くなり
、出来上った酸化物系超電導粉体の粒径がばらつく。(2) If the atomized raw material 6 passes through the classifier 5 etc. and enters the heating furnace 7, if there is a temperature change (for example, the temperature rises), the concentration of the raw material atomized 6 will evaporate. The particle size of the resulting oxide-based superconducting powder varies.
（３）逆に霧状原料６の温度が降下すると凝縮して霧状
原料６があたかも増粒されたようになり、出来上った酸
化物系超電導粉体の粒径がばらつく（４）従来方法によ
れば平均粒径で０．８ ｐｍ、標準偏差０．３５μ町の
酸化物系超電導粉体が作成できるが、より緻密な酸化物
系超電導成形体を作成するためにはこの粒径では充分で
なく、均一な粒径を持つ粉末が必要となる。(3) On the other hand, when the temperature of the atomized raw material 6 decreases, it condenses and the atomized raw material 6 becomes as if its particles have been increased, and the particle size of the resulting oxide-based superconducting powder varies. (4) Conventional According to this method, oxide-based superconducting powder with an average particle size of 0.8 pm and a standard deviation of 0.35 μm can be created, but in order to create a denser oxide-based superconducting compact, it is necessary to use this particle size. Powder with uniform particle size is required.
（発明の目的）
本発明はこのような点に鑑みてなされたものであり、そ
の目的は、均一な粒径を持つ酸化物系超電導粉体を製造
できる酸化物系超電導粉体の製造方法を提供することに
ある。(Object of the Invention) The present invention has been made in view of the above points, and its purpose is to provide a method for producing oxide-based superconducting powder that can produce oxide-based superconducting powder having a uniform particle size. It is about providing.
（問題点を解決するための手段）
本発明の酸化物系超電導粉体の製造方法は、溶媒に溶か
して溶液とした酸化物系超電導体となる原料の溶液を超
音波振動子にて霧化し、これを酸素を含むガス体で加熱
炉に搬送して霧状原料とした後、加熱酸化させて酸化物
系超電導粉体を製造する方法において、原料溶液と霧状
原料の温度を原料容器から加熱炉に導入されるまで同一
もしくはほぼ同一にすることを特徴とするものである。(Means for Solving the Problems) The method for producing oxide-based superconducting powder of the present invention involves atomizing a solution of a raw material that will become an oxide-based superconductor by dissolving it in a solvent using an ultrasonic vibrator. In the method of producing oxide-based superconducting powder by conveying this to a heating furnace with a gas containing oxygen to make it into atomized raw material, and then heating and oxidizing it, the temperature of the raw material solution and the atomized raw material is controlled from the raw material container. It is characterized by being the same or almost the same until it is introduced into the heating furnace.
次に本発明の実施態様を図面を用いて具体的に説明する
。第１図は本発明の実施に使用した装置の一例を示す説
明図である０本発明は次のＡ−Ｃの工程により構成され
る。このＡ−Ｃの工程は第１図のＡ−Ｃのブロックに対
応する。Next, embodiments of the present invention will be specifically described using the drawings. FIG. 1 is an explanatory diagram showing an example of an apparatus used in carrying out the present invention. The present invention is constructed by the following steps A to C. This step A-C corresponds to blocks A-C in FIG.
（Ａ）酸化物系超電導粉体となる原料溶液を霧化して粒
子径のそろった霧状原料を作ると共に、原料溶液と霧状
原料の温度を同一もしくはほぼ同一に保持する工程。(A) A step of atomizing the raw material solution that will become the oxide-based superconducting powder to produce a mist of raw material with a uniform particle size, and maintaining the temperature of the raw material solution and the atomized raw material at the same or almost the same temperature.
ＣＢ）前記霧状原料を加熱酸化して酸化物系超電導粉体
とする工程。CB) A step of heating and oxidizing the atomized raw material to obtain an oxide-based superconducting powder.
（Ｃ）ａ化物系超電導粉体を脱水して補集する工程。(C) A step of dehydrating and collecting the a-ide superconducting powder.
これらのＡ、Ｂ、Ｃの工程は第１図のように連続化され
ている。以下これらの各工程について詳細に説明する。These steps A, B, and C are continuous as shown in FIG. Each of these steps will be explained in detail below.
