Recent Patenting Trends in NanoParticle Manufacturing

Recent Patenting Trends in
NanoParticle Manufacturing

Nanoformulation 2010

Stockholm, 11/06/2010
11th June 10
Ilian Iliev, CEO and co founder of CambridgeIP
Quentin Tannock, Chairman and Co Founder of CambridgeIP
Karishma Jain, Associate Consultant

© 2010 CambridgeIP Ltd. All rights reserved

Contents
• CambridgeIP background
• Patent landscaping – a primer
• Patenting in Nanotech broadly
• Patenting in Nanoparticle Manufacturing

© 2010 CambridgeIP Ltd. All rights reserved.
2

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Contents

4

A reminder: why Patent Landscaping is necessary

Patents can be a highly reliable source of information about an
industry
• Patents as data are structured, comparable, objective and information rich
• Information on technology, inventors, linkages to other fields…

But… there are major
challenges related to
• Defining your technology
space
• Identifying relevant A simple search for
patents ‘silicon device’ returns
671,882 patents! Where
• Interpreting the results do you begin?

Akin to finding multiple needles in multiple haystacks

5 © 2009. CambridgeIP. Ltd. Allrights
© 2010 CambridgeIP
All rights reserved.
reserved

Multiple patents protect a single product or
process

Valves and Mouthpiece
Canister

6 Actuation System © 2010 © 2010 CambridgeIP Ltd. All rights reserved.
CambridgeIP. All rights
reserved

Discovery of networks and knowledge flows
Case Study:Plastic Logic,
Cambridge University Spin-
Blue: Inventor
off Red: Owner
Size: Quantity

Number of Patents: Annual and Cumulative
Number of New Applications Cumulative

60 400

350
50
300
Patents - Cumulative

40
Patents - Yearly

250

30 200

150
20
100
10
50

0 0

7
1998 1999 2000 2001 2002 2003 2004 2005 2006 2007 2008 2009 2010
© 2010

© 2010 CambridgeIP Ltd. All rights reserved

Contents

8

Nano-context: Key Conclusions from Previous
Research (1)
Patent trends research indicates that nanotechnology:
• Is a cross-cutting technology applicable to multiple market sectors
• Has high levels of public development and support , compared to the average in other
fields
• Global development and application
– US is a leader in terms of volume of patent filings , and is highly diversified
– Nanobiotechnology dominates European patent filings
– Nanoelectronics dominates Japan activity

Source: EPO (2007)
9

Nano-context: Key Conclusions from Previous
Research (2)
CambridgeIP research reveals:
• Higher inter-relation between patents in nano-field
– Higher patent forward citation rates for patents relative to forward citation rates observed elsewhere
– Rising strength of China: Rise in China patenting rates (accompanied by acquisitions of companies and
technologies by Chinese companies)
– Russia: Russian nanotechnology developments are often be overlooked in the English speaking world. Many
clients have little or no exposure to patent and non-patent literature in Cyrillic. The role of RusNano?
• Patenting rates slow down from 2004 in some nanotechnology sub-spaces, in part
driven by:
– Delays in patentn filings (perhaps due to „time to market‟ and other considerations)
– Fewer nano patents granted: Increased sophistication and rigor of the nano-patent examination process
– Lower levels of VC investment: end of the honeymoon?

• Multiple & varied technology areas with inter-dependencies and growing
number of applications

1996: A relatively 2006: An „explosion‟ of
small number of activity across an ever-
IPCs is associated increasing array of
with the industrial applications: no
nanotechnology single „core area can be
field discerned: indicative of a
„raft‟ or a „platform‟
technology entering
maturity

1

Industry Example: Photovoltaics patents and nano-
related patents Assignee
OVERALL
Patent #

