JPS63295427A - Compound shown by tmgazn9o12 and having hexagonal lamellar structure and its production - Google Patents
Compound shown by tmgazn9o12 and having hexagonal lamellar structure and its productionInfo
- Publication number
- JPS63295427A JPS63295427A JP12906987A JP12906987A JPS63295427A JP S63295427 A JPS63295427 A JP S63295427A JP 12906987 A JP12906987 A JP 12906987A JP 12906987 A JP12906987 A JP 12906987A JP S63295427 A JPS63295427 A JP S63295427A
- Authority
- JP
- Japan
- Prior art keywords
- layer
- compound
- compd
- heated
- oxide
- 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
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 15
- 239000011701 zinc Substances 0.000 claims description 12
- ZIKATJAYWZUJPY-UHFFFAOYSA-N thulium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Tm+3].[Tm+3] ZIKATJAYWZUJPY-UHFFFAOYSA-N 0.000 claims description 10
- 229910052733 gallium Inorganic materials 0.000 claims description 8
- 150000002500 ions Chemical class 0.000 claims description 8
- 239000011787 zinc oxide Substances 0.000 claims description 7
- 229910052775 Thulium Inorganic materials 0.000 claims description 6
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 229910001195 gallium oxide Inorganic materials 0.000 claims description 5
- 229910052725 zinc Inorganic materials 0.000 claims description 5
- 230000001590 oxidative effect Effects 0.000 claims description 3
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 11
- 239000004065 semiconductor Substances 0.000 abstract description 5
- 239000003054 catalyst Substances 0.000 abstract description 4
- 239000013078 crystal Substances 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 2
- 238000003475 lamination Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 description 8
- 239000000843 powder Substances 0.000 description 6
- 230000003287 optical effect Effects 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 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
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 239000008204 material by function Substances 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
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 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
- 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
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- FRNOGLGSGLTDKL-UHFFFAOYSA-N thulium atom Chemical compound [Tm] FRNOGLGSGLTDKL-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G15/00—Compounds of gallium, indium or thallium
- C01G15/006—Compounds containing, besides gallium, indium, or thallium, two or more other elements, with the exception of oxygen or hydrogen
Abstract
Description
【発明の詳細な説明】
産業上の利用分計
本発明は光機能材料、半導体材料及び触媒材料として有
用な新規化合物であるＴｗ＋ＧａＺｎ＠Ｊ２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 Industrial Application The present invention relates to a compound having a hexagonal layered structure represented by Tw+GaZn@J2, which is a new compound useful as an optical functional material, a semiconductor material, and a catalyst material, and its production. Regarding the law.
従来技術
従来、（マｂ”Ｆｅ”０３）＠Ｆｅ”ｅｌ（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 (Mab"Fe"03)@Fe"el (n is an integer) was synthesized by the present applicant and is known.
ＹｂＦｅ２１５４． Ｙｂ１ＦｅｌＯｙ、 Ｙｂ１Ｆｅ
４６Ｂ、及びＹｂ１Ｆｅ４６Ｂ １の六方晶系としての
格子定数、Ｙｂ１５． 、、層、 Ｆｅ６．、ｇ層＃
Ｆ＠＊０ｍ ａｓ層の単位格子内におけろ暦数を示すと
表−１の通りである。YbFe2154. Yb1FelOy, Yb1Fe
46B, and the lattice constant of Yb1Fe46B 1 as a hexagonal system, Yb15. , , layer, Fe6. , g-layer #
Table 1 shows the calendar numbers in the unit cell of the F@*0m as layer.
これらの化合物は酸化鉄（Ｆｅｅ） １モルに対して、
ＹｂＦｅＱａがｎモル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。These compounds are based on 1 mole of iron oxide (Fee),
It is a compound with a layered structure that is thought to be composed of n moles of YbFeQa.
発明の目的
本発明は（ＹｂＦｅ１５３）ｎＦｅｅ＋の化学式におい
て、ｎ＝ｌ／、に相当しＹｂ″４の代わりにＴｗｓ”を
Ｆｅ”の代わりにＧａ”を、Ｆｅ”の代わりに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。Purpose of the Invention The present invention is based on the chemical formula of (YbFe153)nFee+, which corresponds to n=l/, and replaces Yb'4 with Tws, Fe' with Ga', and Fe' with Zn'. The object of the present invention is to provide novel compounds.