（Ａ）工程
第１図のＡブロックにおいて、容器３１内の溶液化され
た酸化物系超電導体となる原料の溶液２は恒温槽３０で
一定温度に保持されている。また容器３１内の原料溶液
２はマイクロチューブポンプ３２により一定速度で容器
３３に移送される。(A) Process In block A of FIG. 1, the solution 2 of the raw material that will become the oxide-based superconductor that has been turned into a solution in the container 31 is maintained at a constant temperature in a constant temperature bath 30. Further, the raw material solution 2 in the container 31 is transferred to the container 33 at a constant speed by the microtube pump 32.
容器３３中の原料溶液２の贋はマイクロチューブポンプ
３２により供給、排出されて常に一定量となっている。The counterfeit raw material solution 2 in the container 33 is supplied and discharged by the microtube pump 32, so that a constant amount is always maintained.
容器３３内の原料溶液２は霧化装置３により霧化される
。霧化された原料溶液２は流量コントローラｌから供給
される酸素含有ガス体にて分級器５に導入され、ここで
重量差により粒径分布が關御され粒径数ＩＬｍ程度の粒
子群からなる霧状原料６とされる。The raw material solution 2 in the container 33 is atomized by the atomizer 3 . The atomized raw material solution 2 is introduced into a classifier 5 using an oxygen-containing gas supplied from a flow rate controller 1, where the particle size distribution is controlled by the weight difference and consists of a particle group with a particle size of about several ILm. It is referred to as atomized raw material 6.
また第１図のＡブロックは図示されていない恒温装置に
より恒温槽として、容器３１及び３２内の溶液原料２を
同一温度に保持できるようにしである。Block A in FIG. 1 is configured as a constant temperature bath using a constant temperature device (not shown) so that the solution raw materials 2 in the containers 31 and 32 can be maintained at the same temperature.
（Ｂ）工程
第１図のＡブロックにおいて得られた霧状原料６は同図
Ｂブロックに送られ、同ブロック内の加熱炉７内で加熱
酸化されて酸化物系超電導粉体９となる。(B) Process The atomized raw material 6 obtained in block A in FIG. 1 is sent to block B in the same figure, and is heated and oxidized in a heating furnace 7 in the same block to become oxide-based superconducting powder 9.
（Ｃ）工程
第１図のＢブロックにおいて得られた酸化物系超電導粉
体９は同図Ｃブロックに送られ、冷媒１２で冷却されて
いる水分補集ＷＩＯ内で脱水及び分級が行なわれる。脱
水された酸化物系超電導粉体は補集器１５に導入され、
そこで１０００〜８ｏｏｏｖの直流電圧により荷電され
、補集板１６上に堆積させて補集する。(C) Process The oxide-based superconducting powder 9 obtained in block B in FIG. 1 is sent to block C in the same figure, where it is dehydrated and classified in a water collector WIO cooled by a refrigerant 12. The dehydrated oxide-based superconducting powder is introduced into the collector 15,
There, it is charged with a DC voltage of 1000 to 8 ooov, deposited on the collection plate 16, and collected.
（作用）
本発明の酸化物系超電導粉体の製造方法においては、霧
化装置３中の原料溶液２の量が常に一定となるため超音
波振動子にて霧化される原料溶液霧の粒径変化が抑制さ
れ均一となる。ちなみに霧化装置３中の溶液量が減少す
ると原料溶液霧の粒径が大きくなる。(Function) In the method for producing oxide-based superconducting powder of the present invention, since the amount of the raw material solution 2 in the atomization device 3 is always constant, particles of the raw material solution mist atomized by the ultrasonic vibrator Changes in diameter are suppressed and uniform. Incidentally, as the amount of solution in the atomizer 3 decreases, the particle size of the raw material solution mist increases.
また第１図のＡブロックを恒温としたので加熱炉７に導
入される前まで原料溶液２及び霧状原料６の温度が同一
温度となり、原料溶液２の蒸発凝固がおさえられ、原料
の濃度変化がなく１粒子径の均一な酸化物系Ｍｉ電導粉
体が作成できる。ちなみに溶液濃度が濃くなると粒子径
は大きくなり、薄くなると小さくなる。In addition, since the A block in Fig. 1 is kept at a constant temperature, the temperature of the raw material solution 2 and the atomized raw material 6 are the same until they are introduced into the heating furnace 7, and the evaporation and solidification of the raw material solution 2 is suppressed, resulting in changes in the concentration of the raw material. It is possible to create a uniform oxide-based Mi conductive powder with a particle size of 1 without any particles. Incidentally, as the solution concentration increases, the particle size increases, and as the solution concentration decreases, it decreases.