PV and Wind are the most highly patent low-carbon energy fields SHARP 608
CANON 561
The key patent holders differ between PV overall and nano-PV SANYO 483
MITSUBISHI 416
MATSUSHITA ELECTRIC 359
Number of patents by year
FUJI ELECTRIC CO LTD 258
9 00 Photovoltaic Space and subspaces HITACHI 223
MERCK PATENT GMBH 198
800 KYOCERA CORPORATION 190
KANEGAFUCHI KAGAKU KOGYO KK 184
7 00 OVERALL Nanotech Related
Assignee Patent # Assignee Patent #
6 00
SHARP 608 UNIVERSITY CALIFORNIA 42
5 00 CANON 561 NANOSOLAR INC 41
SANYO 483 KONARKA TECHNOLOGIES INC 40
4 00 MITSUBISHI 416 GENERAL ELECTRIC CO 34
MATSUSHITA ELECTRIC 359 SAMSUNG ELECTRONICS CO LTD 30
FUJI ELECTRIC CO LTD 258 WILLIAM MARSH RICE UNIVERSITY 26
3 00
HITACHI 223 CANON 24
MERCK PATENT GMBH 198 DUPONT 22
2 00 KYOCERA CORPORATION 190 SONY CORP 21
KANEGAFUCHI KAGAKU KOGYO KK 184 NANOSYS INC 19
1 00

0

0

4

6
2
80

88
84

86
82

90
78

98
76

94

96
92

0

0

0

0
20

20

20

20
19

19

19

19

19

19

19

19

19

19

19

19

Nanotech Related Am orphous Silicon Cd Te CIS & CIGS Dy e Sensitized

Source: Chatham House – CambridgeIP (2009) ‘Who Owns Our Low-Carbon Future?’
Full report available for download from CambridgeIP’s website: www.cambridgeip.com
Report was co-authored with Bernice Lee and Felix Preston of Chatham House

Contents

12

Nanoparticle manufacturing background

Nanotechnology has cross-sectoral application

A number of challenges before its full commercial
potential is realised:

• Lack of large scale manufacturing techniques
• Challenge on cost effective production
• Health/safety concerns
• Very long time to market for nano-products
• Unclear regulatory framework – affecting investment decisions
into R&D and manufacturing capacity

13

Patent Study Methodology

We undertook patent research into key nano-particle manufacturing
techniques and identified patents of interest emerging over the last 5 years

• Using expert interviews and our patent data mining we built a
technology matrix covering:
– 15 manufacturing methods
– 14 industry applications
• We conducted a semi-automated and expert-validated analysis of the
space and identified example patents
• In the next slides we show some of our results
• Further research is available on request

14

Nano-Technology Manufacturing Methods

Creating nanoscale devices by using larger, externally-
controlled materials, directing their formation

Method Detail Type
Deposition To settle nanoparticles from a bulk Top Down
techniques material onto a pre-existing surface

Mechanical Production of nanoparticles using Top Down
physical mechanism

Wet chemistry Nanoparticles used in chemical organic Bottom Up
solution

Gas phase synthesis Nanoparticles being produced in gas Bottom Up
phase using various technologies

Production in liquid Liquid CO2 infused with nanoparticles Bottom Up
carbon dioxide for coating/cleaning purposes

Use of scaffolds Use of a mould to build nanoparticles Bottom Up
(polymer)

Using small molecular components, building them
up into more complex assemblies

Technology Matrix:
Bio related Fields

NanoParticles Manufacturing drug delivery/ Medicine – scaffolds for Cosmetics
Techniques (re) diagnostics tissue
Formulation engineering
Deposition techniques
lithography x
Top Down

vacuum coating
spray coating
Mechanical
ball milling x
planetary grinding x
Wet chemistry
Sol-Gel Processing x x x x
Hydrothermal synthesis x x x
microemulsion processing x x x x
Bottom Up

nanoemulsion processing x x x x
Sonochemical processing x x x x
Gas phase synthesis
plasma vaporization
chemical vapour synthesis
laser ablation
Production in liquid CO2 x x x x
Use of scaffolds (polymer) x x x x
16

Technology Matrix:
Environment related Fields
Key area of concern for
climate change policy

NanoParticles Manufacturing fuel cells Photovoltaics construction air purification water
Techniques and concrete purification

lithography x x x x
Top Down

vacuum coating x x x x
spray coating x x x x
Mechanical
ball milling x x
planetary grinding x x
Wet chemistry
Sol-Gel Processing x x x x
Hydrothermal synthesis x x x
microemulsion processing x x x
Bottom Up

nanoemulsion processing x x x
Sonochemical processing x x x
Gas phase synthesis
plasma vaporization x
chemical vapour synthesis x
laser ablation x
Production in liquid CO2 x x x x
Use of scaffolds (polymer) x x
17

