JPS63295434A - Compound shown by lufezn9o12 and having hexagonal lamellar structure and its production - Google Patents
Compound shown by lufezn9o12 and having hexagonal lamellar structure and its productionInfo
- Publication number
- JPS63295434A JPS63295434A JP62129053A JP12905387A JPS63295434A JP S63295434 A JPS63295434 A JP S63295434A JP 62129053 A JP62129053 A JP 62129053A JP 12905387 A JP12905387 A JP 12905387A JP S63295434 A JPS63295434 A JP S63295434A
- Authority
- JP
- Japan
- Prior art keywords
- compound
- compd
- layer
- oxide
- heating
- 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.)
- Granted
Links
- 150000001875 compounds Chemical class 0.000 title claims description 22
- 238000004519 manufacturing process Methods 0.000 title claims description 3
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 7
- 229910052742 iron Inorganic materials 0.000 claims abstract description 6
- 239000011701 zinc Substances 0.000 claims description 15
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 10
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 8
- 150000002500 ions Chemical class 0.000 claims description 6
- 229910052765 Lutetium Inorganic materials 0.000 claims description 5
- 229910003443 lutetium oxide Inorganic materials 0.000 claims description 5
- 239000000203 mixture Substances 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
- 239000011787 zinc oxide Substances 0.000 claims description 4
- 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
- 230000001590 oxidative effect Effects 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 9
- 239000000696 magnetic material Substances 0.000 abstract description 6
- 239000004065 semiconductor Substances 0.000 abstract description 6
- 239000003054 catalyst Substances 0.000 abstract description 4
- 239000013078 crystal Substances 0.000 abstract description 4
- 238000003475 lamination Methods 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 6
- 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
- 239000002994 raw material Substances 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 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
- 210000000481 breast Anatomy 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
- 238000002050 diffraction method 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
- 239000011630 iodine Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 238000010030 laminating 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
- 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
- 238000000634 powder X-ray diffraction Methods 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)
- Catalysts (AREA)
- Soft Magnetic Materials (AREA)
- Recrystallisation Techniques (AREA)
- Compounds Of Iron (AREA)
Abstract
Description
【発明の詳細な説明】
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ＬｕＦｓＺｎ＠５１１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。DETAILED DESCRIPTION OF THE INVENTION Field of Industrial Application The present invention relates to a compound having a hexagonal layered structure represented by LuFsZn@511, which is a new compound useful as a magnetic material, a semiconductor material, a catalyst material, etc., and a method for producing the same. Regarding.
従来技術
従来、（Ｙｂ”Ｆａ”６ｇ）＠Ｆｅ”６（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
出願人によって合成され知られている。Prior Art Conventionally, a compound having a hexagonal layered structure represented by (Yb"Fa"6g)@Fe"6 (n is an integer) was synthesized by the present applicant and is known.
ＹｂＦｅ１ｅ）４． Ｙｂ１Ｆｅ、１０７． Ｙｂ３Ｆ
ｅ４６１．、及びＹｂ４Ｆｅｓ’＋＊の六方晶系として
の格子定数、ｙｂｏ、 、、層、 Ｆｅｏｌ、５層ｐ
Ｆｅ２Ｏ２ｍ５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。YbFe1e)4. Yb1Fe, 107. Yb3F
e461. , and the lattice constant of Yb4Fes'+* as a hexagonal system, ybo, , , layer, Feol, 5 layers p
Table 1 shows the number of layers in the unit cell of the Fe2O2m5 layer.
これらの化合物は酸化鉄（Ｆｅ６） １モルに対して、
ＹｂＦｅ６１がｎ モＡ （ｎ ＝ １ ＊ ２ 、３
−）の割合で化合していると考えられろ層状構造を持つ
化合物である。These compounds are based on 1 mole of iron oxide (Fe6),
YbFe61 is n moA (n = 1 * 2, 3
-) It is considered to be a compound with a layered structure.
発明の目的
代わりにＺｎ”を置きかえて得られる新規な化合物を提
供するにある。The object of the invention is to provide a novel compound obtained by replacing Zn'' instead.