（実施例１）
次に第１図に示した装置を用いて酸化物系超電導粉体を
製造した場合の本発明の実施例を具体的に説明する。(Example 1) Next, an example of the present invention in which oxide-based superconducting powder was manufactured using the apparatus shown in FIG. 1 will be specifically described.
出発原料としては、Ｙ、Ｂａ及びＣｕの硝酸塩即ちＹ
（ＮＯ３）３ ｍ ６Ｈ２０，Ｂａ（ＮＯ３）ｚ及び
Ｃｕ（ＮＯ３）・３Ｈ２０をモル比でＹ：Ｂａ：Ｃｕ＝
１：２：３となるように秤量し、脱イオン水に混合溶解
して溶液濃度がＹ Ｂａ２（ｕ３０７−ｘに換算して０
．０６ｍｏ ／ ／ｌ となるようにした混合溶液を用
いた。又流量コントローラー１から送られる流体搬送用
ガスにはｍ素ガスを用い流量は１７７ｍａｎとした。As starting materials, nitrates of Y, Ba and Cu, i.e. Y
(NO3)3 m 6H20, Ba(NO3)z and Cu(NO3)・3H20 in molar ratio Y:Ba:Cu=
Weigh it so that the ratio is 1:2:3 and mix and dissolve it in deionized water to make the solution concentration YBa2 (0 in terms of u307-x).
．． A mixed solution having a concentration of 0.06 mo//l was used. Further, m element gas was used as the fluid transport gas sent from the flow rate controller 1, and the flow rate was set to 177 man.
溶液の温度は恒温槽３０にて４０℃±２℃に制御し、霧
状原料６の温度も４０℃±２℃とした。The temperature of the solution was controlled at 40°C±2°C in a constant temperature bath 30, and the temperature of the atomized raw material 6 was also set at 40°C±2°C.
前記各原料の混合液を周波数１．７ＭＨｚの超音波振動
子よりなる霧化装置３により平均粒径約８ルｍに微粒子
化し、粒子分級器５により１０４ｍ以上の大きい液滴は
髪果させて回収し、粒子径１０ｇｍ未満の液滴のみを１
０００℃に加熱された加熱炉７に搬送した。The mixed liquid of each of the raw materials was atomized to an average particle size of about 8 m by an atomizer 3 consisting of an ultrasonic vibrator with a frequency of 1.7 MHz, and large droplets of 104 m or more were removed by a particle classifier 5. Collect only droplets with a particle size of less than 10 gm.
The sample was transferred to a heating furnace 7 heated to 000°C.
次にこの霧状原料６を加熱炉７で加熱して酸化物系超電
導粉体９とし、これを冷媒１２で冷却されている水分補
集器１０に導入して脱水及び分級を行なった。水分補集
のための冷媒１２には氷水を用いた。しかる後、このよ
うにして脱水された酸化物系超電導粉体を補集器１５に
導入し、５０００■の直流電圧により荷電して補集板１
６上に堆積させて補集した。尚この際の収率は約６０％
であった。Next, this atomized raw material 6 was heated in a heating furnace 7 to form an oxide-based superconducting powder 9, which was then introduced into a water collector 10 cooled with a refrigerant 12 for dehydration and classification. Ice water was used as the refrigerant 12 for water collection. Thereafter, the oxide-based superconducting powder thus dehydrated is introduced into the collector 15, charged with a DC voltage of 5000 μ, and then transferred to the collector plate 1.
6 and collected. The yield at this time is approximately 60%.
Met.
この実施例により得られた酸化物系ａ電導粉体の形状を
走査電顕で観察したところ、平均粒径２μｍのきれいな
球状の粉体であり、標準偏差は約０．１５ＡＬｍであり
、非常に均一な粒径の酸化物系超電導粉体が得られた。When the shape of the oxide-based a conductive powder obtained in this example was observed using a scanning electron microscope, it was found to be a fine spherical powder with an average particle size of 2 μm, and a standard deviation of about 0.15 ALm, which was extremely Oxide-based superconducting powder with uniform particle size was obtained.