発明の構成
本発明のＴｍＧａＺｎ＠Ｊ２で示される化合物は、イオ
ン結晶モデルでは、Ｔｍ３°（Ｇａ”Ｚｎ”）Ｚｎ＠”
ｅ１１２”−として記載され、その構造は７ｓ＋０１−
ｑ層、 （Ｇａ’。Structure of the Invention In the ionic crystal model, the compound represented by TmGaZn@J2 of the present invention has Tm3°(Ga"Zn")Zn@"
e112”-, its structure is 7s+01-
q layer, (Ga'.
Ｚｎ２′″）ｅｆｔ 、ｓ層およびＺｎＯ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”のＩ ／、はＧａ”
と共に（Ｇａ”°、Ｚｎ２°）’ｊｉ ａｓ層を作り、
残りの・／、はＺｎ０層を作っている。六方晶系として
の格子定数は次の通りである。It is formed by stacking Zn2''')ft, s layer and ZnO layer, and one of its characteristics is that it has remarkable structural anisotropy.I/, of Zn'' is Ga''
Together with (Ga"°, Zn2°) 'ji as layer is created,
The remaining / makes up the Zn0 layer. The lattice constants as a hexagonal crystal system are as follows.
＊＝３．２９２±０．００１（Ａ）
ｃ＝８７．７０±０．０１ （Ａ）
この化合物の面指数（ｈ ｋ ｔ ）、面間隔（ｄ（Ａ
））（ｄＯは実測値ｐ ｄＣは計算値を示す）およびＸ
線に対する相対反射強度（■ ％）を示すと表−２の通
りである。*=3.292±0.001 (A) c=87.70±0.01 (A) Planar index (h k t ), plane spacing (d(A
)) (dO is the measured value p dC is the calculated value) and X
Table 2 shows the relative reflection intensity (%) for the line.
この化合物は光機能材料、半導体材料および触媒材料等
に有用なものである。This compound is useful for optical functional materials, semiconductor materials, catalyst materials, and the like.
表 −２ 乙の化合物は次の方法によって製造し得られる。Table-2 Compound B can be produced by the following method.
金属ツリウムあるいは酸化ツリウムもしくは加熱により
酸化ツリウムに分解される化合物と、金属ガリウムある
いは酸化ガリウムもしくは加熱により酸化ガリウムに分
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、Ｔｗ＋、
Ｇａ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６００℃以上の温度で、大気中、酸化
性雰囲気中あるいはＴｍおよびＧａ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 thulium or thulium oxide or a compound that is decomposed into thulium oxide by heating; Metallic gallium or gallium oxide or a compound that is decomposed into gallium oxide by heating; Metallic zinc or zinc oxide or a compound that is decomposed into zinc oxide by heating. ,Tw+,
Ga and Zn are mixed in an atomic ratio of 1:1:9, and the mixture is heated at a temperature of 600°C or higher in the air, an oxidizing atmosphere, or in a state where Tm and Ga are each in a trivalent ion state and Zn is in a trivalent ion state. It can be produced by heating in a reducing atmosphere that does not reduce the divalent ion 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、光機能材料、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。Further, when used as an optical functional material or a semiconductor material, it is preferable to have high purity since contamination with impurities is avoided.
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
られろ。Examples of compounds whose starting materials yield metal oxides by heating include hydroxides, carbonates, and nitrates of the respective metals.
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、Ｔ＊、 Ｇａ、及び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−相を得ることができ
ない。The mixing ratio of the raw materials requires that the ratio of T*, Ga, and Zn be in an atomic ratio of 1:1:9. If this is removed, a single phase of the target compound cannot be obtained.
この混合物を大気中、酸化性雰囲気中あるいはＴ■およ
びＧａ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６００℃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。This mixture is heated at 600° C. or higher in the air, an oxidizing atmosphere, or a reducing atmosphere in which T and Ga 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 drawn out into the atmosphere.
得られたＴｍＧａＺｎ＠ｆ５□化合物の粉末は無色であ
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１） 、Ｔ＋５１
５１ 、ｓ層、 （Ｇａ、 Ｚｎ）ｅｌｌ、５層、＄ｊ
ヨヒＺｎＯ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 TmGaZn@f5□ compound powder was colorless and was found to have a crystalline structure by powder X-ray diffraction. Its crystal structure is a layered structure1), T+51
51, s layer, (Ga, Zn)ell, 5 layers, $j
It was found that it was formed by stacking ZnO layers.