発明の構成
本発明のＬｕＦｅＺｎ＠０１２で示される化合物は、イ
オッ結晶モデルでは、Ｌｕ’◆（Ｆｅ３◆Ｚｎ”″）Ｚ
ｎ＠”０３．トとして記載され、その構造はＬｕ０１
、ｓ層、 （Ｆｅ、Ｚｎ）０２０６層およびＺｎｅ１
層の積層によって形成されており著しい構造異方性を持
っていることがその特徴の一つである。Ｚｎ”イオンの
ｌ／、はＦｅ”と共に（Ｆｅ”。Structure of the Invention In the iodine crystal model, the compound represented by LuFeZn@012 of the present invention is Lu'◆(Fe3◆Zn'')Z
It is described as n@”03.to, and its structure is Lu01
, s layer, (Fe,Zn)0206 layer and Zne1
One of its characteristics is that it is formed by laminating layers and has significant structural anisotropy. l/ of Zn'' ion is (Fe'') along with Fe''.
Ｚｎ”）６２．５層を作り、残りの・／、はＺｎｅ１層
を作ッテいる。六万品系としての格子定数は次の通りで
ある。62.5 layers of Zn'') are made, and 1 layer of Zne is made of the remaining .
ａ＝３，２９７±ｏ、ｏｏｌ（Ａ）
ｃ＝８７．８４±０．０１ （Ａ）
この化合物の面指数（ｈ ｋ ｆｆｉ ）、面間隔（ｄ
（Ａ））（ｄｏ；よ実測値、ｄｃは計算値を示す）およ
びＸ線に対する相対反射強度（１（％））を示すと表−
２の通りである。a=3,297±o, ool(A) c=87.84±0.01 (A) Planar index (h k ffi ), plane spacing (d
(A)) (do: actually measured value, dc: calculated value) and the relative reflection intensity (1 (%)) for X-rays are shown in Table-
2.
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
可能性が考えられろ。This compound is useful as a magnetic material, a semiconductor material, and a catalytic material. For example, consider the possibility of using them as magnetic materials, semiconductors, and catalyst materials that have two-dimensional properties with strong anisotropy.
表 −２ この化合物は次の方法によって製造し得られる。Table-2 This compound can be produced by the following method.
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ろ化合物と、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
とによって製造し得られる。Metallic lutetium or lutetium oxide or a compound that can be decomposed into lutetium oxide by heating; Metallic iron or iron oxide or a compound that can be decomposed into iron oxide by heating; Metallic zinc or zinc oxide or a compound that can be decomposed into zinc oxide by heating. , Lu, Fe and Zn
are mixed in an atomic ratio of 1:1:9, and the mixture is heated at a temperature of 700°C or higher in the air, in an oxidizing atmosphere, or in a state where Lu and Fe are each in a trivalent ion state and Zn is a divalent ion. It can be produced by heating in a reducing atmosphere that is not reduced by the state.
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。Commercially available starting materials for use in the present invention may be used as they are, but in order to allow the chemical reaction to proceed rapidly, it is better to have a smaller particle size, particularly preferably 10 μm or less.
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ろ化合物としては、
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。Further, when used as a magnetic material or a semiconductor material, it is preferable to have high purity since contamination with impurities is avoided. As a compound whose starting material is a metal oxide obtained by heating,
Examples include hydroxides, carbonates, and nitrates of each metal.
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。The raw materials are thoroughly mixed as they are or together with alcohols, acetone, etc.
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。The mixing ratio of the raw materials needs to be such that the atomic ratio of Lu, Fe, and Zn is 1:1:9.
これをはずすと目的とする化合物の単−相を得ることが
できない。If this is removed, a single phase of the target compound cannot be obtained.
この混合物を大気中、Ｍ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（こ急激に引き出せばよい。This mixture is heated at 700° C. or higher in the air, in an M-forming atmosphere, or in a reducing atmosphere in which Lu and Fe are not reduced from their respective trivalent ion states and Zn from their divalent ion states. 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 pulled out into the atmosphere.
