JPS5943412B2 - Compound having hexagonal layered structure represented by LuFeMnO↓4 and method for producing the same - Google Patents

Compound having hexagonal layered structure represented by LuFeMnO↓4 and method for producing the same

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Publication number
JPS5943412B2
JPS5943412B2 JP56050139A JP5013981A JPS5943412B2 JP S5943412 B2 JPS5943412 B2 JP S5943412B2 JP 56050139 A JP56050139 A JP 56050139A JP 5013981 A JP5013981 A JP 5013981A JP S5943412 B2 JPS5943412 B2 JP S5943412B2
Authority
JP
Japan
Prior art keywords
compound
layered structure
lufemno
structure represented
hexagonal layered
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
Application number
JP56050139A
Other languages
Japanese (ja)
Other versions
JPS57166320A (en
Inventor
昇 君塚
英治 高山
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
KAGAKU GIJUTSUCHO MUKIZAISHITSU KENKYUSHOCHO
Original Assignee
KAGAKU GIJUTSUCHO MUKIZAISHITSU KENKYUSHOCHO
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by KAGAKU GIJUTSUCHO MUKIZAISHITSU KENKYUSHOCHO filed Critical KAGAKU GIJUTSUCHO MUKIZAISHITSU KENKYUSHOCHO
Priority to JP56050139A priority Critical patent/JPS5943412B2/en
Publication of JPS57166320A publication Critical patent/JPS57166320A/en
Publication of JPS5943412B2 publication Critical patent/JPS5943412B2/en
Expired legal-status Critical Current

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  • Compounds Of Iron (AREA)
  • Hard Magnetic Materials (AREA)

Description

【発明の詳細な説明】 本発明は新規化合物であるLuFeMn04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 The present invention relates to a novel compound, LuFeMn04, having a hexagonal layered structure and a method for producing the same.

従来、YFe2qで示される六方晶系の層状構造を有す
る化合物は知られる、っこの化合物はY3+ 。
Conventionally, a compound having a hexagonal layered structure represented by YFe2q is known, and this compound is Y3+.

Fe2+Fe3+OH−で示されるように、鉄の2価イ
オンと3価イオンは5配位の酸素イオンに囲まれ、Yは
6配位の酸素イオンをその周りに持つている化合物であ
り、磁性を持つている。本発明は前記Y3+Fe2+
Fe3+OV化合物 ・のY3+の代りにLu3Ar″
、Fe2+の代りにMn奸を置きかえた新規な化合物お
よびその製造法を提供するにある。
As shown by Fe2+Fe3+OH-, the divalent and trivalent ions of iron are surrounded by five-coordinated oxygen ions, and Y is a compound that has six-coordinated oxygen ions around it, and is magnetic. ing. The present invention provides the Y3+Fe2+
Lu3Ar″ instead of Y3+ in Fe3+OV compound
The object of the present invention is to provide a novel compound in which Mn gas is substituted for Fe2+, and a method for producing the same.

本発明のLuFeMn0lで示される化合物は、この化
合物中、鉄はFe3+イオン、マンガンはMn2+、L
uは3価イオンとして存在しており、Lu3+Fも+M
n1oH−として表わすことができる。
In the compound represented by LuFeMn0l of the present invention, iron is Fe3+ ion, manganese is Mn2+, L
u exists as a trivalent ion, and Lu3+F is also +M
It can be expressed as n1oH-.