又酸化物系超電導粉体のＸ線回折結果は第２図に示す通
りであって、ペロブスカイト構造を持つＹＢａｚＣｕ：
＋０７−ｙの鋭いピークが観察され、ペロブスカイト構
造から離れた異相（例えばＹ２ ＢａＣｕ ０５−Ｘ等
）は認められなく、単相（この実施例ではＣｕ Ｏ）等
の不純物も僅かしか認められな−ｂＸった。The X-ray diffraction results of the oxide-based superconducting powder are shown in Figure 2, and YBazCu with a perovskite structure:
A sharp peak of +07-y was observed, and no foreign phase (e.g. Y2 BaCu 05-X, etc.) separate from the perovskite structure was observed, and only a small amount of impurities such as a single phase (CuO in this example) was observed. It was bX.
更に得られた酸化物超電導粉体についてマイスナー効果
及び超電導特性を測定したところ、マイスナー効果が認
められると共に、臨界温度（Ｔ ｃ）として９０°Ｋ、
臨界電流密度（Ｊｃ）として６００Ａ／ｃｍ２の値が得
られ、従来の方法で製造された酸化物系超電導粉体とほ
ぼ同等の超電導特性を有している事がわかった。Furthermore, when the Meissner effect and superconducting properties of the obtained oxide superconducting powder were measured, the Meissner effect was observed, and the critical temperature (Tc) was 90°K.
A value of 600 A/cm2 was obtained as a critical current density (Jc), and it was found that the powder had superconducting properties almost equivalent to those of oxide-based superconducting powder produced by conventional methods.
（実施例２）
次に本発明を上記の実施例とは異なる実施例により具体
的に説明する。(Example 2) Next, the present invention will be specifically explained using an example different from the above-mentioned example.
出発原料として、Ｙ、Ｂａ及びＣｕの硝酸塩即ちＹ （
ＮＯ３）３ ＠６Ｈ２０，Ｂａ（ＮＯ＋）ｚ及びＣｕ（
ＮＯｘ）＊ ３Ｈ２０をモル比でＹ：Ｂａ：Ｃｕ＝１：
２：３となるように秤量し、脱イオン水に混合溶解して
、溶液濃度がＹＢａ２ＣｕｓＯｙ−ｘに換算して０．０
８ｍｏ／／ノとなるようにした混合溶液を用いた。又流
体搬送用ガスには酸素ガスを用い、流量は１／／ｍ＋ｎ
とした。As starting materials, nitrates of Y, Ba and Cu, namely Y (
NO3)3 @6H20, Ba(NO+)z and Cu(
NOx)* 3H20 in molar ratio Y:Ba:Cu=1:
Weigh it so that the ratio is 2:3, mix and dissolve it in deionized water, and the solution concentration is 0.0 in terms of YBa2CusOy-x.
A mixed solution having a concentration of 8 mo//no was used. Oxygen gas is used as the fluid transport gas, and the flow rate is 1//m+n.
And so.
溶液の温度は恒温槽３０にて６０℃±２℃に制御し、霧
状原料６の温度も６０℃±２℃とした。The temperature of the solution was controlled at 60°C±2°C in a constant temperature bath 30, and the temperature of the atomized raw material 6 was also 60°C±2°C.
前記各原料の混合液を周波数１．７ＭＨｚの超音波振動
子よりなる霧化装置３により微粒子化し、粒子分級器５
により１５Ｂｍ以上の大きい液滴は凝集させて回収し、
粒子径１５４ｍ未満の液滴のみを１０００℃に加熱され
た加熱炉７に搬送した。The mixed liquid of each of the raw materials is atomized by an atomization device 3 consisting of an ultrasonic vibrator with a frequency of 1.7 MHz, and then atomized by a particle classifier 5.
Large droplets of 15 Bm or more are aggregated and collected by
Only droplets with a particle diameter of less than 154 m were transported to a heating furnace 7 heated to 1000°C.
次に加熱炉７内で酸化された酸化物系超電導粉体９を、
冷媒１２で冷却されている水分補集器１０に導入し、こ
こで脱水及び分級を行なった。尚水分補集のための冷媒
１２には氷水を用いた。しかる後このようにして脱水さ
れた酸化物系超電導粉体を補集器１５に導入し、５ｏｏ
ｏｖの直流電圧により荷電して補集板１６上に堆積させ
て補集した。尚この際の収率は約６０％であった。Next, the oxide-based superconducting powder 9 oxidized in the heating furnace 7 is
It was introduced into a water collector 10 cooled by a refrigerant 12, where it was dehydrated and classified. Furthermore, ice water was used as the refrigerant 12 for collecting water. Thereafter, the oxide-based superconducting powder thus dehydrated is introduced into the collector 15, and 5oo
It was charged with a DC voltage of 0.5 m and deposited on a collection plate 16 to be collected. The yield at this time was about 60%.
