硫酸锌

ZnSO4纳米晶的结构表征

孙玉希化12级3班全体成员

Abstract

晶体都具有特定的晶体结构，通过X射线扫描，根据所得的XRD图谱，可以确定样品中存在的物相，可以直接根据图谱，推断晶体状态，硫酸锌的晶体状态为无色斜方晶体，晶胞参数

Crystal data

ZnH12O6.2(SO4).2(H2O) Z = 2

M r = 401.62 D x = 1.884 Mg m-3

Monoclinic, P21/c Mo Kα radiation

a = 6.2393 (4) Å Cell parameters from 6635 reflections

b = 12.6675 (8) Å θ = 2.8–28.2°

c = 9.3591 (6) Å μ = 2.11 mm-1

β = 106.8720 (10)°T = 295 (2) K

V = 707.87 (8) Å3Plane, colorless

Data collection

Bruker SMART APEX area-detector

1433 reflections with I > 2σ(I) diffractometer

φ and ω scan R int = 0.023.000

Absorption correction: multi-scan (based

θmax = 26.5°

on symmetry-related measurements)

T min = 0.518.000, T max = 0.678.000 h = -7 → 7

7273 measured reflections k = -15 → 15

1460 independent reflections l = -11 → 11

Keywords : ZnSO4纳米晶X衍射XRD图结构表征

Introduction:随着材料科学技术的日益发展，无机功能晶体已经成为现代科学技术中不可缺少的应用材料，对无机功能晶体的结晶形态，微观结构，尺寸大小的表征是确定晶体及晶体用途的客观需要

Experimental：通过制得无机晶体ZnSO4，在显微镜下选择合适的晶体后，用X 射线仪测定ZnSO4的晶体结构,得到Znso4的CIF全部内容如下：

Crystal data

ZnH12O6.2(SO4).2(H2O) Z = 2

M r = 401.62 D x = 1.884 Mg m-3

Monoclinic, P21/c Mo Kα radiation

a = 6.2393 (4) Å Cell parameters from 6635 reflections

b = 12.6675 (8) Å θ = 2.8–28.2°

c = 9.3591 (6) Å μ = 2.11 mm-1

β = 106.8720 (10)°T = 295 (2) K

V = 707.87 (8) Å3Plane, colorless

a≠b≠cß,≠90°,所以该晶体结构为斜方晶体，晶胞结构单元数为2

Data collection

Bruker SMART APEX area-detector

1433 reflections with I > 2σ(I) diffractometer

φ and ω scan R int = 0.023.000

Absorption correction: multi-scan (based

θmax = 26.5°

on symmetry-related measurements)

T min = 0.518.000, T max = 0.678.000 h = -7 → 7

7273 measured reflections k = -15 → 15

1460 independent reflections l = -11 → 11

Refinement

Refinement on F2Mixture of independent and constrained

H-atom refinement

R[F2 > 2σ(F2)] = 0.069.000 Calculated weights w = 1/[σ2(F o2) +

(0.1358P)2 + 3.804P] where P = (F o2 +

2F c2)/3

wR(F2) = 0.224.000 (∆/σ)max <0.0001

S = 1.17 ∆ρmax = 0.98.00 e Å-1

1460 reflections ∆ρmin = -2.41 e Å-1

90 parameters Extinction correction: none Geometric parameters (Å, °) for a

Zn1—O1 2.140 (4) Zn1—O3i 2.179 (4)

Zn1—O2 2.179 (4) S1—O5 1.461 (4)

Zn1—O3 2.179 (4) S1—O6 1.482 (4)

Zn1—O1i 2.140 (4) S1—O7 1.479 (4)

Zn1—O2i 2.179 (4) S1—O4 1.473 (4)

O1—Zn1—O2 92.1 (1) O3—Zn1—O3i180.0

O1—Zn1—O3 90.8 (2) O1i—Zn1—O2i92.13 (1)

O1—Zn1—O1i180.0 O1i—Zn1—O3i90.81 (2)

O1—Zn1—O2i87.9 (1) O2i—Zn1—O3i89.42 (1)

O1—Zn1—O3i89.2 (2) O6—S1—O7 109.8 (2)

O2—Zn1—O3 89.4 (1) O4—S1—O7 108.2 (2)

O1i—Zn1—O2 87.9 (1) O4—S1—O5 109.2 (2)

O2—Zn1—O2i180.0 O4—S1—O6 109.8 (2)

O2—Zn1—O3i90.6 (1) O5—S1—O6 110.4 (3)

O1i—Zn1—O3 89.2 (2) O5—S1—O7 109.4 (3)

O2i—Zn1—O3 90.6 (1)

通过以上数据得锌与两个氧形成化学键，硫与四个氧形成化学键，且氧与锌存在三种连接方式，硫与氧也存在两种连接方式（氧的存在方式为2:1）

Symmetry codes: (i) 2-x, -y, 1-z.

Hydrogen-bond parameters (Å, °) for a

D—H H...A D...A D—H...A

O1—H1A...O4i0.8200 1.9500 2.763 (5) 170.00

O1—H1B...O7ii0.8200 1.8800 2.696 (5) 174.00

O2—H2A...O6iii0.8200 2.0400 2.830 (6) 162.00

O2—H2B...O4 0.8100 2.0300 2.795 (5) 157.00

O3—H3A...O5iv0.8200 1.9100 2.714 (5) 168.00

O3—H3B...O6v0.8200 1.9400 2.754 (5) 172.00

O8—H8A...O4vi0.8200 2.2600 2.843 (6) 128.00

O8—H8B...O7 0.8200 2.2200 2.987 (6) 156.00

Symmetry codes: (i) 1-x, -y, 1-z; (ii) 1-x, -1/2+y, 1/2-z; (iii) 1+x, y, z; (iv) 1+x, y, 1+z; (v) 1+x, 1/2-y, 1/2+z; (vi) 1-x, 1/2+y, 1/2-z.

由以上数据可知，氢既参与了化学键的形成，也参与了氢键的形成

Result and discussion

通过试验及结果计算，得出八水硫酸锌的晶体结构为无色斜方晶体

X射线法具有不损伤物品，无污染，快捷。测量精度高，能得到有关晶体完整性的大量信息等优点

Conlusion

View of the title compound with the atom numbering scheme. Displacement ellipsoids for non-H atoms are drawn at the 50% probability level.

Figure captions

C