Single	  Crystal	  Structure	  Analysis	  of	  a	  Single	  Sm2Fe17N3	  Par;cle	
Nobuhito	  Inami1,	  Yasuo	  Takeichi1,	  Tetsuro	  Ueno2,	  Kotaro	  Saito1,	  Ryoko	  Sagayama1,Reiji	  Kumai1,	  Kanta	  Ono1	  	1High	  Energy	  Accelerator	  Research	  Organiza5on	  (KEK),	  Japan	  2Na5onal	  Ins5tute	  for	  Materials	  Science	  (NIMS),	  Japan	  	Introduc;on	Material	

Laoce	  constants	  of	  Sm2Fe17Nx	  (x	  =	  0.0	  –	  2.9)	

Sm2Fe17N3	 Nd2Fe14B	

satura;on	  Ms	  (T)	1.54	

8.85	  	  

1.60	m H 	  (T)	26	7	
Sm2Fe17N3anisotropy	  ÍubÓ£èâ

8.80	  	  0 a479	

315	

a	  (Å)	

Curie	  temperature	  Tc	  (℃)	inves;gated	  by	  X-­‐ray	  powder	  diﬀrac;on	

Crystal	  structure	  of	  Sm2Fe17Nx	  (x	  =	  0.5	  –	  2.9)	
Atomic	  site	  posi;ons	  of	  each	  Sm2Fe17Nx	  are	  same.	

12.70	  	  N	Fe2	12.65	  	  8.75	  	  12.60	  	  2are	  good	  a1s	  Wæ|êuwell	  as	  NdFeB.	   1²Rµ\ 1{ïys8.70	  	   1
}®¸ 1NïkProper;es	  ÛØsëno	  tendencies	  128.65	  	  ÷KEKùnitrogena;on	 ³¦£ø8.60	  	   dras;cally	  expands	
Sm2analysis
Fe17	
N	
Sm22FeFe17
Single-crystal
structureof SmNx	
317N
1211118.55	  	  mi1, Y. Takeichi,T.
Ueno,K.
Saito,R.
Sagayama,
R.
Kumai,K.
Ono
Laoce	  constants	  are	  changed	  by	  an	  amount	  of	  inserted	  nitrogen.	  
0.0	  	   0.5	  	   1.0	  	   1.5	  	   2.0	  	   2.5	  	   3.0	  	  12KEK,Inves;ga;on	  of	  (the	  crystal	  NIMS)
structure	  is	  necessary	  to	  study	  amount	  of	  nitrogen	

12.55	  	  Sm	Fe1	12.50	  	  12.45	  	  $Sm-Fe-N Ð 650˚C  Fe 

Observed Data

SmFeN_N004_2taλ=	  0.688	  Å	AK:ÅÁx·a0.80.7

ÍuÅÁÂÉð»)é
Intensity (x 0.01)

îß&ÅÁÍuÌ X Õl¬ÍuñÅª¾QX·#&

â

0.5

intensi;es	  are	  diﬀerent.	

&('(' Sm-Fe-N Íu)>70*7@Ó£

òqg
0.4

0.3

ð»bM Sm2Fe17N3 ÍubÓ£èâ
0.2

Fe2	  18f	  x	0.2807	

Fe3	9d	x	  z	0.5	  0.5	Fe4	6c	z	0.0954	

Sm	6c	z	0.34548	

N	9e	x	

0.5	

We	  conduct	  to	  1) develop	  a	  micromanipula;on	  system	  for	  picking	  a	  single	  crystal	  par;cle,	  2) analyze	  a	  single	  crystal	  structure	  of	  Sm2Fe17Nx	  ﬁne	  par;cles.	  	  '&&NÓ£è"ÊÑ2+9VÖ)¨Ädo`ed	  ring	

0.6

0.50536	  0.49464	  0.15126	

purpose	

Debye	  Scherrer	  ring	

SmFeN_N002_2ta

0.9mò% 3)Sm-Fe-N Íu)¥Úox	  y	  z	Printed from CrystalDiffract 5.2.61, 2)
both	  pa`erns	  from	  a	  same	  sample	È)x¶&fÙ&&


±Ó

18h	  The	  reason	  is	  diﬃculty	  of	  crystal	  structure	  analysis	  with	  ferromagne;c	  powder	  samples.	

Why	  diﬀerence	  powder	  diﬀrac;on	  in	  same	  samples?	  	
Powder	  diﬀrac;on	  pa`erns	  of	  a	  SmFe7N	  sample	  21x#%»à ' Sm-Fe-N ÏÅÁr ôjÅaû1 Ã =FCL6)
Angle-Dispersive X-Rays: SmFeN_N002_2ta

Fe1	  No	  reﬁnements	  are	  performed	  in	  almost	  any	  previous	  reports.	  

12.40	  	  3.5	  	  magne;c	  proper;es.	  

1.0

Fe4	Fe3	c	  (Å)	

Magne;c	  proper;es	  of	  Sm2Fe17N3	_pi&

0.1

0.0

70*7@&

15

16

17

18

19

20
Two Theta [degrees]

21

22

23

24

self	  aligned	  by	  dipole	  interac;on	

25

>,5õ`#&B+0JB;>EIL6 MEMS XÞ

Crystal	  structure	  was	  nFig.
ot	  converged	  by	  Rietveld	  analysis.	  
It	  is	  necessary	  )Òg(ÝÖ)ð»úÝÖ¤n)ÆÝÖ#%µm
Uto	  measure	  X-­‐ray	  diﬀrac;on	  with	  a	  single	  crystal.	