Technology Matrix:
Industry related Fields

NanoParticles Manufacturing automotive aerospace lubricants for paints, smart catalysis electronics
Techniques industrial coatings
components
lithography x x x x x x
Top Down

vacuum coating x x x x x x
spray coating x x x x X x
Mechanical
ball milling x x x x x
planetary grinding x x x x x
Wet chemistry
Sol-Gel Processing x x x x x
Hydrothermal synthesis x x x x x x
microemulsion processing x x x x x
Bottom Up

nanoemulsion processing x x x x x
Sonochemical processing x x x x x
Gas phase synthesis
plasma vaporization x x x x x
chemical vapour synthesis x x x x x
laser ablation x x x x x
Production in liquid CO2 x x x x x x
Use of scaffolds (polymer) x x x x x x
18

Contents
• Technology Field Definition
• Patent Examples
• Appendices

19

Example Patent: Sol-Gel
aerospace paints, smart construction
coatings and concrete

CN101602508

Method for preparing monodisperse nano silicon dioxide
spherical particle hydrosol and application thereof
Assignee: UNIV ZHEJIANG SCIENCE & TECH [CN]
Inventor: JIANJUN CHEN [CN]; NAIYAN WANG [CN]; LINHUI GAO [CN];
ZHAO WANG [CN]
Publication Date: 2009-12-16

Abstract: The invention discloses a method for preparing monodisperse nano silicon
dioxide spherical particle hydrosol and application thereof. The method adopts a sol-gel
method and comprises the following steps: using ammonia as a catalyst for the
hydrolysis of ethyl orthosilicate, and using ethanol as a solvent to prepare nano SiO2
particles, namely adopting a method for preparing the SiO2 particles through a st ber
method so as to obtain a suspension of the SiO2 particles dispersed in the ethanol
solvent; adopting a heating and blasting process to volatize most of the ethanol in the
suspension so as to obtain a nano silicon dioxide particle slurry; and adding an aqueous
solution of alkamine into the slurry to finally prepare a nano SiO2 hydrosol, wherein the
volatized ethanol can be reused after being collected. The hydrosol is applied to modified
water-based external wall coatings, water-based fire-retardant coatings and water-based
woodwork coatings. The nano silicon dioxide does not exist in the form of powder to
avoid agglomeration of nano particles and improve the dispersity of the nano particles in
the water-based coatings, thereby improving the performances of weatherability,
washability, storage stability and the like of the coatings. © 2010 CambridgeIP Ltd. All rights reserved.

20

Cosmetics Medicine – automotive aerospace electronics
diagnostics

CN101602596
Lithium tantalate nano powder and preparation method
thereof
Assignee: UNIV CHINA GEOSCIENCES WUHAN [CN]
Inventor: JIANHUI HU [CN]; YANGAI LIU [CN]; MINGHAO FANG [CN];
ZHANXING SUN [CN]; CHAOHUI HUANG [CN]
Abstract: The invention relates to lithium tantalate nano powder
and a preparation method thereof, and belongs to the technical
field of functional ceramic powder. The lithium tantalate nano
powder is prepared by a sol-gel method. Ta2O5 and Li2CO3 as
main raw materials and citric acid (CA) as a complexing agent
react to form a stable metal-citric acid complex compound which
is used as a tantalum source and a lithium source; an ethylene
glycol (EG) esterifying agent is added into the metal-citric acid
complex compound to form a polymer network with the citric
acid; tantalum ions and lithium ions are evenly dispersed in the
network to form stable polymer precursor sol; and the polymer
precursor sol is dried and calcined to form LiTaO3 nano powder
with good dispersion property. Because the Ta2O5 is used as an
initial raw material of the tantalum, the cost is low; and the
experimental device requirement is low, the process is simple,
and the operation is convenient.
21

Example Patent: Hydrothermal
drug delivery/ Medicine – catalysis automotive aerospace paints, smart electronics
(re) diagnostics coatings
Formulation

MX2009007013
PROCESSES FOR THE HYDROTHERMAL PRODUCTION OF
TITANIUM DIOXIDE.
Assignee: DU PONT [US]
Inventor: CORBIN DAVID RICHARD [US]; HUTCHENSON KEITH W; LI
SHENG; TORARDI CARMINE; MCCARRON EUGENE MICHAEL
Abstract: The present invention provides hydrothermal
processes for the production of titanium dioxide from titanyl
hydroxide. The use of specific crystallization directors, or
additives, can promote the formation of rutile, anatase, or
brookite. Variation of process operating parameters can lead to
either pigmentary-sized or nano-sized rutile.

