JP3527942B2 - Scandium borocarbide and method for producing the same - Google Patents
Scandium borocarbide and method for producing the sameInfo
- Publication number
- JP3527942B2 JP3527942B2 JP2000237491A JP2000237491A JP3527942B2 JP 3527942 B2 JP3527942 B2 JP 3527942B2 JP 2000237491 A JP2000237491 A JP 2000237491A JP 2000237491 A JP2000237491 A JP 2000237491A JP 3527942 B2 JP3527942 B2 JP 3527942B2
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- scb
- scandium
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- borocarbide
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Description
【0001】[0001]
【発明の属する技術分野】本発明は、ホウ炭化スカンジ
ウム化合物およびその製造方法に関する。より詳細に
は、分光素子材料や熱電素子材料等として有用な新規な
ホウ炭化スカンジウム化合物およびその製造方法に関す
る。[0001] The present invention relates to a scandium borocarbide compound and a method for producing the same. More specifically, the present invention relates to a novel scandium borocarbide compound useful as a spectroscopic element material, a thermoelectric element material, and the like, and a method for producing the same.
【0002】[0002]
【従来の技術】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、希土類
多ホウ化物として、YB66が軟X線分光素子材料として
近年開発されている。また、新規な多ホウ化物として、
YB25および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いだされ、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、多彩な多ホウ化物類縁化合物
が発見、供給されることで、新しい機能が発現すること
への期待も大きい。Heretofore, as one of high-performance materials, rare earth and multi boride is interest, for example, as the rare earth multi boride, YB 66 is developed in recent years as a soft X-ray monochromator material I have. Also, as a new polyboride,
YB 25 and YB 50 and their rare earth substitutes, yttrium borosilicate and their rare earth substitutes have been found, their functions have been studied, and it is expected that they will be developed as useful materials. Furthermore, the discovery and supply of various polyboride-related compounds has high expectations for the development of new functions.
【0003】[0003]
【発明が解決しようとする課題】YB66軟X線分光素子
材料の熱伝導度は低く、輝度の高い放射光ビームライン
での使用に難点があり、利用できる範囲が限られてお
り、これを代替できる機能を持つ高熱伝導度材料の開発
が待たれている。軟X線分光材料としての必要条件は、
長いd−値を持つ回折面がある、電気伝導性がある、軽
い元素で構成されている、Mg、Al、Siなど測定対
象となる元素を含まない、耐熱性に優れる、などであ
る。これらを満足できる材料として多ホウ化物は他には
ない優れた材料と言える。しかし、従来知られているA
lB12などの多ホウ化物はAlを含むということの他
に、分解化合物で、大型結晶の育成が望めない。また、
ホウケイ化物はSiを含むので、適当とは言えない。Thermal conductivity of the YB 66 soft X-ray monochromator material [0008] is low, there is a drawback in the use of a high radiated light beam line luminance, have a limited range available, it Development of a high thermal conductivity material having a function that can be substituted is awaited. The requirements for a soft X-ray spectroscopic material are:
There is a diffractive surface having a long d-value, electric conductivity, constituted by a light element, does not include an element to be measured such as Mg, Al, and Si, and has excellent heat resistance. Polyboride can be said to be an excellent material that can not be satisfied as a material that can satisfy these. However, the conventionally known A
Multi borides such lB 12 to other things it includes Al, the decomposition compound, can not be expected growth of large crystals. Also,
Boricides are not suitable because they contain Si.
【0004】本発明の課題は、機能性材料として実用的
にも利用可能で、特にYB66軟X線分光素子材料を代替
できる新規な希土類多ホウ化物を提供することである。An object of the present invention is practical to also be used as functional materials is to provide a novel rare earth multi borides which can particularly replace YB 66 soft X-ray monochromator material.
