JP3146346B2 - Scandium boride and method for producing the same - Google Patents
Scandium boride and method for producing the sameInfo
- Publication number
- JP3146346B2 JP3146346B2 JP17642097A JP17642097A JP3146346B2 JP 3146346 B2 JP3146346 B2 JP 3146346B2 JP 17642097 A JP17642097 A JP 17642097A JP 17642097 A JP17642097 A JP 17642097A JP 3146346 B2 JP3146346 B2 JP 3146346B2
- Authority
- JP
- Japan
- Prior art keywords
- scandium
- producing
- scb
- scandium boride
- compound
- 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.)
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- Crystals, And After-Treatments Of Crystals (AREA)
Description
【０００１】[0001]
【産業上の利用分野】この発明は、ホウ化スカンジウム
化合物及びその製造方法に関する。より詳細には熱電素
子材料や分光素子材料等として有用な新規なホウ化スカ
ンジウム化合物及びその製造方法に関する。The present invention relates to a scandium boride compound and a method for producing the same. More specifically, the present invention relates to a novel scandium boride compound useful as a thermoelectric element material, a spectroscopic element material, and the like, and a method for producing the same.
【０００２】[0002]
【従来技術】従来から高機能材料の一つとして希土類多
ホウ化物が関心を持たれており、例えばＹＢ66は、軟Ｘ
線分光素子材料として近年開発されている。また、ＹＢ
25及びＹＢ50とその希土類置換体、ホウケイ化イットリ
ウムとその希土類置換体が見出され、それらの持つ機能
が検討され、有用材料として開発されることが期待され
ている。さらに、多彩な多ホウ化物が発見、供給される
ことで、新しい機能が発現されることへの期待も大き
い。BACKGROUND OF THE INVENTION are rare multi boride as a conventionally highly functional material is interest, for example, YB 66 is a soft X
Recently, it has been developed as a material for X-ray spectroscopy. Also, YB
25 and YB 50 and its rare earth substitutions, borosilicate yttrium and its rare earth substitutions were found, functions of them are considered, it is expected to be developed as a useful material. In addition, there is great expectation that new functions will be developed by the discovery and supply of various polyborides.
【０００３】[0003]
【発明が解決しようとする課題】このような状況のもと
に本発明者は新規な希土類多ホウ化物について種々検討
した結果、新規なホウ化スカンジウムを見出し、本発明
を完成したもので、本発明の目的は、機能性材料として
実用的にも利用可能な新しいホウ化スカンジウムを提供
することである。Under such circumstances, the present inventors have conducted various studies on novel rare earth polyborides, and have found a novel scandium boride, and have completed the present invention. An object of the invention is to provide a new scandium boride that can be practically used as a functional material.
【０００４】[0004]
【課題を解決するための手段】本発明は、一般式ＳｃＢ
18+x （−３＜Ｘ＜３）で示されるホウ化スカンジウム化
合物であり、また、Ｓｃ2Ｏ3に下記の反応式（１）に基
づく割合のホウ素を混合して得た混合物をペレット状に
成形し、該ペレット状物を真空中で１５００〜１８５０
℃の温度範囲で０．５〜２時間保持して反応させること
を特徴とする一般式ＳｃＢ 18+x （−３＜Ｘ＜３）で示さ
れるホウ化スカンジウム化合物の製造方法である。 Ｓｃ2Ｏ3＋（３９＋２Ｘ）Ｂ→２ＳｃＢ 18+x ＋３ＢＯ（１）According to the present invention, there is provided a compound of the general formula ScB
18 + x is a boride scandium compound represented by (-3 <X <3), also mixture pellets obtained by mixing a boron ratio based on the reaction formula (1) below the Sc 2 O 3 And the pellets are vacuumed at 1500-1850.
