Materials design of layered alkali silicates;
functionalization with inorganic species
Masashi Morita1 and Makoto Ogawa*2

1Division of Applied Chemistry, Institute of Engineering, Tokyo University of Agriculture and Technology,

2-24-16 Naka-cho, Koganei, Tokyo 184-8588, Japan
2School of Energy Science and Engineering, Vidyasirimedhi Institute of Science and Technology(VISTEC), 555 Moo 1 Payupnai, Wangchan, Rayong 21210, Thailand
E-mail: makoto.ogawa@vistec.ac.thLayered alkali silicates, which are composedof alternately stacked SiO4 sheets andexchangeable interlayer alkaline cations,have been investigated for fundamental
science and practical applications. The
silanol groups (SiOH/SiO–) on the layer
surface have been used to react for cationexchange and grafting to design various
nanostructures. Their structures can also be
converted to zeolite frameworks by interlayer
condensation.
Here,
the
preparation,
reactivity for ion exchange, grafting, andisomorphous substitution of layered alkali
silicates are summarized with the emphasison the fixation of heteroelements in/on thesilicates.
Keyword: Layered alkali silicate, Ion exchange, Grafting, Isomorphous substitution, Conversion to zeolite
Masashi Morita received his B.S. (2011) and M.S. (2013) from Waseda University
under the supervision of Professor Makoto Ogawa. From 2013 to 2021, he worked
as a researcher at Panasonic corporation, and was promoted to senior researcher(2017–) and worked as a project leader (2018–). In 2021, he received his Ph.D.
degree from Nagoya University under the supervision of Professor Ryotaro Matsuda.
After receiving his Ph.D. degree, he moved to the Division of Applied Chemistry,
Institute of Engineering at Tokyo University of Agriculture and Technology as an
assistant professor. His current research interests are design and synthesis of
inorganic–organic hybrid materials focusing on 2D materials and metal complexes
for adsorbents and catalysts.
Makoto Ogawa was educated in the Department of Applied Chemistry, Waseda
University, supervised by Professor Chuzo Kato. After postdoctoral research at
RIKEN, he joined Waseda University and worked on inorganic materials chemistry.
In 2015, he moved to Thailand as an opening professor of the School of Energy
Science and Engineering, Vidyasirimedhi Institute of Science and Technology(VISTEC), which opened in 2015 in Rayong, Thailand and continues his research
activity in materials chemistry.

Acc. Mater. Surf. Res. 2023, Vol.8 No.3, 125-134.

125

Materials design of layered alkali silicates;
functionalization with inorganic species
Masashi Morita1 and Makoto Ogawa*2
Division of Applied Chemistry, Institute of Engineering, Tokyo University of Agriculture andTechnology
2
School of Energy Science and Engineering, Vidyasirimedhi Institute of Science andTechnology (VISTEC)

1

1. General introductioniv) high crystallinity, v) facile syntheses in

Layered materials have been investigatedlaboratory and so on. Herein, the function andextensively for a variety of applications

the application of the layered alkali silicates

includingandenvironment,

energy,theirintercalates/hybrids

will

be

electronics/optics, plastics, and life sciencessummarized with the emphasis on theusing their characteristics as ultrathin layer

functionalization with inorganic species.

(nanosheet)surfaceassociating
area,

with

chemicalthermal/chemical stabilities.

1)

the

large

reactivity,

Layered alkali

2. Preparation and characterization oflayered alkali silicatessilicates are class of layered materials

Layered alkali silicates with varied layercomposed of alternately stacked silicate layer

thicknesses are available as summarized inand exchangeable interlayer cations,

2,3)

and

Table 1. Kenyaite and magadiite were foundtheir application in the environment, energy

at Lake Magadi, Kenya in 1967.2) Layered

and life science related fields has beenalkali silicates are commonly synthesized by

Layered alkali silicates arehydrothermal reactions in the laboratory.10-14)

advantageous over smectites, which are

Layered silicates with thicker silicate layer

known naturally occurring layered silicatesforms when silicon: alkali metal ion ratio

reported.

4-8)

9)

used in many industrial applications from theincreased. Silicon source (silica gel, fumed

following viewpoints; i) high cation exchange

silica, alkoxysilane, etc.) was reported tocapacity, ii) the silanol groups on the layer

affect the particle morphology of the resulting

surface for grafting and other host–guest

layered silicates.8) Kanemite is synthesized

reactions, iii) well-defined particle morphology,

from Na2Si2O5, which is prepared by the solid-

Table 1. Typical example of layered alkali silicates and their structures.