【0005】[0005]
【課題を解決するための手段】本発明者は、以上の事情
に鑑み、ScB15C0.8について、鋭意研究を重ね、粉
末X線回折パターンの指数づけに成功し、その結晶構造
が立方晶であることを明らかにすると共に、その存在領
域をも明確にすることに成功した。なお、本発明者は、
ScB15C0.8について、その存在を認め、先に文献
(Y.Shi, A. Leithe-Jasper and T. Tanaka, J. Solid
State Chemistry, 148 (1999) 250)に記載したが、し
かし、粉末X線回折パターンは非常に複雑であったた
め、指数づけはできず、また、当然、結晶構造なども決
定できないままであった。すなわち、ScB15C0.8は
この文献の発表段階においては、未確認の新物質に過ぎ
なかった。Means for Solving the Problems In view of the above circumstances, the present inventors have conducted intensive studies on ScB 15 C 0.8 , succeeded in indexing the powder X-ray diffraction pattern, and have a cubic crystal structure. As well as clarifying the fact, we succeeded in clarifying its existence area. In addition, the present inventor
The existence of ScB 15 C 0.8 was recognized, and the literature (Y. Shi, A. Leithe-Jasper and T. Tanaka, J. Solid)
State Chemistry, 148 (1999) 250), however, the powder X-ray diffraction pattern was so complex that it could not be indexed and, of course, the crystal structure etc. could not be determined. That is, ScB 15 C 0.8 was only an unidentified new substance at the stage of publication of this document.
【0006】本発明は、一般式ScB(15+x)C
(0.8+y)(ただし、−0.5<x<0.5、−
0.3<y<0.4)で示される立方晶系のホウ炭化ス
カンジウム化合物である。The present invention relates to a compound of the general formula ScB ( 15 + x ) C
(0.8 + y ) ( However, -0.5 <x <0.5,-
0.3 <y <0.4) is a cubic scandium borocarbide compound.
【0007】本発明の上記化合物は、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、好ましくはペレット状に成形し、該ペレット状物
を真空中または不活性ガス雰囲気中で1500〜185
0℃の温度範囲で0.5〜5時間保持して反応させてホ
ウ化スカンジウム化合物を得る、さらに、該ホウ化スカ
ンジウム化合物に下記の反応式(2)に基づく割合のホ
ウ素および炭素を混合して得た混合物を、好ましくはペ
レット状に成形し、該ペレット状物を同様の条件で反応
させることによって製造できる。 The above compound of the present invention is obtained by mixing a mixture obtained by mixing Sc 2 O 3 with boron at a ratio based on the following reaction formula (1), preferably into a pellet, and subjecting the pellet to a vacuum. 1500 to 185 in a medium or inert gas atmosphere
A scandium boride compound is obtained by reacting the mixture at a temperature of 0 ° C. for 0.5 to 5 hours to obtain a scandium boride compound. Further, the scandium boride compound is mixed with boron and carbon in proportions based on the following reaction formula (2). The mixture thus obtained is preferably formed into a pellet, and the pellet can be reacted under the same conditions.
【0008】 [0008]
【0009】すなわち、本発明の新規なホウ炭化スカン
ジウムは、その中心組成が、既に知られているSc−B
−C系化合物であるScB17C0.25より少しホウ素量が
少なく、炭素量の多い組成であり、また、ScB15C
1.60より炭素量のみが少ない組成であるところの、B12
クラスターを構造の基本とする希土類のホウ炭化物であ
る。That is, the novel scandium borocarbide of the present invention has a central composition of Sc-B which is already known.
It is -C compound ScB 17 slightly less amount of boron than C 0.25, a high composition of carbon content, also, ScB 15 C
B 12 which is a composition having only a smaller amount of carbon than 1.60
It is a rare earth borocarbide whose basic structure is a cluster.
【0010】B12クラスターを構造の基本とするホウ炭
化物の構造の空隙は小さく、イオン半径の大きい希土類
元素を含むのは容易でないが、本発明者は、Sc−B−
C系を探索することにより、既に知られているScB17
C0.25およびScB15C1.60に加えて、新たに、一般式
ScB(15+x)C(0.8+y)( ただし、−0.
