Question

XRD标准图谱

【求助】铝酸铜 铝酸镍的XRD 标准图谱

Answer 1

PDF#33-0448: QM=Star(S); d=Diffractometer; I=Diffractometer
Copper Aluminum Oxide
Cu Al2 O4 Brown
Radiation=CuKa1 Lambda=1.54056 Filter=
Calibration=Internal(Si) 2T=19.029-111.424 I/Ic(RIR)=1.1
Ref: Lambert, Eysel, Mineralogical-Petrograph. Institute, Universitat Heidelberg, Germany.
ICDD Grant-in-Aid (1980)
Cubic - (Unknown), Fd-3m (227) Z=8 mp=
CELL: 8.075 x 8.075 x 8.075 <90.0 x 90.0 x 90.0> P.S=cF56 (Spinel)
Density(c)=4.580 Density(m)=4.02A Mwt=181.51 Vol=526.54 F(14)=36.6(.0166,23/0)
Ref: Ibid.

Strong Lines: 2.44/X 2.86/6 1.43/4 1.55/3 2.02/2 1.65/2 1.05/1 1.23/1 0.93/1 4.66/1
NOTE: Under Ar-atmosphere decomposition starts at 870 C following the equation: 4 Cu Al2 O4=4 Cu Al O2+2 Al2 O3+O2.
CuO (p.a., Merck)+Al ( O H )3(reinst, Merck) heated for eight days at 950 C.
To replace 00-002-1414.
2-Theta d(?) I(f) ( h k l ) Theta 1/(2d) 2pi/d n^2
19.029 4.6600 4.0 ( 1 1 1) 9.514 0.1073 1.3483 3
31.294 2.8560 55.0 ( 2 2 0) 15.647 0.1751 2.2000 8
36.867 2.4360 100.0 ( 3 1 1) 18.434 0.2053 2.5793 11
44.855 2.0190 16.0 ( 4 0 0) 22.428 0.2476 3.1120 16
55.695 1.6490 16.0 ( 4 2 2) 27.847 0.3032 3.8103 24
59.420 1.5542 25.0 ( 5 1 1) 29.710 0.3217 4.0427 27
65.292 1.4279 35.0 ( 4 4 0) 32.646 0.3502 4.4003 32
74.218 1.2767 3.0 ( 6 2 0) 37.109 0.3916 4.9214 40
77.465 1.2311 7.0 ( 5 3 3) 38.732 0.4061 5.1037 43
82.772 1.1651 3.0 ( 4 4 4) 41.386 0.4291 5.3928 48
91.071 1.0793 4.0 ( 6 4 2) 45.536 0.4633 5.8215 56
94.214 1.0514 8.0 ( 7 3 1) 47.107 0.4756 5.9760 59
99.478 1.0094 3.0 ( 8 0 0) 49.739 0.4953 6.2247 64
111.424 0.9323 6.0 ( 7 5 1) 55.712 0.5363 6.7394 75

PDF#10-0339: QM=Star(S); d=(Unknown); I=Diffractometer
Nickel Aluminum Oxide
Ni Al2 O4 Blue
Radiation=CuKa1 Lambda=1.5405 Filter=Ni
Calibration= 2T=19.070-139.359 I/Ic(RIR)=1.60
Ref: Natl. Bur. Stand. (U.S.), Circ. 539, v9 p42 (1960)

Cubic - Powder Diffraction, Fd-3m (227) Z=8 mp=
CELL: 8.048 x 8.048 x 8.048 <90.0 x 90.0 x 90.0> P.S=cF56 (?)
Density(c)=4.501 Density(m)=4.10A Mwt=176.66 Vol=521.27 F(18)=28.0(0.021,30/0)
Ref: Ibid.

Strong Lines: 2.43/X 2.01/7 1.42/6 1.55/3 4.65/2 2.85/2 0.82/2 1.05/1 1.23/1 1.64/1
NOTE: Sample prepared at NBS, Gaithersburg, Maryland, USA, by heating coprecipitated hydroxides at 1300 C.
Spectroscopic analysis showed <1.0% Na; <0.1% Co, Si; <0.01% Cr, Fe, Mg; <0.001% Ca, Mn.
Pattern taken at 25 C.
2-Theta d(?) I(f) ( h k l ) Theta 1/(2d) 2pi/d n^2
19.070 4.6500 20.0 ( 1 1 1) 9.535 0.1075 1.3512 3
31.406 2.8460 20.0 ( 2 2 0) 15.703 0.1757 2.2077 8
37.009 2.4270 100.0 ( 3 1 1) 18.505 0.2060 2.5889 11
44.996 2.0130 65.0 ( 4 0 0) 22.498 0.2484 3.1213 16
55.972 1.6415 8.0 ( 4 2 2) 27.986 0.3046 3.8277 24
59.661 1.5485 30.0 ( 5 1 1) 29.831 0.3229 4.0576 27
65.535 1.4232 60.0 ( 4 4 0) 32.767 0.3513 4.4148 32
68.991 1.3601 <1 ( 5 3 1) 34.495 0.3676 4.6196 35
74.409 1.2739 <1 ( 6 2 0) 37.205 0.3925 4.9322 40
77.742 1.2274 10.0 ( 5 3 3) 38.871 0.4074 5.1191 43
78.812 1.2134 <1 ( 6 2 2) 39.406 0.4121 5.1782 44
83.103 1.1613 8.0 ( 4 4 4) 41.551 0.4306 5.4105 48
91.506 1.0753 4.0 ( 6 4 2) 45.753 0.4650 5.8432 56
94.662 1.0476 12.0 ( 7 3 1) 47.331 0.4773 5.9977 59
99.923 1.0061 8.0 ( 8 0 0) 49.961 0.4970 6.2451 64
112.005 0.9291 8.0 ( 7 5 1) 56.002 0.5382 6.7627 75
117.753 0.8998 8.0 ( 8 4 0) 58.877 0.5557 6.9829 80
139.359 0.8214 16.0 ( 8 4 4) 69.680 0.6087 7.6494 96

Answer 2

衍射峰位置偏移是正常的，和你的样品制备历史也有一定关系。回答你的问题：---前几个峰都比标准卡的峰向后偏了点，但后两个峰又能对上，那我这个物质是那个晶相吗？应该是。以下是我遇到的几种情况：（1）我以前水相制备某物质，该物晶胞内有羟基会导致晶格在某个方向上拉长，表现在某些衍射峰峰位发生偏移。（2）在参杂微量其他物质时（体积含量低于5%？）XRD分析观察不到参杂物的衍射峰但是通常都会影响晶格常数，衍射峰位置也会偏移。（3）在形成固溶体时，也是保持其中一种物质的晶型，但通常衍射峰会偏移。也有我没遇到的情况，以上信息供您参考。