この結晶は第1図に示すような六方晶系の層状構造を持
つている。図中最大の丸は酸素、最小の黒丸はFeとM
nを、中丸はLuを示す。FeとMnはランダムに入つ
ている。マンガンの2価イオンと鉄の3価イオンは5配
位の酸素イオンによつて囲まれ、結晶学的には同一の位
置を占めている。またLuは6配位の酸素ををその周り
に持つている。陰イオンである酸素は緻密構造をとつて
いる。この結晶の面指数(hKl)、面間隔(dA)(
doは実測dcは計算値を示す)、X線に対する相対反
射強度(I%)は第1表の通りである。
This crystal has a hexagonal layered structure as shown in FIG. The largest circle in the figure is oxygen, and the smallest black circle is Fe and M.
n and the middle circle indicates Lu. Fe and Mn are entered randomly. Divalent ions of manganese and trivalent ions of iron are surrounded by five-coordinated oxygen ions and occupy the same position crystallographically. Moreover, Lu has six-coordinated oxygen around it. Oxygen, an anion, has a dense structure. The plane index (hKl) and the plane spacing (dA) of this crystal (
(do is actually measured dc is a calculated value), and the relative reflection intensity (I%) for X-rays is as shown in Table 1.

そして空間群はR3mで、ぞの晶癖は板状晶で、格子定
数は下記の通りである。ao■ 3.4450±O、0
004(A)Q■25.632±O、007(A)第1
表れKldo〔A−ldcCA〕 I〔%〕0038.
5578.544830064.27 4 4.2 7
2 3 8101 2.9 9 6 2.9 6 3
10 010 2 2.9 09 2.9 0 6
70 09 2.8 4 8 2.8 48 4610
4 2.7 0 6 2.7 0 5 9 210
5 2.5 7 9 2.5 7 9 6 910 7
2.312 4 2.312 9 17108 2.
1824 2.1834 281010 1.9 4
3 5 1.9 4 4 2 3 5110 1.72
31 1.7225 491131.68901.68
851010131.64621.644912116
1.59751.597517この化合物は磁性材料な
らびに半導体材料として有用なものである。
The space group is R3m, the crystal habit is plate-like, and the lattice constant is as follows. ao ■ 3.4450±O, 0
004(A)Q■25.632±O, 007(A) 1st
Expression Kldo [A-ldcCA] I [%] 0038.
5578.544830064.27 4 4.2 7
2 3 8101 2.9 9 6 2.9 6 3
10 010 2 2.9 09 2.9 0 6
70 09 2.8 4 8 2.8 48 4610
4 2.7 0 6 2.7 0 5 9 210
5 2.5 7 9 2.5 7 9 6 910 7
2.312 4 2.312 9 17108 2.
1824 2.1834 281010 1.9 4
3 5 1.9 4 4 2 3 5110 1.72
31 1.7225 491131.68901.68
851010131.64621.644912116
1.59751.597517 This compound is useful as a magnetic material as well as a semiconductor material.

この化合物は次の方法によつて製造し得られる。This compound can be produced by the following method.

ルテチウム酸化物(Lu2O3)、マンガン酸化物(M
nO)および酸化鉄(Fe2O3)を、モル比で約1対
2対1の割合で混合し、該混合物を非酸化性雰囲気下で
900℃以下の温度で加熱することによつて製造するこ
とができる。本発明に用いるルテチウム酸化物は市販の
ものをそのまま使用してもよいが、酸化物相互の反応を
速やかに進行させるためには、粒径が小さい程よく、特
に10μm以下であることが好ましい。
Lutetium oxide (Lu2O3), manganese oxide (M
nO) and iron oxide (Fe2O3) in a molar ratio of about 1:2:1, and heating the mixture at a temperature of 900 ° C. or less in a non-oxidizing atmosphere. can. Commercially available lutetium oxides used in the present invention may be used as they are, but in order to speed up the reaction between the oxides, the smaller the particle size, the better, particularly preferably 10 μm or less.