この実施例により得られた酸化物系超電導粉体の形状を
走査電顕で観察したところ平均粒径２．８１Ｌｍのきれ
いな球状の粉体であり、標準偏差は約０．１５４ｍであ
り、非常に均一な粒径の酸化物系超電導粉体が得られた
。When the shape of the oxide-based superconducting powder obtained in this example was observed using a scanning electron microscope, it was found to be a fine spherical powder with an average particle size of 2.81 Lm, and a standard deviation of about 0.154 m. Oxide-based superconducting powder with uniform particle size was obtained.
又その酸化物系超電導粉体のＸ線回折結果、マイスナー
効果及び超電導特性を測定したところ実施例１の場合と
同様の特性が確認された。Furthermore, when the oxide-based superconducting powder was subjected to X-ray diffraction, Meissner effect, and superconducting properties were measured, the same properties as in Example 1 were confirmed.
（発明の効果） 本発明の製造方法によれば次のような効果がある。(Effect of the invention) The manufacturing method of the present invention has the following effects.
（１）比較的簡易な工程で、微細で且つ球状の酸化物系
超電導粉体を製造することができ、この粉体を用いるこ
とにより緻密で超電導特性の優れた酸化物超電導成形体
を得ることができる。(1) Fine and spherical oxide-based superconducting powder can be produced through a relatively simple process, and by using this powder, a dense oxide superconducting molded body with excellent superconducting properties can be obtained. Can be done.
（２）ｔａ化装ｆｆ１３中の原料溶液２の量が常に一定
となるため、超音波振動子にて霧化される原料溶液霧の
粒径変化が抑制されて均一となり、また加熱炉７に導入
される前まで原料溶液２及び霧状原料６の温度を同一温
度としであるので粒子径の均一な酸化物系超電導粉体が
作成できる。(2) Since the amount of the raw material solution 2 in the TA converter ff13 is always constant, the particle size change of the raw material solution mist atomized by the ultrasonic vibrator is suppressed and becomes uniform, and it is also introduced into the heating furnace 7. Since the temperature of the raw material solution 2 and the atomized raw material 6 are kept at the same temperature before being mixed, an oxide-based superconducting powder having a uniform particle size can be produced.
第１図は本発明の実施に使用する装置の一例を示す説明
図、第２図は実施例にて得られた酸化物系超電導粉体の
Ｘ線回折結果の一例を示すチャート図、第３図は従来の
製造方法の実施に使用される装置の説明図である。
１は流量コントローラー
２は原料溶液
３は霧化装置
４は霧化された原料
５は粒子分級器
６は霧状原料
７は加熱炉
８は温度制御用センサー
９は酸化物系超電導粉体
１０は水分補集器
１１は容器
１２は冷媒
１３は水
１４は酸化物超電導粉体
１５は補集器
１６は補集板
１７は出口
１８はモーター
１９は攪拌羽根
２０は電極
２１はアース
３０は恒温槽
３１は容器
３２はマイクロチューブポンプ
３３は容器FIG. 1 is an explanatory diagram showing an example of the apparatus used in carrying out the present invention, FIG. 2 is a chart diagram showing an example of the X-ray diffraction results of the oxide-based superconducting powder obtained in the example, and FIG. The figure is an explanatory diagram of an apparatus used to carry out a conventional manufacturing method. 1 is the flow rate controller 2 is the raw material solution 3 is the atomizer 4 is the atomized raw material 5 is the particle classifier 6 is the atomized raw material 7 is the heating furnace 8 is the temperature control sensor 9 is the oxide-based superconducting powder 10 Moisture collector 11, container 12, refrigerant 13, water 14, oxide superconducting powder 15, collector 16, collector plate 17, outlet 18, motor 19, stirring blade 20, electrode 21, ground 30, constant temperature bath 31 is a container 32 is a micro tube pump 33 is a container
Claims (2)
る原料溶液を超音波振動子にて霧化し、これを酸素を含
むガス体で加熱炉に搬送して霧状原料とし、それを加熱
酸化させて酸化物系超電導粉体を製造する方法において
、原料溶液と霧状原料の温度を原料容器から加熱炉に導
入されるまで同一もしくはほぼ同一温度としたことを特
徴とする酸化物系超電導粉体の製造方法。(1) A raw material solution that will become an oxide superconductor dissolved in a solvent is atomized using an ultrasonic vibrator, and this is conveyed to a heating furnace using a gas containing oxygen to form a mist raw material. A method for producing an oxide-based superconducting powder by heating and oxidizing the powder, characterized in that the temperature of the raw material solution and the atomized raw material are kept at the same or almost the same temperature until they are introduced from the raw material container into the heating furnace. Method for producing superconducting powder.
