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首页调控孔结构的单分散介孔二氧化硅纳米球的大规模简便合成
调控孔结构的单分散介孔二氧化硅纳米球的大规模简便合成
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"Kong结构可调的单分散介孔二氧化硅纳米球的简便大规模合成" 本文是一篇关于介孔二氧化硅纳米粒子(Mesoporous Silica Nanoparticles, MSNs)的研究论文,主要关注如何在温和条件下大规模合成具有可控孔隙结构的单分散纳米球。在生物医学领域,MSNs因其独特的性质,如大比表面积、可调的孔径和良好的生物相容性,被广泛应用于药物传递、成像和非均相催化。然而,制造粒径小于200nm并具有精确孔隙分布的Kong网络仍存在挑战。 作者通过模板溶胶-凝胶技术成功地解决了这一问题,该技术在常压下进行,使用十六烷基三甲基铵(CTA+)作为模板表面活性剂,并结合小的有机胺(SOA)作为矿化剂。实验发现,通过调整SOA的浓度,可以控制介孔的形态,例如在超低SOA浓度下,甲苯磺酸(Tos-)和溴化物(Br-)会引导形成星状(ST)或树莓状(RB)通道形态;而在高SOA浓度下,两者则产生蠕虫状(WO)形态。这种形态变化归因于胶束电栅栏的离子竞争机制,即在形成过程中,不同的抗衡离子会引导不同的自组装过程。 此外,研究中还提到,通过特定的SOA可以实现纳米粒子的轻松回收和再分散,这使得该方法具备了公斤级别的高产率生产能力,对工业化应用具有重要意义。这一创新技术不仅克服了过去合成过程中的困难,也为未来设计和制备具有定制孔结构的纳米材料提供了新途径,可能在药物递送系统、催化剂载体、生物传感器等领域展现出广泛应用前景。 这篇研究论文展示了如何通过精细调控反应条件来实现介孔二氧化硅纳米球的单分散性和孔隙结构的控制,这对于优化这些材料的性能和扩大其在生物医学和催化等领域的应用具有深远影响。
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Facile Large-Scale Synthesis of Monodisperse Mesoporous Silica
Nanospheres with Tunable Pore Structure
Kun Zhang,*
,†
Lang-Lang Xu,
†
Jin-Gang Jiang,
†
Nathalie Calin,
‡
Koon-Fung Lam,
∥
San-Jun Zhang,
§
Hai-Hong Wu,*
,†
Guang-Dong Wu,
†
Be
len Albela,
‡
Laurent Bonneviot,*
,‡
and Peng Wu
†
†
Shanghai Key Laboratory of Green Chemistry and Chemical Processes, Department of Chemistry, East China Normal University,
Shanghai, China
‡
Laboratoire de Chimie, UMR-CNRS 5182, E
cole Normale Supe
rieure de Lyon, Universite
de Lyon, Lyon, France
§
State Key Laboratory of Precision Spectroscopy, East China Normal University, Shanghai, China
∥
Department of Chemical Engineering, University College London, Torrington Place, London, United Kingdom
*
S
Supporting Information
ABSTRACT: Mesoporous silica nanoparticles (MSNs)
are experiencing rapid development in the biomedical field
for imaging and for use in heterogeneous catalysis.
Although the synthesis of MSNs with various morpholo-
gies and particle sizes has been reported, synthesis of a
pore network with monodispersion control below 200 nm
is still challenging. We achieved this goal using mild
conditions. The reaction occurred at atmospheric pressure
with a templating sol−gel technique using cetyltrimethy-
lammonium (CTA
+
) as the templating surfactant and
small organic amines (SOAs) as the mineralizing agent.