5<x<0.5、−0.3<y<0.4)で示されるホ
ウ炭化スカンジウム化合物を単一相として合成すること
に成功した。[0010] B 12 basic void structure of boric carbide clusters structure is small, but it is not easy to include a large rare earth ion radius, the present inventors have, Sc-B-
By searching the C system, the already known ScB 17
In addition to C 0.25 and ScB 15 C 1.60 , a new general formula ScB ( 15 + x ) C (0.8 + y ) ( provided that -0.
The scandium borocarbide compound represented by 5 <x <0.5, -0.3 <y <0.4) was successfully synthesized as a single phase.
【0011】このホウ炭化スカンジウム化合物の存在領
域は、一般式で示すと、一般式ScB(15+x)C
(0.8+y)( ただし、−0.5<x<0.5、−
0.3<y<0.4)であり、その結晶構造は立方晶
で、格子定数a=2.0310(1)nm、(ただし、
括弧内の数字は最終桁の誤差の範囲を示す)である。そ
の代表組成の化合物は、x=0,y=0であるScB15
C0.8である。なお、係数x,yが上記の範囲を超える
と、所定のホウ炭化スカンジウム化合物は得られず、そ
れぞれの領域で、種々の組成のホウ化スカンジウムおよ
び異なる結晶系に属する別のホウ炭化スカンジウム化合
物等との混合物となる。The scandium borocarbide compound can be represented by the general formula ScB (15+ x ) C
(0.8 + y ) ( however, -0.5 <x <0.5,-
0.3 <y <0.4) , the crystal structure is cubic, and the lattice constant a = 2.0310 (1) nm, where
The number in parentheses indicates the range of error of the last digit). The compound of the representative composition is ScB 15 where x = 0 and y = 0.
C is 0.8 . If the coefficients x and y exceed the above ranges, a predetermined scandium borocarbide compound cannot be obtained. In each region, scandium boride of various compositions and another scandium borocarbide compound belonging to a different crystal system are used. And a mixture with
【0012】YB66の熱伝導度は、室温において約2x
10-2W/cmKであるのに比し、ScB15C0.8では
1.2x10-1W/cmKであり、およそ6倍高い値を
示す。このホウ炭化スカンジウム化合物は、およそ19
00℃まで安定に存在するが、それを超えるとホウ化ス
カンジウム、別のホウ炭化スカンジウム、炭化ホウ素な
どの混合物に固相のまま分解する。[0012] Thermal conductivity of the YB 66 is about 2x at room temperature
Compared to 10 −2 W / cmK, ScB 15 C 0.8 is 1.2 × 10 −1 W / cmK, which is approximately 6 times higher. This scandium borocarbide compound contains approximately 19
It exists stably up to 00 ° C., but if it exceeds this temperature, it decomposes into a mixture of scandium boride, another scandium borocarbide, boron carbide, etc. in a solid phase.
【0013】この発明の化合物の製造方法としては、S
c2O3にホウ素を混合して得た混合物をペレット状に成
形し、これを真空中(1x10-2Pa)または不活性ガ
ス雰囲気中で1500〜1850℃、より好ましくは、
1650〜1750℃の温度範囲で、真空中での反応は
0.5〜5時間、より好ましくは、2〜3時間、不活性
ガス雰囲気中の反応では、3〜8時間、より好ましく
は、5〜6時間保持して十分反応させてホウ化スカンジ
ウム化合物を得る。The method for producing the compound of the present invention includes
A mixture obtained by mixing boron with c 2 O 3 is formed into a pellet, which is then placed in a vacuum (1 × 10 −2 Pa) or an inert gas atmosphere at 1500 to 1850 ° C., more preferably,
In a temperature range of 1650 to 1750 ° C., the reaction in a vacuum is 0.5 to 5 hours, more preferably 2 to 3 hours, and the reaction in an inert gas atmosphere is 3 to 8 hours, more preferably 5 to 5 hours. The reaction is carried out sufficiently for 6 hours to obtain a scandium boride compound.