*7@X Õ£èâ

·-F4.D>FGLow&]&ÂÉN Íu)>70*7@P§[+CL3K1@IL9)Y KEK Photon Factory¯w)Ü½ 20µm bMÍu!À?F71dz)á¯&'ö^âÙ8L6)&Experimental	  methods	]Table s1ystem	  bÓ£èâ
micromanipula;on	  for	  picking	  a	  $$'Óvﬁne	  par;cle		  X-­‐ray	  diﬀrac;on	  measurement	

torGOF '' 1.94%,
X-­‐ray	  diﬀractometer	  at	  KEK	  BL8A/B	

#%º&Í%T2-­‐dimensional	  diﬀrac;on	  pa`ern	  by	  imaging	  plate	ÅÁð»SmFeN	  sample	  with	  grease	&A	  microgripper	  fabricated	  by	  MEMS	ω	  scan	glass	  needle	

H. Sun: J. Magn. Magn.

2-­‐dimensional	  X-­‐ray	  detector	  (inside)	

1990).

bayashi, N. Imaoka, T.
It	  enable	  us	  to	  pick	  a	  par;cle	  of	  approximately	  10	  μm.	  

nd Y. Nakagawa: IEEE2326 (1992).

. Lawier, H. Sun and J. E.

incident	  energy	  (wave	  length):	  18	  keV	  	  (0.688	  Å)	  Results	  and	  discussion	

Table 1 Structure of Sm2Fe17N3 obtained from single-crystal
Laoce	  constants	  of	  Sm2Fe17Nx	
Single	  crystal	  structure	  analysis	  of	  Sm2Fe17Nx	
X-ray diffraction patterns.

ÂÉ°)e

Clear,	  sharp	  diﬀrac;on	  spots	  were	  obtained.	

Fig. 1 Schematic of the pick-up and micro- manipulation
system.

Phys., 69, 3007 (1991).

ìÇv¿täO¡goniometer	

R-­‐factor	  =	  1.94%,	  wR2	  =	  2.47%,	  Goodness	  of	  Fit	  =	  0.831	
N	  occupancy	  was	  slightly	  changed,	  and	  the	  value	  converged	  on	  1.0.	  →	  nitrogen	  =	  3	Chemical Formula: Sm2Fe17N3

 Rhombohedral R-3m

sample	 0°	  →	  180°	 Sm 6c (0.0000, 0.0000, 0.3431)

Fe 9d (0.5000, 0.0000, 0.5000)

5°	  oscilla;on	  for	  20	  min.	
180°	  rota;on	  in	  total	 Fe1	  18h (0.5048, 0.0096, 0.1524)

N 9e2	
(0.5000, 0.0000, 0.0000)
36	
36	  diﬀrac;on	  pa`erns	
Indexing,	  Integra;ng,	  Scaling	  of	  diﬀrac;on	  spots	  merge	
R-­‐merge	  =	  2.32%	  Diﬀerence	  of	  distances	  between	  Fe-­‐Fe	  and	  Fe-­‐Sm	

a = 8.7206Å,

Sm2Fe17	  	  	  	  	  	  	  	  	  Sm2Fe17N3	  c = 12.6345Å

space	  group	Fe1	  18h	Fe 18f(No.	  
(0.2826,166)	 0.0000, 0.0000)
R3m

Fe 6c (0.0000, 0.0000, Fe2	0.0948)18f	
a	  =	  b	  =	  8.7206	  Å	Fe3	9d	c	  =	  12.6345	  Å	β=90°	 α=90°	
γ=120°	x	  y	  z	0.5	  0.5	  0.16667	

0.504819	  0.495179	  0.152431	

x	0.33333	

0.282628	x	  z	

0.5	  
0.5	0.5	  0.5	Fe4	6c	z	

0.097	

0.094825	

Sm	6c	z	0.33333	

0.343085	

N	9e	x	-­‐	0.5	

Fe2	N	

Sm2Fe17N3	N	

Fe4	Fe3	
Sm	

Sm2Fe17	Fe1	Each	  atomic	  site	  in	  Sm2Fe17N3	  was	  determined.	
The	  Fe2	  (18f)	  site	  shims	  largely	  from	  Sm2Fe17.	

Summary	• We	  have	  developed	  a	  micromanipula;on	  system	  for	  picking	  a	  ﬁne	  par;cle.	  
We	  succeeded	  to	  pick	  a	  single	  crystal	  Sm2Fe17N3	  par;cle.	  
• We	  conducted	  X-­‐ray	  diﬀrac;on	  of	  a	  single	  Sm2Fe17Nx	  par;cle.	  	  We	  also	  succeeded	  to	  determine	  a	  single	  crystal	  structure	  of	  a	  single	  Sm2Fe17N3	  par;cle.	  
• In	  the	  future,	  this	  method	  enable	  us	  to	  analyze	  rela;on	  between	  crystal	  structure	  and	  magne;c	  proper;es	  with	  diﬀerence	  amount	  of	  nitrogen.	  

2.464Å	2.857Å	Fe2	2.857Å	2.857Å	3.154Å	Sm	Distance	  between	  Fe2	  sites	  reduces	  13.8	  %,	  whereas	  that	  between	  Fe2	  and	  Sm	  site	  expands	  10.4%.