Acc. Mater. Surf. Res. 2023, Vol.8 No.3, 125-134.

126

state reaction at 700 °C, by the reaction withhydrogen bonding between the terminal

H2O.15,16)

silanol group of the silicate layer. HUS-3, its

The structures and the reactivity of thecrystal structure has not been solved,20) was

layered alkali silicates have been investigatedconverted into a CDO-type zeolite bysystematically.3,4) The structures of layered

calcination, indicating that the structure ofsilicates have been discussed in the analogy

HUS-3 has partially similar to that of the CDO-

to those of zeolite, and the uses of layeredtype zeolite.

silicates as zeolite precursors have been

Advanced

reported.

5,17)

data

analyses (powder X-ray diffraction data andtypes: NSI, CDO, RRO etc.) are obtained only

3D electron diffraction)11,12) have been used to

by topotactic condensation of the layered

solve the crystal structures of magadiite andsilicates.

zeolites

and(framework

18)

Some

characterization

In order to extend the materials’

kenyaite.

variation, the preparation of novel layered
alkali silicates has been examined. As an

3. Reactions of layered alkali silicatesexample,3.1. Ion exchange

layeredsilicates

named

as

Hiroshima University Silicates (HUSs) seriesi) Inorganic cation27)

are synthesized by hydrothermal reactions bySano, Ikeda and their co-workers.

19,20)The ion exchange selectivity of magadiiteInand octosilicate was reported by Wolf andHUS-1, tetramethylammonium (TMA) ions

Schwieger as the following order; H+ > Na+ >used as a structure-directing agent are

Li+ > K+.21) Proton exchanged forms havelocated in the interlayer space (Figure 1).19)

been used extensively. Rojo et al. and Lagaly

The chemical composition of HUS-1 iset

Si10O24H6 ･ 2(TMA)) and its framework

alkylamine and pyridine derivatives into

topology is similar to sodalite cage zeolites.

protonatedAs compared with other layered silicates

Protonated layered silicates are useful as the(Table 1), the interlayer distance is very shortintermediate for pillaring and grafting.24-26)(about 0.15 nm) as each layer is stacked byal.

investigated the intercalation ofmagadiite

systematically.22,23)

Muraishi reported the preparation of alkali
metal cation (Li+, Na+, K+, Rb+, Cs+)
exchanged-magadiites and kenyaite28,29) andtheir structures were investigated by XRD,
thermalanalyses,

and

FT-IR

spectroscopy.30,31) The

cationexchange

reactions of magadiite with metal ions (Mg2+,
Ca2+, Al3+, Co2+, Cu2+, Zn2+, Fe3+, etc.) were
quantitatively investigated by Muraishi and
Hatsushika.32-34) In addition to the cation
Figure 1. Structural model of HUS-1 viewed

exchange, formation of hydroxide on thealong

surface[010]

direction.

Reprinted

withpermission from ref (19). Copyright (2011)

may

occur

dependontheexperimental condition and metal ions.

American Chemical Society.

Acc. Mater. Surf. Res. 2023, Vol.8 No.3, 125-134.

127

Figure 2. Adsorption isotherms of Zn2+ (●)
and Cd2+ ( □ ) on a) magadiite, b)
octosilicate, and c) ion-exchange resin(IRC748,

Organo)fromaseawater-Figure 3. Schematic drawing of the crownmimicking solution containing Zn2+ and Cd2+.

ether (15-crown-5) assisted for ion exchange

The dotted lines denote the cation exchangewith [Ru(bpy)3]2+. Reprinted with permission

capacities. Reprinted with permission fromfrom ref (42). Copyright (1999) Americanref (38). Copyright (2011) John Wiley andChemical Society.

Sons.

The adsorption isotherms of Eu3+, In3+ and2+

space.

Platinum

tetraammine

cation([Pt(NH3)4]2+) and silver diamine cation

Pb on magadiite and octosilicate from water([Ag(NH3)2]+) were also intercalated into thewere reported to be H-type, indicating strong

interlayer space of magadiite and subsequentinteractions between the silicate sheets ofcalcination to form the metallic Pt and Ag

magadiite and the metal ions.
concentration
magadiite

2+

of

Zn

from

a

35-37)

over

Selective

Cd2+

onto

seawater-mimicking

solution was reported as shown in Figure 2.38)

nanoparticles in the range of 5–12 and 3–5nm,

respectively.40,41)

Tris(2,2′-

bipyridine)ruthenium(II) cation ([Ru(bpy)3]2+)
exchanged magadiite was obtained by the aidof a crown ether (15-crown-5), which interactsii) Complex ionswith Na+ to promote the ion exchange

