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Li4[TaN3]的合成与晶体结构解析
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"《Li4[TaN3]的制备及晶体结构》是一篇发表于2002年的学术论文,由R. Niewa、D. A. Zherebtsov、H. Borrmann和R. Kniep四位作者在德国德累斯顿马克斯·普朗克固态化学研究所共同完成。该研究旨在纪念迪特尔·芬斯克教授60岁生日。论文的核心内容集中在新型锂氮化 tantalate (V)——Li4[TaN3]的制备方法和其晶体结构的研究。 Li4[TaN3]的合成是在1470K高温下进行的,通过将Li15[CrN4]2N与焊接的钽管内壁反应,同时在金属锂的存在下进行。这一过程显示出其独特的合成途径,对于理解锂基化合物的形成机制具有重要意义。 实验结果显示,Li4[TaN3]形成了无色的单晶(板状),空间群为Ibca,即No.73,具有相应的晶格参数:a=491.85(4) pm,b=973.59(6) pm,c=1415.0(1) pm,Z=8,R1=0.0288。这些数值表明其晶体结构呈现出Li2O的超结构特征,暗示着锂离子在化合物中的有序排列可能对整体性能有显著影响。 论文的引言部分指出,近十年来,三元和高氮化金属盐的研究领域发展迅速,尤其是无机固体材料科学中的一个重要分支。Li4[TaN3]作为这一领域内的新成员,它的发现和结构分析不仅提供了新的化学组合的可能性,也为理解氮化物材料的物理性质和潜在应用提供了宝贵的线索。 这篇论文对于理解Li4[TaN3]的合成条件、晶体生长机制以及其可能的化学和物理性质具有重要的参考价值,对于从事固态化学、材料科学和电池技术等领域的研究人员来说,是不可或缺的参考资料。"
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Preparation and Crystal Structure of Li
4
[TaN
3
]
R. Niewa*, D. A. Zherebtsov, H. Borrmann, and R. Kniep
Dresden, Max-Planck-Institut für Chemische Physik fester Stoffe
Received June 21st, 2002.
Dedicated to Professor Dieter Fenske on the Occasion of his 60
th
Birthday
Abstract. The new lithium nitridotantalate(V), Li
4
[TaN
3
], was pre-
pared by reaction of Li
15
[CrN
4
]
2
N with the wall of a welded Ta
ampoule in the presence of metallic Li at 1470 K. Li
4
[TaN
3
]forms
colourless single crystals (platelets, space group Ibca, No. 73, a ⫽
491.85(4) pm, b ⫽ 973.59(6) pm, c ⫽ 1415.0(1) pm, Z ⫽ 8, R1 ⫽
0.0288). The crystal structure is described as Li
2
O superstructure
Synthese und Kristallstruktur von Li
4
[TaN
3
]
Inhaltsübersicht. Das neue Lithiumnitridotantalat(V) Li
4
[TaN
3
]
wurde durch Umsetzung von Li
15
[CrN
4
]
2
N mit der Wand einer Ta-
Ampulle bei 1470 K einkristallin erhalten. Li
4
[TaN
3
] kristallisiert
in Form von farblosen Plättchen (Raumgruppe Ibca, Nr. 73, a ⫽
491,85(4) pm, b ⫽ 973,59(6) pm, c ⫽ 1415,0(1) pm, Z ⫽ 8, R1 ⫽
Introduction
In the last decade, the study of ternary and higher nitrido-
metalates has been a rapidly growing field of inorganic solid
state chemistry [1⫺3]. As one branch, ternary lithium nitri-
dometalates have attracted considerable attention. The reac-
tion product(s) in many nitride-systems often strongly de-
pend not only on the reaction conditions, but also on the
starting materials chosen [2]. For some time now, we are
trying to prepare new nitridocompounds from ternary nitri-
dometalates via decomposition reactions in different atmos-
pheres [4, 5], or by conversion reactions starting from ter-
nary nitridocompounds [6, 7]. These approaches already
were successful to gain products that can not be prepared
by direct reactions from the respective binaries or elements,
or to yield samples of higher purity. Here we report on a
new lithium nitridotantalate(V), Li
4
[TaN
3
], prepared by re-
dox-reaction of a ternary nitridochromate(VI) and elemen-
tal tantalum in the presence of excess lithium.