【0014】上記温度範囲より低い温度では十分還元反
応が進まず、所望のホウ炭化スカンジウムを得ることは
できない。また、高い温度では、生成したホウ炭化スカ
ンジウムが分解し、異なる化合物の混合物となる。ま
た、反応をさせるSc2O3にホウ素を混合して得た混合
物のままでは反応が十分に進行しない恐れがあるので、
反応を容易に起こさせ、全量が反応できるように加圧成
形してペレット状にすることが望ましい。At a temperature lower than the above temperature range, the reduction reaction does not proceed sufficiently, and a desired scandium borocarbide cannot be obtained. At higher temperatures, the resulting scandium borocarbide decomposes to form a mixture of different compounds. Further, if the mixture obtained by mixing boron with Sc 2 O 3 to be reacted may not proceed sufficiently,
It is desirable that the reaction is easily caused and the pellet is formed by pressure molding so that the whole amount can be reacted.
【0015】さらに、このホウ化スカンジウム化合物に
ホウ素および炭素を混合して得た混合物をペレット状に
成形し、同様の条件で反応させて得る。Sc2O3とホウ
素、得られたホウ化スカンジウムとホウ素および炭素と
の割合は、それぞれ次の式を満足させるような量比であ
る。Further, a mixture obtained by mixing the scandium boride compound with boron and carbon is formed into a pellet, and the mixture is reacted under the same conditions. The proportions of Sc 2 O 3 and boron, and the resulting scandium boride, boron and carbon are quantitative ratios that satisfy the following equations.
【0016】 [0016]
【0017】[0017]
【実施例】実施例1
反応後の形式的な組成がScB15となるように、原料と
してSc2O3およびBを、Sc2O3 + 33B →
2ScB15 + 3BO↑に基づき混合した。混合物を
静水圧加圧(250MPa)により、ペレット状に成形
した後、真空中(1x10-2Pa)、1700℃で2時
間反応させた。BOは揮発性の物質であるから反応中の
蒸発により系外に排出される。EXAMPLES Example 1 Sc 2 O 3 and B were used as raw materials and Sc 2 O 3 + 33B → so that the formal composition after the reaction was ScB 15.
Mixed based on 2ScB 15 + 3BO}. The mixture was formed into pellets by isostatic pressing (250 MPa), and reacted in vacuum (1 × 10 −2 Pa) at 1700 ° C. for 2 hours. Since BO is a volatile substance, it is discharged out of the system by evaporation during the reaction.
【0018】反応生成したペレットを乳鉢で粉砕した
後、この化合物の組成をScB15と仮定し、形式的な組
成がScB15C0.8となるよう炭素を加え、十分混合し
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=2.0310nmの立方晶
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ScB15.0C0.79であった。[0018] After the reaction the resulting pellets were ground with a mortar, the composition of this compound assuming ScB 15, formal composition added carbon so as to be ScB 15 C 0.8, mixed well and then, again isostatic A pellet was formed by pressure, and a second reaction was performed under the same conditions as described above. The product was analyzed by powder X-ray diffraction, and the spectrum of FIG. 1 was obtained. This confirmed that the product was a novel compound consisting of a single phase having a cubic crystal form with a lattice constant a = 2.0310 nm. Further, as a result of chemical analysis of the product, the composition of the product was ScB 15.0 C 0.79 .
【0019】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、生成物をタングステ
ンカーバイドの乳鉢で粉砕し、平均粒径80μm程度の
粉末とした。得られた粉末を硝酸、塩酸とともに、15
0℃、16時間加圧分解した。得られた溶液を用い、S
cはEDTAを指示薬とした滴定法により、またBはI
CP発光分光分析装置で定量分析した。炭素は、粉末を
酸素気流中で燃焼させ、生成するCO2濃度を測定する
手法のLECO社製炭素分析装置を用い分析した。The chemical analysis for knowing the chemical composition of the product was performed by the following method. First, the product was pulverized in a tungsten carbide mortar to obtain a powder having an average particle size of about 80 μm. The obtained powder is mixed with nitric acid and hydrochloric acid in 15
The mixture was decomposed under pressure at 0 ° C. for 16 hours. Using the obtained solution, S
c is a titration method using EDTA as an indicator, and B is I
Quantitative analysis was performed with a CP emission spectrometer. The carbon was analyzed using a carbon analyzer manufactured by LECO, which measures the concentration of CO 2 generated by burning the powder in an oxygen stream.