また磁性材料として用いる場合は不純物の混入をきらう
ので、原料は純度が高く、また約1000℃で数時間空
気中で仮焼したものが望ましい。酸化マンガンは通常の
試薬特級程度のものでよい。粒径は前記ルテチウム酸化
物と同様な理由で10μm以下であることが好ましい。
また、1000℃で1日間炭酸ガスと水素の混合ガス(
混合比容量で1対1)中で仮焼し、O℃に急冷させたも
のが反応が早くなるので好ましい。酸化鉄は試薬特級程
度のものでよい。その粒径は前記と同様に10μm以下
であることが好ましい。また800℃で1日間空気中で
仮焼したものが好ましい。これらの原料をそのまま、あ
るいはアルコール類、アセトン等を入れ十分混合する。
これらの混合割合はLU2O3、Fe2O!をモル比で
1対2対1の割合である。
When used as a magnetic material, since contamination with impurities is to be avoided, the raw material should preferably be of high purity and should have been calcined in air at about 1000° C. for several hours. Manganese oxide of ordinary reagent grade level may be used. The particle size is preferably 10 μm or less for the same reason as the lutetium oxide.
In addition, a mixed gas of carbon dioxide and hydrogen (
Preferably, the mixture is calcined in a mixing ratio of 1:1 (volume ratio: 1:1) and rapidly cooled to 0° C., since the reaction speeds up. The iron oxide may be of special reagent grade. As mentioned above, the particle size is preferably 10 μm or less. Moreover, it is preferable to calcined in air at 800° C. for one day. These raw materials are thoroughly mixed as they are or with alcohol, acetone, etc. added.
These mixing ratios are LU2O3, Fe2O! The molar ratio is 1:2:1.

この割合をはずれると目的とする層状化合物を得ること
ができない。これらの混合物を石英またはガラスの容器
に封入して非酸化性雰囲気下で加熱する。それはマンガ
ンが2価の状態であるので、酸化性雰囲気(例えば大気
中)下ではマンガンが酸化されて3価になつてしまうの
で、非酸化性雰囲気下であることが必要である。加熱温
度は900℃以上であればよく、また加熱時間は10分
以上、好ましくは1時間以上である。加熱の際の昇温速
度は制約はない。反応終了後はO℃に急冷するかあるい
は大気中に急激に引出せばよい。得られたLuFeMn
O4化合物は、黒色金属光沢を有し、粉末X線回折法に
よつて結晶構造を有することが分つた。
If this ratio is exceeded, the desired layered compound cannot be obtained. These mixtures are sealed in a quartz or glass container and heated under a non-oxidizing atmosphere. Since manganese is in a divalent state, in an oxidizing atmosphere (for example, in the atmosphere), manganese will be oxidized and become trivalent, so it is necessary to be in a non-oxidizing atmosphere. The heating temperature may be 900°C or higher, and the heating time is 10 minutes or more, preferably 1 hour or more. There are no restrictions on the rate of temperature increase during heating. After the reaction is completed, it may be rapidly cooled to 0°C or rapidly drawn out into the atmosphere. The obtained LuFeMn
The O4 compound had a black metallic luster and was found to have a crystalline structure by powder X-ray diffraction.

化合物中の鉄イオンの価数はメスバウエル効果の測定で
、またマンガンイオンの価数は試料を空気中で加熱する
際の試料の重量変化を測定する重量分析法によつて決定
した。実施例純度99.9%以上のルテチウム酸化物(
LU2O3)粉末、純度99.9%以上の酸化マンガン
(MnO)粉末および純度99.9%以上の鉄酸化物(
Fe2O3)粉末をモル比で1対2対1の割合に秤量し
、乳鉢内でアセトンを加えて十分に混合して平均粒径数
μmの微粉末混合物を得た。
The valence of iron ions in the compound was determined by measuring the Mössbauer effect, and the valence of manganese ions was determined by gravimetric analysis, which measures the change in weight of the sample when it is heated in air. Example: Lutetium oxide with a purity of 99.9% or more (
LU2O3) powder, manganese oxide (MnO) powder with a purity of 99.9% or more, and iron oxide (MnO) powder with a purity of 99.9% or more.
Fe2O3) powder was weighed at a molar ratio of 1:2:1, acetone was added in a mortar, and the mixture was thoroughly mixed to obtain a fine powder mixture with an average particle size of several μm.