A method for producing a scandium boride compound represented by the general formula ScB18 + x (-3 <X <3), wherein the reaction is carried out while maintaining the temperature in a temperature range of 0.5 to 2 hours. Sc 2 O 3 + ( 39 + 2X) B → 2ScB 18 + x + 3BO (1)
【０００５】即ち、本発明の新規なホウ化スカンジウム
化合物は、既に知られているＳｃ−Ｂ系化合物の中のＳ
ｃＢ2、ＳｃＢ12、Ｓｃドープβボロンなどの一連の化
合物に加えて、その存在が確立されたものである。この
ホウ化スカンジウム化合物の安定存在領域は、一般式で
示すと、ＳｃＢ 18+x （−３＜Ｘ＜３）であり、その結晶
構造は正方晶で、格子定数ａ＝ｂ＝１．０２８８ｎｍ、
ｃ＝１．４２４１ｎｍである。その代表組成の化合物
は、Ｘ＝０であるＳｃＢ18である。なお、係数Ｘが上記
の範囲を超えると、所定のホウ化スカンジウム化合物は
得られず、Ｘ≦−３ではＳｃＢ12が含まれるようにな
り、３≦ＸではＳｃドープβボロンが含まれるようにな
る。That is, the novel scandium boride compound of the present invention is a compound of the type known as Sc-B-based compounds.
In addition to a series of compounds such as cB 2 , ScB 12 and Sc-doped β-boron, their existence has been established. The stable existence region of this scandium boride compound is represented by ScB 18 + x (−3 <X <3) in a general formula, its crystal structure is tetragonal, and lattice constant a = b = 1.0288 nm;
c = 1.4241 nm. Compounds of the representative compositions are ScB 18 is X = 0. When the coefficient X exceeds the above range, a predetermined scandium boride compound cannot be obtained, and ScB 12 is included when X ≦ −3, and Sc-doped β boron is included when 3 ≦ X. Become.
【０００６】このホウ化スカンジウム化合物は、およそ
１８５０℃まで安定に存在するが、それを越えるとＳｃ
Ｂ12とＳｃドープβボロンの混合物に固相のまま分解す
る。The scandium boride compound exists stably up to about 1850 ° C.
Decomposed remains in a solid phase B 12 and mixtures Sc doped β boron.
【０００７】この発明の化合物の製造方法としては、Ｓ
ｃ2Ｏ3とホウ素を混合した後ペレット状に成形し、これ
を真空中（１×１０-2Ｐａ）で約１５００〜１８５０℃
の温度範囲で０．５〜１８５０時間保持して反応させる
のであって、Ｓｃ2Ｏ3とホウ素との割合は、ＳｃＢ 19 を
製造する場合は次の反応式を満足させるような量比であ
る。 Ｓｃ2Ｏ3＋４１Ｂ→２ＳｃＢ19＋３ＢＯThe process for producing the compound of the present invention includes
After mixing c 2 O 3 and boron, the mixture is formed into a pellet, which is heated to about 1500 to 1850 ° C. in a vacuum (1 × 10 −2 Pa).
At a temperature of 0.5 to 1850 hours, and the ratio of Sc 2 O 3 to boron is ScB 19 .
In the case of production, the ratio is such that the following reaction formula is satisfied. Sc 2 O 3 + 41B → 2ScB 19 + 3BO
【０００８】[0008]
【実施例】実施例１ 反応後の形式的な組成がＳｃＢ19となるように、原料と
してＳｃ2Ｏ3およびＢを、Ｓｃ2Ｏ3＋４１Ｂ→２ＳｃＢ
19＋３ＢＯに基づき、混合した。混合物を、静水圧加圧
により、ペレット状に成形した後、真空中１７００℃で
１時間反応させた。生成したペレットを乳鉢で粉砕した
後、再度静水圧加圧によりペレットとし、前記と同一条
件で二回目の反応をさせた。生成物を粉末Ｘ線回折法に
より分析し、図１のスペクトラムが得られた。これか
ら、生成物は、格子定数、ａ＝ｂ＝１．０２８８ｎｍ、
ｃ＝１．４２４１ｎｍの正方晶の結晶形をとる単一相か
らなる新規化合物であることが確認された。また、生成
物の化学分析の結果、生成物の組成はＳｃＢ18.3であっ
た。EXAMPLES Example 1 Sc 2 O 3 and B were used as raw materials and Sc 2 O 3 + 41B → 2ScB so that the formal composition after the reaction was ScB 19.
