JPH0435419B2 - - Google Patents
Info
- Publication number
- JPH0435419B2 JPH0435419B2 JP62129053A JP12905387A JPH0435419B2 JP H0435419 B2 JPH0435419 B2 JP H0435419B2 JP 62129053 A JP62129053 A JP 62129053A JP 12905387 A JP12905387 A JP 12905387A JP H0435419 B2 JPH0435419 B2 JP H0435419B2
- Authority
- JP
- Japan
- Prior art keywords
- compound
- heating
- oxide
- decomposed
- lutetium
- 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
- 150000001875 compounds Chemical class 0.000 claims description 21
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 20
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 18
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 15
- 239000011701 zinc Substances 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 12
- 150000002500 ions Chemical class 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 239000011787 zinc oxide Substances 0.000 claims description 7
- 229910052725 zinc Inorganic materials 0.000 claims description 6
- 229910003443 lutetium oxide Inorganic materials 0.000 claims description 5
- MPARYNQUYZOBJM-UHFFFAOYSA-N oxo(oxolutetiooxy)lutetium Chemical compound O=[Lu]O[Lu]=O MPARYNQUYZOBJM-UHFFFAOYSA-N 0.000 claims description 5
- 229910052765 Lutetium Inorganic materials 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 230000001590 oxidative effect Effects 0.000 claims description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- OHSVLFRHMCKCQY-UHFFFAOYSA-N lutetium atom Chemical compound [Lu] OHSVLFRHMCKCQY-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 description 7
- 239000000696 magnetic material Substances 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/009—Compounds containing, besides iron, two or more other elements, with the exception of oxygen or hydrogen
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/76—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by a space-group or by other symmetry indications
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Iron (AREA)
- Catalysts (AREA)
- Soft Magnetic Materials (AREA)
- Recrystallisation Techniques (AREA)
Description
産業上の利用分野
本発明は磁性材料、半導体材料及び触媒材料等
として有用な新規化合物であるLuFeZn9O12で示
される六方晶系の層状構造を有する化合物および
その製造法に関する。
従来技術
従来、(Yb3+Fe3+O3)oFe2+O(nは整数を示す)
で示される六方晶系の層状構造を有する化合物は
本出願人によつて合成され知られている。
YbFe2O4,Yb2Fe3O7,Yb3Fe4O10及びYb4Fe5
O13の六方晶系としての格子定数、YbO1.5層,
FeO1.5層,Fe2O2.5層の単位格子内における層数
を示すと表−1の通りである。
これらの化合物は酸化鉄(FeO)1モルに対し
て、YbFeO3がnモル(n=1,2,3……)の
割合で化合していると考えられる層状構造を持つ
化合物である。
INDUSTRIAL APPLICATION FIELD The present invention relates to a compound having a hexagonal layered structure represented by LuFeZn 9 O 12 , which is a new compound useful as a magnetic material, a semiconductor material, a catalyst material, etc., and a method for producing the same. Conventional technology Conventionally, (Yb 3+ Fe 3+ O 3 ) o Fe 2+ O (n indicates an integer)
The compound having a hexagonal layered structure represented by is synthesized by the applicant and is known. YbFe 2 O 4 , Yb 2 Fe 3 O 7 , Yb 3 Fe 4 O 10 and Yb 4 Fe 5
Lattice constant of O 13 as hexagonal system, YbO 1.5 layer,
Table 1 shows the number of layers in the unit cell of 1.5 FeO layers and 2.5 Fe 2 O layers. These compounds have a layered structure in which YbFeO 3 is thought to be combined at a ratio of n moles (n=1, 2, 3...) per mole of iron oxide (FeO).