The ion exchange of complex cations has
also been reported. Dailey and Pinnavaia
investigatedtheintercalationofreaction (Figure 3).42) [Ru(bpy)3]2+ and acationic cyanine dye were intercalated into

cobaltthe interlayer space using alkylammonium-

sepulchrate (sep) complex into the interlayer

exchanged magadiite as an intermediate.43,44)+

space of magadiite by the reaction of Na -The

surfacemodificationoflayeredmagadiite and Co(sep)Cl3 at 100 °C.39)

silicates is one of the promising materials

However, a part of Co(sep) complex was

design to adsorb metal and complex ions.45)

2+

decomposed to Co , resulted the presenceof both Co2+ and Co(sep)3+ in the interlayer
Acc. Mater. Surf. Res. 2023, Vol.8 No.3, 125-134.

For example, the layer surface modification ofoctosilicate with organosulfonic acid moiety
128adsorbed[Ru(bpy)3]2+

in

the

interlayer

space.46,47) The amount of the immobilizedorganosulfonic-acid moiety is important for
the intercalation capability and the mobility
and the spatial distribution of [Ru(bpy)3]2+ inthe interlayer space.
3.2. Reaction of the intercalated metal ions
The functional design of layered silicateshas been extended by the reaction of theintercalated cation in the interlayer space.
The intercalated metal ions (Zn2+, Ag+ and[Cd(NH3)4]2+)

inmagadiite

have

been

converted to metal oxide, metallic and metalsulfide nanoparticles, respectively, (ZnO, Ag

Figure 4. The molecular structures of (a) Li+,and CdS) by the oxidation, reduction and(b) Cu2+ and (c) Al3+ ion coordinated with 8-

sulfidation.48-50)hydroxyquinoline.

For

example,Agnanoparticles (average size: 24 nm) formed
from Ag+-exchanged

magadiitebythereduction using NaBH4.49) This reduction
method (no surface modification of layered
silicates)

led

the

aggregationofAg

nanoparticles on the external surface of
magadiite.

Preparationofmetallic

nanoparticles in the interlayer space oflayered silicates will be introduced in Section
3.3.
In addition, in-situ formation of the complex
has been reported by the reaction of theintercalated metal ions and organic ligands inthe interlayer space. This concept was used
to introduce the catalytic and adsorptive
active sites, and also expect to exhibit uniqueproperties. Wang et al. reported the formationof metal 8-hydroxyquinoline complexes in theinterlayer space by the solid-solid reaction of
Li+, Cu2+ and Al3+-exchanged magadiite(Figure 4).51) The fluorescence of thesecompounds was different from those of theircrystals, indicating the influence on the
Acc. Mater. Surf. Res. 2023, Vol.8 No.3, 125-134.

complexes confined in a 2D nanospace. As ananoscopicallyconfiedmetal–organic

framework (MOFs) or porous coordination
polymer (PCP),52) formation of a coordination
polymer in the interlayer space of layered
silicates has also been reported.53) The hybrid
microporous material adsorbed methanolfrom a methanol/water vapor mixture.
3.3.

Immobilizationofmetallic

nanoparticles
Thesurfacemodification

withsilanecoupling reagents is one of the promisingstrategies for the immobilization of metallic
nanoparticles.54,55) The organic modificationoftheinterlayer

silanolgroupswithmercaptopropylsilylgroup,

urea

andiminodiacetate functional groups has beenreported for their strong interactions with
noble metals. The adsorption of metal
precursors (HAuCl4, AgNO3 and K2PdCl4) on
theorganicallymodifiedoctosilicate/magadiite and the in-situ
129reduction by NaBH4 have been reported foraqua-Fe(III) complex stabilized on the silicate

the immobilization of Au (Figure 5), Ag, andsurface of protonated magadiite.60) The

Pd nanoparticles/nanoplates.56-58) The Ag/Pd

location and the state of a dimeric aqua-

nanoplates showed higher catalytic activity

Fe(III)

species

were

confirmed

for

XANES/EXAFS

spectraandthehydrolysis

of

NH3BH3anddehydrogenation of formic acid than spherical
nanoparticles.

57,58)

bydensityfunctional theory (DFT) calculations. The
aqua-Fe(III) species-immobilized magadiite
exhibited higher UV-shielding performance
than TiO2 rutile.
Using the reactivity of silanol groups on avariety of nanostructured layered silicates,
various metal complexes and molecularspeciesmaydenselybeimmobilized/stabilized on silicate surfaces.
3.5. Doping of heteroelements into the

Figure 5. TEM images of Au nanoparticle intheinterlayer

space

of

silicate layer

octosilicate.