22

Example Patent: Sonochemical
automotive electronics

KR20080096023
METHOD OF PREPARING LITHIUM TITANATE NANOPARTICLES
UNDER SONOCHEMICAL CONDITION
Assignee: SAMSUNG ELECTRONICS CO LTD [KR]; UNIV CHUNG ANG IND
[KR]; SEOUL NAT UNIV IND FOUNDATION [KR]
Inventor: SHIM IL WUN [KR]; KWAK HO YOUNG [KR]; LEE SEUNG SOO
[KR]; BYUN KI TAEK [KR]; PARK JONG PIL [KR]; KIM SIN KYU [KR]
Abstract: A manufacturing method of lithium titanate nano particle is provided to
raise a composition and a purity of the lithium titanate by using the precursor
manufactured by coating the lithium hydroxide which is reactant onto a surface of
titanium dioxide. The lithium titanate nano particle can be mass-produced by heat-
treating in the more mild condition in a short time. Furthermore, the lithium
titanate nano particle manufactured from the manufacturing method is usefully
used as the lithium secondary battery cathode material. A lithium titanate nano
particle is manufactured by manufacturing precursor manufactured by coating the
lithium hydroxide onto a surface of the titanium dioxide, and heat-treating the
precursor at the low temperature less than 500deg.C for the short time in the
alcohol solution by performing the sonochemical reaction under the multiplexer
sound wave luminescence condition. The alcohol solution contains a titanium
dioxide(TiO2) and a lithium hydroxide(LiOH).

23

Example Patent: Spray Coating
automotive aerospace paints, smart
coatings

US20090022995
IN-SITU NANOPARTICLE FORMATION IN POLYMER CLEARCOATS
Assignee: University of Kentucky, Institute for Sustainable Manufacturing
(?)
Inventor: GRAHAM USCHI URSULA M [US]; KHATRI RAJESH [US]; DAVIS
BURT H [US]

Abstract: Methods and compositions for forming a transparent
clear coat characterized by a desired property, such as a color
effect, resistance to UV light-induced degradation and/or scratch
resistance, on a substrate are detailed according to embodiments
of the present invention. Particular compositions and methods for
producing a transparent clear coat layer include nanoparticles
formed in-situ during curing of a transparent clear coat. Curable
clear coat compositions are described according to embodiments
of the present invention which include one or more substantially
dissolved nanoparticle precursors.

24

Example Patent: Ball Milling
catalysis fuel cells

WO2009011981
METHOD OF FORMING STABLE FUNCTIONALIZED
NANOPARTICLES
Assignee: UNIV TULANE [US]; MITCHELL BRIAN S [US]; FINK MARK J [US]; HEINTZ
ANDREW S [US]
Inventor: MITCHELL BRIAN S [US]; FINK MARK J [US]; HEINTZ ANDREW S [US]

Abstract: A novel top-down procedure for synthesis of stable
passivated nanoparticles uses a one-step mechanochemical
process to form and passivate the nanoparticles. High-energy ball
milling (HEBM) can advantageously be used to mechanically
reduce the size of material to nanoparticles. When the reduction
of size occurs in a reactive medium, the passivation of the
nanoparticles occurs as the nanoparticles are formed. This results
in stable passivated silicon nanoparticles. This procedure can be
used, for example in the synthesis of stable alkyl- or alkenyl-
passivated silicon and germanium nanoparticles. The covalent
bonds between the silicon or germanium and the carbon in the
reactive medium create very stable nanoparticles.