【表】
発明の目的
本発明は(YbFeO3)oFeOの化学式において、
n=1/9に相当しYb3+の代わりにLu3+をFe2+の代
わりにZn2+を置きかえて得られる新規な化合物
を提供するにある。
発明の構成
本発明のLuFeZn9O12で示される化合物は、イ
オン結晶モデルでは、Lu3+(Fe3+Zn2+)Zn8 2+O12
2−として記載され、その構造はLuO1.5層,(Fe,
Zn)O2.5層およびZnO層の積層によつて形成され
ており著しい構造異方性を持つことがその特徴の
一つである。Zn2+イオンの1/9はFe3+と共に
(Fe3+Zn2+)O2.5層を作り、残りの8/9はZnO層を
作つている。六方晶系としての格子定数は次の通
りである。
a=3.297±0.001(Å)
c=87.84±0.01 (Å)
この化合物の面指数(hkl),面間隔(d(Å))
(dpは実測値,dcは計算値を示す)およびX線に
対する相対反射強度(I(%))を示すと表−2の
通りである。
この化合物は磁性材料,半導体材料および触媒
材料として有用なものである。例えば、異方性の
強い2次元的性質を持つ磁性体・半導体および触
媒物質としての利用の可能性が考えられる。[Table] Purpose of the invention The present invention is based on the chemical formula of (YbFeO 3 ) o FeO,
The object of the present invention is to provide a novel compound obtained by replacing Yb 3+ with Lu 3+ and Fe 2+ with Zn 2+ , corresponding to n=1/9. Structure of the Invention In the ionic crystal model, the compound represented by LuFeZn 9 O 12 of the present invention is Lu 3+ (Fe 3+ Zn 2+ )Zn 8 2+ O 12
2- , its structure is LuO 1.5 layer, (Fe,
It is formed by laminating a Zn)O 2.5 layer and a ZnO layer, and one of its characteristics is that it has significant structural anisotropy. 1/9 of the Zn 2+ ions together with Fe 3+ form the (Fe 3+ Zn 2+ )O 2.5 layer, and the remaining 8/9 form the ZnO layer. The lattice constants as a hexagonal crystal system are as follows. a=3.297±0.001 (Å) c=87.84±0.01 (Å) Planar index (hkl), plane spacing (d (Å)) of this compound
(d p is an actual measurement value, d c is a calculated value) and the relative reflection intensity (I (%)) for X-rays is shown in Table 2. This compound is useful as a magnetic material, a semiconductor material, and a catalytic material. For example, it is possible to use them as magnetic materials, semiconductors, and catalyst materials that have two-dimensional properties with strong anisotropy.
【表】【table】
【表】【table】
【表】
この化合物は次の方法によつて製造し得られ
る。
金属ルテチウムあるいは酸化ルテチウムもしく
は加熱により酸化ルテチウムに分解される化合物
と、金属鉄あるいは酸化鉄もしくは加熱により酸
化鉄に分解される化合物と、金属亜鉛あるいは酸
化亜鉛もしくは加熱により酸化亜鉛に分解される
化合物と、Lu,FeおよびZnの割合が原子比で1
対1対9の割合で混合し、該混合物を700℃以上
の温度で、大気中、酸化性雰囲気中あるいはLu
およびFeが各々3価イオン状態、Znが2価イオ
ン状態より還元されない還元雰囲気中で加熱する
ことによつて製造し得られる。
本発明に用いる出発物質は市販のものをそのま
ま使用してもよいが、化学反応を速やかに進行さ
せるためには粒径が小さい方がよく、特に10μm
以下であることが好ましい。
また、磁性材料,半導体材料として用いる場合
には不純物の混入をきらうので、純度の高いこと
が好ましい。出発物質が加熱により金属酸化物を
得る化合物としては、それぞれの金属の水酸化
物,炭酸塩,硝酸塩等が挙げられる。
原料はそのまま、あるいはアルコール類,アセ
トン等と共に充分に混合する。
原料の混合割合は、Lu,Fe,Znの割合が原子
比で1対1対9の割合であることが必要である。