Production of small pore sizes was performed for the first
time, using pure and redispersible monodispersed porous
nanophases with either stellate (ST) or raspberry-like
(RB) channel morphologies. Tosylate (Tos
−
) counterions
favored ST and bromide (Br
−
) RB morphologies at
ultralow SOA concentrations. Both anions yielded a worm-
like (WO) morphology at high SOA concentrations. A
three-step formation mechanism based on self-assembly
and ion competition at the electrical palisade of micelles is
proposed. Facile recovery and redispersion using specific
SOAs allowed a high yield production at the kilogram
scale. This novel technique has practical applications in
industry.
C
onsiderable progress has been made in the past decade in
the synthesis of mesoporous materials with a defined
topology and morphology.
1−5
The synthesis of surfactant
templated mesoporous silica nanoparticles (MSNs) smaller
than 200 nm is emph asized because of th eir potential
applications in cell imaging, disease diagnosis, drug/gene/
protein storage or delivery, separation, and heterogeneous
catalysis.
6−11
Chemical stability, consistent pore structure, easy
large-scale purification, and recovery from colloidal solutions
are required for any industrial application of MSNs.
12−17
Soft-templating synthesis of MSNs is the best and easiest
method because there is little aggregation, involving a well-
defined pore structure, uniform morphologies, and particle size
control. Polymorphic and polydispersed MSNs are produced
under kinetic control using dilution and acid quenching.
14,15
Growth inhibitor additives, such as a triblock copolymer
(F127),
12
triethanol amines (TEAH
3
),
18−20
and functional
organosilanes, improve the process, resulting in better particle
size control. Without the addition of any additives, control of
pore size and structure is poor.
13,21,22
Several groups have
synthesized MSNs with radial-oriented mesochannels and a
conical pore shape using microemulsion media.
23−26
These
stellate structures are ideal scaffolds for biological, medical, and
catalytic applications, as the pore structures are accessible by
large molecules.
27−29
These structures are either too large
(>200 nm) for application in life sciences or too complex to be
produced at a large scale. Thus, reliable large-scale production
of MSNs with tunable porosity and particle size, particularly
<200 nm, is highly desirable.
12−26,30
In this work, the first kilogram scale synthesis of pure
nanophases of monodisperse MSNs smaller than 130 nm with
stellate (ST), raspberry (RB), or worm-like (WO) morphol-
Received: November 29, 2012
Published: January 30, 2013
Table 1. Textural Characteristics of Calcined MSNs
Synthesized in Various Reaction Conditions
sample
a
S
BET
b
(m
2
/g)
V
total
c
(mL/g)
V
inter
d
(mL/g)
D
BJH
e
(nm) PSD
f
(nm)
MSN-L-T1 435 2.13 0.32 54 74 ± 8
MSN-L-T2 552 1.45 0.41 16 115 ± 10
MSN-L-T3 590 1.38 0.42 17 130 ± 12
MSN-L-B2 675 1.27 0.43 2.3/54 40 ± 3
MSN-H-T2 837 1.71 0.64 2.9/54 90 ± 12
MSN−H-
B2
g
1154 1.58 1.00 2.7 50 to 80
a
L and H stand for low and high TEAH
3
/TEOS molar ratio, x = 0.026
and 8.0; T and B stand for Tosylate (Tos
−
) and bromide (Br
−
)
counterions; n stands for SOA with 1 = TEA, 2 = TEAH
3
, and 3 =
AHMPD, respectively.
b
S
BET
is the specific surface area measured from
N2 physisorption.
c
V
total
is the total internal pore volume measured at
P/P
o
= 0.99.
d
V
inter
is the internal pore volume measured at P/P
o
=
0.80.
e
D
BJH
is the pore diameter calculated from the BJH theoretical
model (add ca. 0.7 nm for BdB or DFT equivalent).
f
Particle size
distribution (PSD) was determined by measuring the diameters of at
least 100 particles under TEM (Figure S1).
g
From ref 18.
Communication
pubs.acs.org/JACS
© 2013 American Chemical Society 2427 dx.doi.org/10.1021/ja3116873 | J. Am. Chem. Soc. 2013, 135, 2427−2430
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