Based on 19 + 3BO, mixed. The mixture was formed into pellets by hydrostatic pressure, and then reacted at 1700 ° C. in vacuum for 1 hour. The resulting pellets were pulverized in a mortar, and then pelletized again by hydrostatic pressure, and subjected to a second reaction under the same conditions as described above. The product was analyzed by powder X-ray diffraction, and the spectrum of FIG. 1 was obtained. From this, the product has a lattice constant, a = b = 1.0288 nm,
It was confirmed that the compound was a novel compound consisting of a single phase having a tetragonal crystal form with c = 1.2412 nm. As a result of the chemical analysis of the product, the composition of the product was ScB 18. 3.
【０００９】なお、生成物の化学組成を知るための化学
分析は以下の方法で行った。まず、生成物をステンレス
の乳鉢で粉砕し、平均粒径８０μｍ程度の粉末とした。
この際、不純物としてステンレスが混入するが、これを
塩酸溶液で溶解し、洗浄して除去した。得られた粉末を
硝酸、塩酸と共に、１５０℃、１６時間加圧分解した。
得られた溶液を用い、ＳｃはＥＤＴＡを指示薬とした滴
定法により、またＢはＩＣＰ発光分光分析装置で定量分
析した。The chemical analysis for knowing the chemical composition of the product was performed by the following method. First, the product was pulverized in a stainless mortar to obtain a powder having an average particle size of about 80 μm.
At this time, stainless steel was mixed in as an impurity, which was dissolved in a hydrochloric acid solution and washed and removed. The obtained powder was decomposed under pressure at 150 ° C. for 16 hours together with nitric acid and hydrochloric acid.
Using the obtained solution, Sc was quantitatively analyzed by a titration method using EDTA as an indicator, and B was quantitatively analyzed by an ICP emission spectrometer.
【００１０】実施例２ 実施例１と同様に、反応後の形式的な組成がＳｃＢ19.5
となるように、原料としてＳｃ2Ｂ3およびＢを混合し、
同一条件で反応を行った。生成物の粉末Ｘ線回折法によ
り分析したところ、実施例１と同様の結晶系の単一化合
物であることが確認された。また生成物の化学組成はＳ
ｃＢ18.8であった。[0010] Example 2 As in Example 1, the formal composition after reaction ScB 19. 5
Sc 2 B 3 and B are mixed as raw materials so that
The reaction was performed under the same conditions. The product was analyzed by a powder X-ray diffraction method, and it was confirmed that the product was a single compound having the same crystal system as in Example 1. The chemical composition of the product is S
It was cB 18. 8.
【００１１】[0011]
【発明の効果】以上述べたように、本発明によっていま
までその存在を知ることのなかった、新規なホウ化スカ
ンジウムを提供することが可能となり、新規材料として
熱電素子材料や分光素子材料などの新しい機能材料とし
ての利用を可能とすることが出来た。As described above, according to the present invention, it is possible to provide a novel scandium boride which was not known until now, and as a new material such as a thermoelectric element material or a spectroscopic element material. It could be used as a new functional material.
【図１】実施例１におけるＳｃＢ18.3の粉末Ｘ線回折パ
タ−ンである。. ScB 18 in FIG. 1 EXAMPLE 1 3 powder X-ray diffraction pattern - is down.