これをはずすと目的とする化合物の単一相を得る
ことができない。
この混合物を大気中,酸化性雰囲気中あるいは
LuおよびFeが各々3価イオン状態,Znが各々2
価イオン状態から還元されない還元雰囲気中で
700℃以上で加熱する。加熱時間は数時間もしく
はそれ以上である。加熱の際の昇温速度には制約
はない。加熱終了後急冷するか、あるいは大気中
に急激に引き出せばよい。
得られたLuFeZn9O12化合物の粉末は褐色であ
り、粉末X線回折法によつて結晶構造を有するこ
とが分かつた。その結晶構造は層状構造であり、
LuO1.5層,(Fe,Zn)O2.5層,およびZnO層の積
重ねによつて形成されていることが分かつた。
実施例
純度99.99%以上の酸化ルテチウム(Lu2O3)
粉末,純度99.9%以上の酸化鉄(Fe2O3)粉末,
試薬特級の酸化亜鉛(ZnO)粉末をモル比で1対
1対14の割合に秤量し、めのう乳鉢内でエタノー
ルを加えて、約30分間混合し、平均粒径数μmの
微粉末混合物を得た。該混合物を白金管内に封入
し、1450℃に設定された管状シリコニツト炉内に
入れ、7日間加熱し、その後、試料を炉外にとり
だし室温まで急速に冷却した。
得られた試料は、LuFeZn9O12単一相であり、
粉末X線回折法によつて、各面指数(hkl),面間
隔(dp)および相対反射強度を測定した結果は表
−2の通りであつた。
六方晶系としての格子定数は
a=3.297±0.001(Å)
c=87.84±0.01 (Å)
であつた。
上記の格子定数および表−2の面指数(hkl)
より算出した面間隔(dc(Å))は、実測の面間隔
(dp(Å))と極めてよく一致していた。
発明の効果
本発明は磁性材料,半導体材料及び触媒として
有用な新規化合物を提供する。[Table] This compound can be produced by the following method. Metallic lutetium or lutetium oxide or a compound that is decomposed into lutetium oxide by heating; Metallic iron or iron oxide or a compound that is decomposed into iron oxide by heating; Metallic zinc or zinc oxide or a compound that is decomposed into zinc oxide by heating. , the proportion of Lu, Fe and Zn is 1 in atomic ratio
The mixture is mixed at a ratio of 1:9, and the mixture is heated at a temperature of 700°C or higher in air, an oxidizing atmosphere, or Lu
and Fe in a trivalent ion state, and Zn in a divalent ion state by heating in a reducing atmosphere in which they are not reduced. Commercially available starting materials may be used as they are, but in order for the chemical reaction to proceed quickly, it is better to have a small particle size, especially 10 μm.
It is preferable that it is below. Further, when used as a magnetic material or a semiconductor material, it is preferable to have high purity since contamination with impurities is avoided. Examples of compounds whose starting materials yield metal oxides by heating include hydroxides, carbonates, and nitrates of the respective metals. The raw materials are thoroughly mixed as is or together with alcohols, acetone, etc. The mixing ratio of the raw materials needs to be such that the ratio of Lu, Fe, and Zn is 1:1:9 in atomic ratio.
If this is removed, a single phase of the target compound cannot be obtained. This mixture is stored in the air, in an oxidizing atmosphere, or
Lu and Fe are each in a trivalent ion state, and Zn is each in a 2-valent state.