Experimental
All manipulations were carried out in an argon filled glove box
(p(O
2
,H
2
O) < 0.1 ppm). Single crystals of Li
4
[TaN
3
] were prepared
* Dr. R. Niewa
MPI für Chemische Physik fester Stoffe
Nöthnitzer Str. 40
D-01187 Dresden
e-mail: niewa@cpfs.mpg.de
Z. Anorg. Allg. Chem. 2002, 628, 2505⫺2508 WILEY-VCH Verlag GmbH, 69451 Weinheim, Germany, 2002 0044⫺2313/02/628/2505⫺2508 $ 20.00⫹.50/0 2505
with ordered occupation of the tetrahedral sites by Li and Ta. The
resulting arrangement leads to infinite chains
1
⬁
[TaN
2
N
2/2
4⫺
] run-
ning along [100].
Keywords: Nitrides; Tantalum; Lithium; Crystal structure
0,0288). Die Kristallstruktur wird als Li
2
O-Überstruktur mit ge-
ordneter Besetzung der Tetraederlücken einer kubisch dichten Pa-
ckung aus N beschrieben. Die gefundene Anordnung führt zu un-
endlichen Ketten
1
⬁
[TaN
2
N
2/2
4⫺
], welche entlang [100] verlaufen.
from Li
15
[CrN
4
]
2
N [8] in a welded Ta ampoule in presence of excess
Li. This assembly was heated in Ar atmosphere to 1470 K for 20 h
and then slowly cooled (100 h to 870 K), before the furnace was
switched off and allowed to cool down naturally. Li
15
[CrN
4
]
2
Nwas
synthesized from Li
3
N (prepared from Li metal, Roth 99.99 %, in
flowing N
2
, Messer-Griesheim 99.999 %, additionally purified by
passing over molsieve, Roth 3 A
˚
, and BTS-catalyst, Merck) and Cr
(powder, Alfa, 99,9 %) in flowing N
2
for 20 h at 1070 K. The final
oxygen content in Li
15
[CrN
4
]
2
N was less than 0.01 % (LECO ana-
lyzer TC-436 DR, hot extraction technique). After synthesis of
Li
4
[TaN
3
] the excess Li metal was extracted with liquid ammonia.
The only products observed after the reaction are chromium den-
drites and colourless plates of Li
4
[TaN
3
], both up to 1 mm in size.
The solids could be separated manually. Li
4
[TaN
3
] is sensitive
against moisture by rapid formation of ammonia.
For powder X-ray diffraction measurements, the purified samples
of the ternary nitride were ground and sealed in glass capillaries
(diameter 0.2 mm). The measurements were performed on a Huber
image plate Guinier camera in the 2θ-range of 10°-100° (expose
time 3 ⫻ 8 h) using CuKα
1
-radiation. Fig. 1 presents the powder
diagram together with the calculated intensity profile. Differences
in intensities are most likely due to preferred orientation of the
crystallites with the shape of platelets (esp. the reflections (002),
(004), (006) and (008) exhibit intensities in the experimental pattern
too high compared with the calculated diagram).
X-ray diffraction intensity data of a single crystal (0.1 mm ⫻
0.1 mm ⫻ 0.05 mm sealed in a glass capillary) were collected on a
MSC-Rigaku CCD applying MoKα-radiation. Initial indexing of
the powder pattern and the data from the single crystal resulted in
an orthorhombic unit cell with the dimensions a ⫽ 491.85(4) pm,
b ⫽ 973.59(6) pm, c⬘⫽707.5(1) pm (Guinier data). Close inspec-
tion of the powder pattern revealed one weak unindexed peak call-
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