フロントページの続き (56)参考文献 “Ａ Ｓｉｎｇｌｅ−Ｃｒｙｓｔａｌ Ｄｉｆｆｒａｃｔｏｍｅｔｒｙ Ｉｎ ｖｅｓｔｉｇａｔｉｏｎ ｏｆ Ｓｃａ ｎｄｉｕｍ ｉｎ β−Ｒｈｏｍｂｏｈ ｅｄｒａｌ Ｂｏｒｏｎ”，ＢＥＮＧＴ ＣＡＬＬＭＥＲ，ＪＯＵＲＮＡＬ Ｏ Ｆ ＳＯＬＩＤ ＳＴＡＴＥ ＣＨＥＭ ＩＳＴＲＹ，1978，ＶＯＬ．23，ｐ. 391−398 (58)調査した分野(Int.Cl.7，ＤＢ名) C01B 35/00 - 35/18 ＣＡ（ＳＴＮ) ＲＥＧＩＳＴＲＹ（ＳＴＮ)Continuation of the front page (56) References “A Single-Crystal Diffraction Investigation of Scandium in β-Rhombod edral Boron”, BENGT CALLMER, JOURNAL ACCESS MEM. 23, pp. 391-398 (58) Fields investigated (Int. Cl. 7 , DB name) C01B 35/00-35/18 CA (STN) REGISTRY (STN)
Claims (2)
される結晶系が正方晶系である単一相からなるホウ化ス
カンジウム化合物。1. A scandium boride compound comprising a single phase in which the crystal system represented by the general formula ScB 18 + x (−3 <X <3) is a tetragonal system .
割合のホウ素を混合して得た混合物をペレット状に成形
し、該ペレット状物を真空中で１５００〜１８５０℃の
温度範囲で０．５〜２時間保持して反応させることを特
徴とする一般式ＳｃＢ 18+x （−３＜Ｘ＜３）で示される
ホウ化スカンジウム化合物の製造方法。 Ｓｃ2Ｏ3＋（３９＋２Ｘ）Ｂ→２ＳｃＢ 18+x ＋３ＢＯ（１）2. A mixture obtained by mixing Sc 2 O 3 with boron in a ratio based on the following reaction formula (1) is formed into pellets, and the pellets are heated in a vacuum at a temperature of 1500 to 1850 ° C. A method for producing a scandium boride compound represented by the general formula ScB18 + x (-3 <X <3), wherein the reaction is carried out while maintaining the temperature for 0.5 to 2 hours. Sc 2 O 3 + ( 39 + 2X) B → 2ScB 18 + x + 3BO (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17642097A JP3146346B2 (en) | 1997-06-17 | 1997-06-17 | Scandium boride and method for producing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17642097A JP3146346B2 (en) | 1997-06-17 | 1997-06-17 | Scandium boride and method for producing the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH1111935A JPH1111935A (en) | 1999-01-19 |
| JP3146346B2 true JP3146346B2 (en) | 2001-03-12 |
Family
ID=16013394
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP17642097A Expired - Lifetime JP3146346B2 (en) | 1997-06-17 | 1997-06-17 | Scandium boride and method for producing the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3146346B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4060803B2 (en) * | 2002-03-28 | 2008-03-12 | カウンシル・オブ・サイエンティフィック・アンド・インダストリアル・リサーチ | Method for producing zirconium boride powder |
| JP4840755B2 (en) * | 2005-11-11 | 2011-12-21 | 独立行政法人物質・材料研究機構 | Rare earth polyboride-based thermoelectric conversion material doped with metal low boride and its production method |
| US11142809B2 (en) | 2015-02-10 | 2021-10-12 | Scandium International Mining Corp. | Systems and processes for recovering scandium values from laterite ores |
-
1997
- 1997-06-17 JP JP17642097A patent/JP3146346B2/en not_active Expired - Lifetime
Non-Patent Citations (1)
| Title |
|---|
| "Ａ Ｓｉｎｇｌｅ−Ｃｒｙｓｔａｌ Ｄｉｆｆｒａｃｔｏｍｅｔｒｙ Ｉｎｖｅｓｔｉｇａｔｉｏｎ ｏｆ Ｓｃａｎｄｉｕｍ ｉｎ β−Ｒｈｏｍｂｏｈｅｄｒａｌ Ｂｏｒｏｎ"，ＢＥＮＧＴ ＣＡＬＬＭＥＲ，ＪＯＵＲＮＡＬ ＯＦ ＳＯＬＩＤ ＳＴＡＴＥ ＣＨＥＭＩＳＴＲＹ，１９７８，ＶＯＬ．２３，ｐ．３９１−３９８ |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH1111935A (en) | 1999-01-19 |
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