25

Example Patent: Ball Milling
fuel cells

KR20090074360
POROUS NANOCARBON MANUFACTURING METHOD USING
BALL MILLING
Assignee: LEE IN SOON [KR]
Inventor: LEE IN SOON [KR]; PARK TAE HEE [KR]

Abstract: A method for manufacturing porous nano carbon
through ball milling is provided to control the maximum speed of
a motor of a ball mill based on the sizes of containers. A method
for manufacturing porous nano carbon through ball milling
comprises the following steps of: putting 10g-10kg of natural
graphite or processed artificial graphite with the size of 10mum -
20cm in a ball mill's container; and settling a ball with the size of
8-150mm and the weight of 400g-450kg in the ball mill's
container. The size of the ball depends on the weight of carbon
inputted. The container has 98mm of height and 90mm of inner
diameter. The processing speeds of the ball mill have rotation
speed of 32000rpm and revolution speed of 1200rpm.

26

Example Patent: Chemical Vapour Synthesis

Large Scale Manufacturing
aerospace paints, smart fuel cells electronics
coatings

EP1867386
Method for the production of nanoparticles
Assignee: Applied Materials, Inc (?)
Inventor: WENDLING THOMAS
Abstract: The present invention relates to methods for the
production of nanoparticles which may be optionally coated. In
particular, the present invention relates to methods for the
production of nanoparticles characterized in that precursors are
subjected to substantially the same amount of activation energy
in the activation zone at a predetermined concentration of
precursors and at a predetermined time of exposure to the
activation energy. Furthermore, the present invention relates to
nanoparticles produced by the methods according to the present
invention. Finally, the present invention concerns a device for
producing nanoparticles according to the method of the present
invention. The activation energy is selected from the group of RF
plasma, MW plasma, IR plasma, thermal plasma, heat, photon
absorption, plasma by electric discharge or radioactive radiation
or sonar energy.

27

Example Patent: Production in Liquid CO2
Medicine – automotive aerospace Photovoltaics air electronics
diagnostics purification

US2010044646
Supercritical fluid process for producing nano graphene
platelets
Assignee: Angstron Materials, Inc. (?)
Inventor: ZHAMU ARUNA [US]; JANG BOR Z [US]

Abstract: The present invention provides a process for producing
pristine or non-oxidized nano graphene platelets (NGPs) that are
highly conductive. The process comprises: (i) subjecting a
graphitic material to a supercritical fluid at a first temperature and
a first pressure for a first period of time in a pressure vessel and
then (ii) rapidly depressurizing the fluid at a fluid release rate
sufficient for effecting exfoliation of the graphitic material to
obtain the NGP material. Conductive NGPs can be used as a
conductive additive in transparent electrodes for solar cells or flat
panel displays (e.g., to replace expensive indium-tin oxide),
battery and supercapacitor electrodes, and nanocomposite for
electromagnetic wave interference (EMI) shielding and static
charge dissipation, etc.

28

Example Patent: Use of Scaffolds
Photovoltaics Fuel Cells electronics
coatngs

US2010035062
MANUFACTURING METHODS OF MAGNESIUM-VANADIUM
COMPOSITE OXIDE NANOPARTICLE AND MAGNESIUM-
VANADIUM COMPOSITE OXIDE NANOPARTICLE
MANUFACTURED BY THE SAME
Assignee: Schaefer School of Engineering & Science (?)
Inventor: LIM CHUL TACK [KR]; CHOI CHANG HWAN [KR]; CHUN
BYOUNG JIN [KR]; YANG JIN HYUCK [KR]

Abstract: Provided are manufacturing methods of a magnesium-
vanadium composite oxide nanoparticle that make it possible to
manufacture a composite oxide of several tens of nanometers in
size containing two kinds of metals, and also to accurately design
and manufacture a product material having a desired ratio
between the metals, and a magnesium-vanadium composite
oxide nanoparticle manufactured by the manufacturing methods.
In the manufacturing method, a solution containing a magnesium
salt and a vanadium salt is prepared. An organic polymer having
nano-sized pores is dipped in the prepared solution, and is then
heated until the organic polymer is calcined, thereby
manufacturing a magnesium-vanadium composite oxide
nanoparticle.
29

Toxicology

New EU regulation may require cosmetics
manufacturers to list any nanoparticles contained in
products marketed within the European Union

• Approved on November 2009 by the Council of the
European Union
• All ingredients present in the product in the form of
nanomaterials should be clearly indicated in the list of
ingredients