て、超音波発生装置に収納された容器中の原料溶液の量
を常時一定量にすることを特徴とする特許請求の範囲第
１項記載の酸化物系超電導粉体の製造方法。(2) In the step of atomizing the solution raw material using an ultrasonic vibrator, the amount of the raw material solution in the container housed in the ultrasonic generator is always kept constant. A method for producing an oxide-based superconducting powder as described in 2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62335981A JPH01176207A (en) | 1987-12-29 | 1987-12-29 | Production of oxide superconducting powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62335981A JPH01176207A (en) | 1987-12-29 | 1987-12-29 | Production of oxide superconducting powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01176207A true JPH01176207A (en) | 1989-07-12 |
Family
ID=18294461
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62335981A Pending JPH01176207A (en) | 1987-12-29 | 1987-12-29 | Production of oxide superconducting powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01176207A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011098867A (en) * | 2009-11-07 | 2011-05-19 | Univ Of Fukui | Method for producing fine particle of metal oxide or metal |
| JP2019026507A (en) * | 2017-07-28 | 2019-02-21 | 住友金属鉱山株式会社 | Method for producing transition metal composite oxide particles |
-
1987
- 1987-12-29 JP JP62335981A patent/JPH01176207A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011098867A (en) * | 2009-11-07 | 2011-05-19 | Univ Of Fukui | Method for producing fine particle of metal oxide or metal |
| JP2019026507A (en) * | 2017-07-28 | 2019-02-21 | 住友金属鉱山株式会社 | Method for producing transition metal composite oxide particles |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US7081267B2 (en) | Nanostructured powders and related nanotechnology | |
| Bae et al. | Synthesis and microstructure of Pd/SiO 2 nanosized particles by reverse micelle and sol–gel processing | |
| Cabanas et al. | Spherical iron oxide particles synthesized by an aerosol technique | |
| JPH01176207A (en) | Production of oxide superconducting powder | |
| US5395821A (en) | Method of producing Pb-stabilized superconductor precursors and method of producing superconductor articles therefrom | |
| US20090298699A1 (en) | Process for producing raw material powder for oxide superconductor | |
| Pebler et al. | Synthesis of superconducting oxides by aerosol pyrolysis of metal-EDTA solutions | |
| JPH01179724A (en) | Production of oxide superconducting powder | |
| JPH01179723A (en) | Production of oxide superconducting powder | |
| Lyons et al. | Nanophase oxide formation by intraparticle reaction | |
| JPH01176221A (en) | Production of oxide superconducting powder | |
| JPH01188415A (en) | Production of oxide superconducting powder | |
| JPH0574530B2 (en) | ||
| JPH01176222A (en) | Production of oxide based superconducting powder | |
| JP2835083B2 (en) | Manufacturing method of oxide superconductor | |
| JPH03109207A (en) | Production of oxide superconducting powder occluding oxygen or gaseous ozone | |
| Joutsensaari et al. | Generation of nanophase fullerene particles via aerosol routes | |
| JPH02137709A (en) | Production of oxide superconductor powder | |
| CN103769608A (en) | Nano-silver sol separating method | |
| Mančić et al. | High TC superconducting powders synthesis from aerosol | |
| Zhang et al. | The principle of vapor-phase technics and application in synthesis of M x O y nanomaterials | |
| JPH01226724A (en) | Method for synthesizing fine oxide particles as starting material | |
| JPH0193403A (en) | Production of ceramic-based superconducting material and apparatus therefor | |
| JPH01197318A (en) | Production of oxide superconducting powder | |
| KR20120066817A (en) | Nano-sized powder manufacturing apparatus through evaporation, condensation and gathering in oil |