該混合物を透明石英管(内径8mm)内に入れて真空ポ
ンプを用いて管内を1σ3mmHgの真空度に下げ、約
1時間維持し、ガスバーナーで溶封した。これを100
00Cに設定された箱型のシリコニツト炉内に入れ、約
1日間加熱し、その後試料を取出し、室温まで急速に冷
却した。得られたものはLuFeMnO4の六方晶系の
層状化合物であつた。その結晶の性状は第1表に示す。
通りであつた。
The mixture was placed in a transparent quartz tube (inner diameter 8 mm), the vacuum inside the tube was lowered to 1σ3 mmHg using a vacuum pump, the vacuum was maintained for about 1 hour, and the tube was melt-sealed with a gas burner. This is 100
The sample was placed in a box-shaped siliconite furnace set at 00C and heated for about 1 day, after which the sample was removed and rapidly cooled to room temperature. What was obtained was a hexagonal layered compound of LuFeMnO4. The properties of the crystal are shown in Table 1.
It was hot on the street.

【図面の簡単な説明】[Brief explanation of drawings]

図面は本発明のLuFeMnO4の結晶構造の図である
。 中丸・・・・・・LUl最小黒丸・・・・・・Feおよ
びMnl最大丸・・・・・・酸素。
The drawing is a diagram of the crystal structure of LuFeMnO4 of the present invention. Middle circle...LUl smallest black circle...Fe and Mnl largest circle...oxygen.

Claims (1)

【特許請求の範囲】 1 LuFeMnO_4で示される六方晶系の層状構造
を有する化合物。 2 ルテチウム酸化物(Lu_2O_3)、マンガン酸
化物(MnO)および酸化鉄(Fe_2O_3)を、モ
ル比で約1対2対1の割合で混合し、この混合物を非酸
化性雰囲気下で900℃以上の温度で加熱することを特
徴とするLuFeMnO_4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 LuFeMnO_4. 2 Lutetium oxide (Lu_2O_3), manganese oxide (MnO) and iron oxide (Fe_2O_3) are mixed in a molar ratio of approximately 1:2:1, and this mixture is heated at 900°C or higher in a non-oxidizing atmosphere. A method for producing a compound having a hexagonal layered structure represented by LuFeMnO_4, which comprises heating at a certain temperature.
JP56050139A 1981-04-03 1981-04-03 Compound having hexagonal layered structure represented by LuFeMnO↓4 and method for producing the same Expired JPS5943412B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP56050139A JPS5943412B2 (en) 1981-04-03 1981-04-03 Compound having hexagonal layered structure represented by LuFeMnO↓4 and method for producing the same

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP56050139A JPS5943412B2 (en) 1981-04-03 1981-04-03 Compound having hexagonal layered structure represented by LuFeMnO↓4 and method for producing the same

Publications (2)

Publication Number Publication Date
JPS57166320A JPS57166320A (en) 1982-10-13
JPS5943412B2 true JPS5943412B2 (en) 1984-10-22

Family

ID=12850809

Family Applications (1)

Application Number Title Priority Date Filing Date
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Country Status (1)

Country Link
JP (1) JPS5943412B2 (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06347424A (en) * 1993-06-08 1994-12-22 Hamamatsu Photonics Kk Soft x-ray nondestructive examination device
JPH0715673U (en) * 1993-08-31 1995-03-17 株式会社サンキプラン Work conveyor

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6758894B1 (en) * 2003-04-17 2004-07-06 The Shepherd Color Company Strontium iron manganese black pigment

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06347424A (en) * 1993-06-08 1994-12-22 Hamamatsu Photonics Kk Soft x-ray nondestructive examination device
JPH0715673U (en) * 1993-08-31 1995-03-17 株式会社サンキプラン Work conveyor

Also Published As

Publication number Publication date
JPS57166320A (en) 1982-10-13

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