得られたＬｕＦｅＺｎ＠６１２化合物の粉末は褐色であ
り、粉末Ｘ線回折法によって結晶構造を有することが分
かった。その結晶構造は層状構造であり、Ｌ ｕ ｏ
Ｉ ＩＩ ｓ層ｐ （Ｆａ、 Ｚｎ）Ｑ２．５層、およ
びＺｎ（５層の積重ねによって形成されていることが分
かった。The obtained LuFeZn@612 compound powder was brown in color and was found to have a crystal structure by powder X-ray diffraction. Its crystal structure is a layered structure, and L u o
It was found that the I II s layer p (Fa, Zn) was formed by stacking 2.5 Q layers and 5 Zn layers.
実施例
純度９９．９９％以上の酸化ルテチウム（Ｌｕ２ｅｓ）
粉末、純度９９．９％以上の酸化鉄（Ｆｌｉｌ＊ｅ）＊
）粉末。Example Lutetium oxide (Lu2es) with a purity of 99.99% or more
Powder, iron oxide (Fil*e) with a purity of 99.9% or more*
) powder.
試薬特級の酸化亜鈴（Ｚｎ６）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分間部合し、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ット炉内に入れ、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
。Weighed reagent-grade dumbbell oxide (Zn6) powder at a molar ratio of 1:1:14, added ethanol in an agate mortar, and mixed for about 30 minutes to form a fine powder mixture with an average particle size of several μm. Obtained. The mixture was sealed in a platinum tube, placed in a tubular siliconite furnace set at 1450°C, and heated for 7 days.
Thereafter, the sample was taken out of the furnace and rapidly cooled to room temperature.
得られた試料は、ＬｕＦｅＺｎ５Ｏ＋ ＊単−相であり
、粉末ｘ、Ｉ１１回折法に折流て、各面指数（ｈｋｌ）
。The obtained sample was LuFeZn5O+ *single-phase, and was analyzed by powder x, I11 diffraction method, and each surface index (hkl)
.
面間隔（ｄ、）および相対反射強度を測定した結果は表
−２の通りであった。The results of measuring the interplanar spacing (d,) and relative reflection intensity are shown in Table 2.
六方晶系としての格子定数は 乳＝３，２９７±０．００１（久） ｃ＝８７．８４±０．０１ （Ａ） であった。The lattice constant as a hexagonal system is Breasts = 3,297±0.001 (long) c=87.84±0.01 (A) Met.
上記の格子定数および表−２の面指数（ｈ ｋ ｌ ）
より算出した面間隔（ｄｃ（Ａ））は、実測の面間隔（
ｄｏ（Ａ））と極めてよく一致していた。The above lattice constant and the plane index (h k l ) in Table 2
The surface spacing (dc(A)) calculated from the actually measured surface spacing (dc(A)) is
do(A)).
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。Effects of the Invention The present invention provides novel compounds useful as magnetic materials, semiconductor materials, and catalysts.
Claims (2)
の層状構造を有する化合物(1) Compound having a hexagonal layered structure represented by LuFeZn_9O_1_2
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ＬｕＦｅＺｎ＿９Ｏ＿１＿２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。(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 heated at a temperature of 700°C or higher in the air, in an oxidizing atmosphere, or when Lu and Fe are each trivalent. ionic state, Zn is 2
A method for producing a compound having a hexagonal layered structure represented by LuFeZn_9O_1_2, which comprises heating in a reducing atmosphere that does not reduce the valence 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 true JPS63295434A (en) | 1988-12-01 |
| JPH0435419B2 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) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06340440A (en) * | 1993-05-26 | 1994-12-13 | Shigiya Seiki Seisakusho:Kk | Device for cracking sheet grass by folding and its associated device |
-
1987
- 1987-05-26 JP JP62129053A patent/JPS63295434A/en active Granted
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06340440A (en) * | 1993-05-26 | 1994-12-13 | Shigiya Seiki Seisakusho:Kk | Device for cracking sheet grass by folding and its associated device |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0435419B2 (en) | 1992-06-11 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EXPY | Cancellation because of completion of term |