【0020】実施例2
実施例1と同様にし、反応後の組成がScB12になるよ
うに原料としてSc2O3およびBを混合し、同一条件で
反応を行った。さらに、最終組成がScB15C0.8とな
るよう、反応生成物にホウ素と炭素を混合し、同一条件
で反応を行った。生成物を粉末X線回折法により分析し
たところ、実施例1と同様の結晶形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ScB15.1
C0.81であった。Example 2 In the same manner as in Example 1, Sc 2 O 3 and B were mixed as raw materials so that the composition after the reaction became ScB 12 , and the reaction was carried out under the same conditions. Further, boron and carbon were mixed with the reaction product so that the final composition became ScB 15 C 0.8, and the reaction was performed under the same conditions. The product was analyzed by a powder X-ray diffraction method. As a result, it was confirmed that the product was a single compound having the same crystal form as in Example 1. The chemical composition of the product was ScB 15.1
C was 0.81 .
【0021】実施例3
実施例1と同様にし、反応後の組成がScB2になるよ
うに原料としてSc2O 3およびBを混合し、同一条件で
反応を行った。さらに、最終組成がScB15C0 .8とな
るよう、反応生成物にホウ素と炭素を混合し、同一条件
で反応を行った。生成物を粉末X線回折法により分析し
たところ、実施例1と同様の結晶形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ScB14.9
C0.78であった。Embodiment 3
In the same manner as in Example 1, the composition after the reaction was ScBTwoWill be
Sc as raw materialTwoO ThreeAnd B under the same conditions
The reaction was performed. Furthermore, the final composition is ScB15C0 .8Tona
Mix boron and carbon with the reaction product
The reaction was carried out. The product was analyzed by powder X-ray diffraction.
As a result, it was a single compound having the same crystal form as in Example 1.
It was confirmed that. The chemical composition of the product is ScB14.9
C0.78Met.
【0022】[0022]
【発明の効果】以上述べたように、本発明は、新規なホ
ウ炭化スカンジウムを創出し、その製造方法を提供する
ものであり、分光素子材料や熱電素子材料として従来公
知のYB66軟X線分光素子材料に代替できる優れた新規
材料を提供することができた。As described above, according to the present invention, the present invention is to create novel boric carbide scandium, there is provided a method of manufacturing a conventionally known YB 66 soft X-ray as a spectroscopic element material and a thermoelectric element material An excellent new material that can be substituted for the spectral element material was provided.
【図1】実施例1におけるScB15.0C0.8の粉末X線
回折パターンである。FIG. 1 is a powder X-ray diffraction pattern of ScB 15.0 C 0.8 in Example 1.
───────────────────────────────────────────────────── フロントページの続き (58)調査した分野(Int.Cl.7,DB名) C01B 35/18 CA(STN) REGISTRY(STN) JSTPlus(JOIS)──────────────────────────────────────────────────続 き Continued on the front page (58) Field surveyed (Int. Cl. 7 , DB name) C01B 35/18 CA (STN) REGISTRY (STN) JSTPlus (JOIS)
Claims (2)
(0.8+y)(ただし、−0.5<x<0.5、−
0.3<y<0.4)で示される立方晶の結晶構造をと
るホウ炭化スカンジウム化合物。1. The formula ScB ( 15 + x ) C
(0.8 + y ) ( However, -0.5 <x <0.5,-
A scandium borocarbide compound having a cubic crystal structure represented by 0.3 <y <0.4) .
結晶構造をとり、熱伝導度が1.2×10 −1 W/cm
Kであるホウ炭化スカンジウム化合物。 2. A cubic crystal represented by the formula ScB 15 C 0.8
It has a crystal structure and thermal conductivity of 1.2 × 10 −1 W / cm
A scandium borocarbide compound which is K.
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