The introduction of heteroelements into

Reprinted with permission from ref (56).
Copyright(2007)

Americansilica/silicate framework by the isomorphous

Chemical

substitution of Si is important for theSociety.

development of catalyst and adsorbent. The
doping of heteroelements (Al3+, Ti4+ and Co2+)
into

3.4. Graftingthesilicatelayer(kanemite

andTaking advantage of the reactivity of silanol

magadiite) during the crystallization of thegroups on the layer surface, grafting haslayered silicates has been reported.61-66) The

been

the

Al-containing magadiites (6.4–12.7 sites/nm2)

immobilization of organic functionalities on

had a higher density of surface hydroxyl

and in the interlayer space of the layeredgroups (silanol/aluminols) than magadiite (Al-silicates.5,7) Along this line, active/unstable

free, 4.7 sites/nm2).66) The Al-containing

metal complexes have been immobilized in

magadiites adsorbed Pb2+ and methylene

the interlayer space of layered silicates. Ti(IV)blue efficiently from single/binary-component

acetylacetonate was grafted in the interlayer

solutions.

reported

space

of

a

extensively

layeredsilicate,

for

HUS-2

Ti-containing octosilicates and magadiites(Si20O40(OH)4·4[C5H14NO]). The grafted Ti on

were

the

hydrothermal reactions using TiCl4 as the Ti

silicate

existedasanisolatedsuccessfully

prepared

by

the

The

source in the starting mixture of magadiite

photocatalytic

and octosilicate.67) Spectroscopic studies

activity than the representative titanosilicate,(UV−vis absorption and XAFS spectra)

TS-1, and high selectivity for partial oxidationsuggested that the incorporated Ti wasof cyclohexane.59) Ide et al. reported a dimerictetrahedrally coordinated with oxygen bytetrahedrally
product

coordinatedexhibitedhigherspecies.

Acc. Mater. Surf. Res. 2023, Vol.8 No.3, 125-134.

130

substituting Si in the silicate sheets. The

The preparation, the reactivity for ion

capacity of the framework incorporation of Ti

exchange, the grafting, and the isomorphouswithout structural alteration was Si/Ti = 50

substitution of layered alkali silicates wereand 100 for magadiite and octosilicate,summarized to show the present status of therespectively (Figure 6). In the case of the Ti-

chemistry, the function and the application ofcontaining octosilicate (Si/Ti = 50), Ti existed

their intercalates/hybrids. Using the reactivity

asspeciesof silanol groups on the surface of layered

coordinatedsilicates, a wide variety of metal ions, metal

species. In addition, as the Si/Ti ratio

complexes, metal oxide/sulfide compounds,

increased (Si/Ti = 10 and 20 for magadiiteandand octosilicate), the products were notimmobilized. The isomorphous substitution of

crystalline phases as shown by their XRD

Si4+ in the frameworks of layered silicates withpatterns. The capacity of the incorporation ofother metal cations, such as Al3+ and Ti4+, has

Ti into the silicate framework by the

been used to obtain novel functional layered

isomorphous substitution of Si is higher forsilicates.

atetrahedrally

togetherwithcoordinatedoctahedrally

the silicates with thicker silicate layers(magadiite > octosilicate, Table 1).

metallic

have

been

The functionalization of the interlayer
space,

The applications of the layered silicates

nanoparticles

external

surfaceandsilicate

framework of layered silicates with inorganic

doped with heteroelements as the precursor

elements

has

been

reportedandtheof porous materials are worth investigating

conversion of the heteroelements doped

further. Novel materials’ design by thelayered silicates into porous structures suchfunctionalization through the ion exchange

as zeolites, mesoporous silicas, and pillaredand grafting will be done.

layered structures is worth investigating
further.
5. Acknowledgement

MakotoOgawa

isgratefulfortheDistinguished Professor Grant (Grant number
N41A640072) from the National ResearchCouncil of Thailand (NRCT). This work was
supported by a Moonshot project (Grant
number JPNP18016) from the New Energy
andIndustrial

Technology

Developmentof

Organization (NEDO), Japan, and joint

isomorphous substitution of Si with Ti in the

research program of the Institute of Materials

silicate layers. Reprinted with permission

and Systems for Sustainability, Nagoya

from ref (67). Copyright (2022) American

University.

Figure6.

Schematicdrawing

Chemical Society.

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