In a reducing atmosphere that does not reduce from the valent ion state
Heat over 700℃. Heating time is several hours or more. There are no restrictions on the rate of temperature increase during heating. After heating, it can be rapidly cooled, or it can be rapidly drawn out into the atmosphere. The obtained LuFeZn 9 O 12 compound powder was brown in color and was found to have a crystalline structure by powder X-ray diffraction. Its crystal structure is layered,
It was found that it was formed by stacking 1.5 layers of LuO, 2.5 layers of (Fe, Zn)O, and a layer of ZnO. Example Lutetium oxide (Lu 2 O 3 ) with a purity of 99.99% or more
Powder, iron oxide (Fe 2 O 3 ) powder with a purity of 99.9% or more,
Weigh out reagent-grade zinc oxide (ZnO) powder at a molar ratio of 1:1:14, add ethanol in an agate mortar, and mix for about 30 minutes to obtain a fine powder mixture with an average particle size of several μm. Ta. The mixture was sealed in a platinum tube, placed in a tubular siliconite furnace set at 1450°C, and heated for 7 days, after which the sample was taken out of the furnace and rapidly cooled to room temperature. The obtained sample is a single phase of LuFeZn 9 O 12 ,
Table 2 shows the results of measuring each plane index (hkl), plane spacing ( dp ), and relative reflection intensity by powder X-ray diffraction. The lattice constants as a hexagonal crystal system were a=3.297±0.001 (Å) and c=87.84±0.01 (Å). The above lattice constants and the surface index (hkl) in Table 2
The calculated interplanar spacing (d c (Å)) was in extremely good agreement with the actually measured interplanar spacing (d p (Å)). Effects of the Invention The present invention provides novel compounds useful as magnetic materials, semiconductor materials, and catalysts.
Claims (1)
を有する化合物。 2 金属ルテチウムあるいは酸化ルテチウムもし
くは加熱により酸化ルテチウムに分解される化合
物と、金属鉄あるいは酸化鉄もしくは加熱により
酸化鉄に分解される化合物と、金属亜鉛あるいは
酸化亜鉛もしくは加熱により酸化亜鉛に分解され
る化合物と、Lu,FeおよびZnの割合が原子比で
1対1対9の割合で混合し、該混合物を700℃以
上の温度で大気中、酸化性雰囲気中あるいはLu
およびFeが各々3価イオン状態、Znが2価イオ
ン状態より還元されない還元雰囲気中で加熱する
ことを特徴とするLuFeZn9O12で示される六方晶
系の層状構造を有する化合物の製造法。[Claims] 1. A compound having a hexagonal layered structure represented by LuFeZn 9 O 12 . 2 Metallic lutetium or lutetium oxide or a compound that is decomposed into lutetium oxide by heating; Metallic iron or iron oxide or a compound that is decomposed into iron oxide by heating; and Metallic zinc or zinc oxide or a compound that is decomposed into zinc oxide by heating. and Lu, Fe, and Zn in an atomic ratio of 1:1:9, and the mixture is exposed to air, oxidizing atmosphere, or Lu at a temperature of 700°C or higher.
A method for producing a compound having a hexagonal layered structure represented by LuFeZn 9 O 12 , which comprises heating in a reducing atmosphere in which Fe is not reduced to a trivalent ion state and Zn is not reduced to a divalent ion state.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP62129053A JPS63295434A (en) | 1987-05-26 | 1987-05-26 | Compound shown by lufezn9o12 and having hexagonal lamellar structure and its production |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP62129053A JPS63295434A (en) | 1987-05-26 | 1987-05-26 | Compound shown by lufezn9o12 and having hexagonal lamellar structure and its production |
Publications (2)
Publication Number | Publication Date |
---|---|
JPS63295434A JPS63295434A (en) | 1988-12-01 |
JPH0435419B2 true JPH0435419B2 (en) | 1992-06-11 |
Family
ID=14999920
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP62129053A Granted JPS63295434A (en) | 1987-05-26 | 1987-05-26 | Compound shown by lufezn9o12 and having hexagonal lamellar structure and its production |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS63295434A (en) |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH07106923B2 (en) * | 1993-05-26 | 1995-11-15 | 株式会社シギヤ精機製作所 | Flat glass breaking method and related equipment |
-
1987
- 1987-05-26 JP JP62129053A patent/JPS63295434A/en active Granted
Also Published As
Publication number | Publication date |
---|---|
JPS63295434A (en) | 1988-12-01 |
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Legal Events
Date | Code | Title | Description |
---|---|---|---|
EXPY | Cancellation because of completion of term |