The ruling defines nanomaterial as 'an insoluble or
1,160 L’Oréal patents including ‘nano’ biopersistant and intentionally manufactured material with one
or more external dimensions, or an internal structure, on the
scale from 1 to 100 nm'.
30

Nanotoxicology: A Large Network

Pioneers in the prevention
Own 3 patents on Now working with the EC
Cell Nanotoxicology
(See next Slide)

Specialized Magazine

A Network of Universities and Institutes

Database

31

Example Patent: Toxicology
Nanotoxicity

WO2007094870
TOXICOLOGY AND CELLULAR EFFECT OF MANUFACTURED
NANOMATERIALS
Assignee: UNIV CALIFORNIA
Inventor: CHEN FANQING [US]
Abstract: The increasing use of nanotechnology in consumer
products and medical applications underlies the importance of
understanding its potential toxic effects to people and the
environment. Herein are described methods and assays to predict
and evaluate the cellular effects of nanomaterial exposure. We
have performed whole genome expression array analysis and high
content image analysis-based phenotypic measurements on
human skin fibroblast cell populations exposed to multiwall
carbon nano-onions (MWCNOs), multiwall carbon nanotubes
(MWCNTs), and semiconductor nanocrystals. Here we demonstrate
that exposing cells to nanomaterials at cytotoxic doses induces
cell cycle arrest and increases apoptosis/necrosis, activates genes
involved in cellular transport, metabolism, cell cycle regulation,
and stress response.; Certain nanomaterials induce genes
indicative of a strong immune and inflammatory response within
skin fibroblasts. Furthermore, the described MWCNOs can be used
as a therapeutic in the treatment of cancer due to its cytotoxicity. © 2010 CambridgeIP Ltd. All rights reserved.
32

Contents
• Project Background and Definitions
• Technology Matrix
• Patent Examples
• Conclusion

33

Patterns noticed in initial searches:

• Most nanoparticle manufacturing patents primarily target
a specific material or class of materials rather than an
application
• The application patents typically tend to be for
formulations involving several components, and methods
for manufacturing them
• Many of the recent patents are from key emerging
market locations including China and Russia
• Many of the patents are about the manufacturing
method and the nanoparticles: indicative of early stage
of development of process


Volume/Quality Requirements for
Nanoparticle Manufacturing
We know some of the volume/quality requirements for nanoparticle manufacturing

High
Scaffolds for Drug Fuel Cells
tissue formulations/
engineering Photovoltaic
delivery

Medical Cosmetics
Quality Requirements

Diagnostics

Catalysis Air
purification

Automotive
Aerospace

Water
purification
Industrial
lubricants
Paints/coatings
Experimental
applications Cement/
Construction
Low
Low Volume Requirements High

The key question will be which are the technologies that become adopted/accepted in each of these fields
As the technology matures, the different industry field requirements will determin industrial reserved.
© 2010 CambridgeIP Ltd. All rights
R&D

…and finally…
Please contact Ilian Iliev for a copy of the results and any other
questions you may have:

Ilian.iliev@cambridgeip.com
+44 77 863 73965

Thank You !
Ilian Iliev Quentin Tannock
(CEO and Co Founder) (Chairman and Co Founder)
ilian.iliev@cambridgeip.com Quentin.Tannock@cambridgeip.com
GSM: +44-077-863-73965 GSM: +44-077-862-10305
Tel: +44-1223-370-098 Tel: +44-1223-370-098

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Fax: +44 (0) 1223 370 040 © 2010 CambridgeIP Ltd. All rights reserved.

36 © 2010 Cambridge Intellectual Property Ltd. All rights reserved.

Example Patent: Planetary grinding
Cosmetics drug drug delivery Medicine –
reformulation / diagnostics
reconstitution

WO2007109244
NOVEL NANOPARTICLES FOR DELIVERY OF ACTIVE AGENTS
Assignee: MOREHOUSE SCHOOL OF MEDICINE [US]; LILLARD JAMES W
[US]; SINGH RAJESH [US]; SINGH SHAILESH [US]
Inventor: LILLARD JAMES W [US]; SINGH RAJESH [US]; SINGH SHAILESH
[US]

Abstract: Milled nanoparticles comprising a biolgically active
agent, at least one biopolymer and a coating containing at least
one coating which is a polymer or ligand are produced using
milling and coating techniques which have not previously been
used for these applications