実施例
純度９９．９９％９％以上化ツリウム（Ｔ■２０３）粉
末、純度９９．９％以上の酸化ガリウム（Ｇａ１５３）
粉末、試薬特級の酸化亜鉛（Ｚｎ（５）粉末をモル比で
１対１対１８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、１４５
０℃に設定された管状シリフニット炉内に入れ、４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。Examples Thulium (T203) powder with a purity of 99.99% or more, gallium oxide (Ga153) with a purity of 99.9% or more
Powder, reagent grade zinc oxide (Zn(5) powder) was weighed at a molar ratio of 1:1:18, ethanol was added in an agate mortar, and the mixture was mixed for about 30 minutes to form a powder with an average particle size of several μm. A fine powder mixture was obtained.The mixture was sealed in a platinum tube and 145
The sample was placed in a tubular Silifknit furnace set at 0°C and heated for 4 days, after which the sample was taken out of the furnace and rapidly cooled to room temperature.
得られた試料は、Ｔ■にａＺｎ＠０１２単−相であり、
粉末Ｘ＠回折法によって面指数（ｈｋｘ）、面間隔（ｄ
、）および相対反射強度（１％）を測定した。その結果
は表−２の通りであった。The obtained sample was aZn@012 single-phase in T■,
Planar index (hkx), plane spacing (d
, ) and relative reflection intensity (1%) were measured. The results were as shown in Table-2.
六万品系としての格子定数は ａ＝３．２９２±０．００１（Ａ） ｃ＝８７．７０±ｏ、０１ （Ａ） であった。The lattice constant for the 60,000-product system is a=3.292±0.001(A) c=87.70±o, 01 (A) Met.
上記の格子定数および表−２の面指数（ｈ ｋ ｔ ）
より算出した面間隔（ｄＣ（Ａ））は、実測の面間隔（
ｄ ｏ （λ））と極めてよく一致していた。The above lattice constant and the surface index (h k t ) in Table 2
The surface spacing (dC(A)) calculated from the actually measured surface spacing (dC(A)) is
d o (λ)).
発明の効果
本発明は光機能材料、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 optical functional materials, semiconductor materials, and catalysts.
Claims (2)
の層状構造を有する化合物(1) Compound with hexagonal layered structure represented by TmGaZn_9O_1_2
により酸化ツリウムに分解される化合物と、金属ガリウ
ムあるいは酸化ガリウムもしくは加熱により酸化ガリウ
ム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、Ｔｍ
、Ｇａ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６００℃以上の温度で大気中、酸化
性雰囲気中あるいはＴｍおよびＧａ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ＴｍＧａＺｎ＿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 thulium or thulium oxide or a compound that decomposes into thulium oxide when heated; Metallic gallium or gallium oxide or a compound that decomposes into gallium oxide when heated; and Metallic thulium or zinc oxide or a compound that decomposes into zinc oxide when heated. and Tm
, Ga and Zn are mixed in an atomic ratio of 1:1:9, and the mixture is heated at a temperature of 600°C or higher in the air, in an oxidizing atmosphere, or in a state where Tm and Ga are each in a trivalent ion state and Zn is in a trivalent ion state. TmGaZn_9O_1 characterized by being heated in a reducing atmosphere that does not reduce the state from a divalent ion state
A method for producing a compound having a hexagonal layered structure represented by _2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12906987A JPS63295427A (en) | 1987-05-26 | 1987-05-26 | Compound shown by tmgazn9o12 and having hexagonal lamellar structure and its production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12906987A JPS63295427A (en) | 1987-05-26 | 1987-05-26 | Compound shown by tmgazn9o12 and having hexagonal lamellar structure and its production |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63295427A true JPS63295427A (en) | 1988-12-01 |
| JPH0333654B2 JPH0333654B2 (en) | 1991-05-17 |
Family
ID=15000312
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP12906987A Granted JPS63295427A (en) | 1987-05-26 | 1987-05-26 | Compound shown by tmgazn9o12 and having hexagonal lamellar structure and its production |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63295427A (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS606894A (en) * | 1983-06-24 | 1985-01-14 | 株式会社東芝 | Nuclear fuel aggregate |
-
1987
- 1987-05-26 JP JP12906987A patent/JPS63295427A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS606894A (en) * | 1983-06-24 | 1985-01-14 | 株式会社東芝 | Nuclear fuel aggregate |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0333654B2 (en) | 1991-05-17 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EXPY | Cancellation because of completion of term |