37

electronics

CN101597035
Method for preparing nano vanadium nitride electrode
material
Assignee: UNIV SICHUAN [CN]
Inventor: HENG LIU [CN]; LING LU [CN]
Abstract: The invention relates to a method for preparing a nano
vanadium nitride electrode material for a super capacitor. The
method comprises the following steps: using analytically pure
vanadium pentoxide as an initial raw material, preparing a
precursor of nano vanadium nitride by a sol-gel method, filtering
sol of V2O5, refrigerating the precursor for 20 to 30 hours at the
temperature of between 20 DEG C below zero and 50 DEG C
below zero in a refrigerator, then putting the precursor into a
refrigeration dryer, and refrigerating and drying the precursor for
20 to 30 hours; and performing nitriding and reducing reaction
on the precursor for 1 to 3 hours at the temperature of between
550 and 800 DEG C under the atmosphere of ammonia gas to
obtain nano-scale vanadium nitride granules. The method is
simple to operate, and can prepare the spherical vanadium nitride
granules of about 12 nanometers; and the vanadium nitride
granules used as the electrode material for the super capacitor
have specific capacity of 398 to 608 F/g.
38

Example Patent: Laser Ablation
aerospace lubricants for paints, smart
industrial coatings
components

US20050287308
Method for producing nanoparticles and nanostructured films
Assignee: UNIV TEXAS
Inventor: BECKER MICHAEL F [US]; KETO JOHN W [US]; KOVAR
DESIDERIO [US]

Abstract: A method for producing composite, shelled, alloy and
compound nanoparticles as well as nanostructured films of
composite, shelled, alloy and compound nanoparticles by using
laser ablation of microparticles is disclosed.

39

Example Patent: Gas Phase Solid Gel
aerospace paints, smart construction
coatings and concrete

CN1915811
Method for preparing Nano carbon white from fly ash based
on gas phase sol gel method
Assignee: UNIV JIANGSU [CN]
Inventor: NI LIANG JIANG [CN]
Abstract: This invention relates to a sol-gel method for
preparing nanoscale white carbon black from fly ashes, NaF and
concentrated H2SO4. The method comprises: (1) dissolving fly
ashes in HNO3, and sintering at a high temperature to obtain
SiO2; (2) dropping concentrated H2SO4 onto SiO2 and SiF4 to
generate SiF4 gas, introducing SiF4 gas into solution of sodium
dodecyl sulfate, Sodium dodecyl sulfonate and cetyltrimethyl
ammonium bromide, hydrolyzing to obtain sol and then gel, and
calcining to obtain nanoscale white carbon black. The obtained
nanoscale white carbon black has diameters of about 20nm, and a
specific surface area of 58-631 m2/g. Besides, the nanoscale
white carbon black is semi-transparent white, and has such
advantages as high purity, no obvious aggregation, high
dispersibility and high activity. The method has such advantages
as mild reaction conditions, easy control of the techniques and
simple process.

40

drug delivery/ paints, smart
(re) coatings
Formulation

WO2008072239
FORMATION OF NANOMETRIC CORE-SHELL PARTICLES
HAVING A METAL OXIDE SHELL
Assignee: SOL GEL TECHNOLOGIES LTD (Israel)
Inventor: TOLEDANO OFER [IL]; SERTCHOOK HANAN [IL]; ABU-REZIQ
RAED [IL]; BAR-SIMANTOV HAIM [IL]; SHAPIRO LEORA [IL]
Abstract: A process for preparing nanocapsules having a core-
shell structure, comprising: (a) preparing an oil-in-water
emulsion by emulsification of an oily phase that comprises a core
material, in an aqueous phase, under high shear forces, wherein
one or both of the oily phase, and the aqueous phase comprises a
sol-gel precursor; (b) subjecting the emulsion obtained in (a) to a
high pressure homogenization to obtain a nano-emulsion; and
(c) applying conditions for hydrolyzing and polycondensing the
sol-gel precursor to obtain nanocapsules having a metal oxide
shell encapsulating the core material, said nanocapsules have a
particle size distribution of: d10 = 10-80 nm, d50 = 30-200 nm,
and d90 = 70-500 nm, in diameter. The invention also relate to
nanocapsules having the above particle size distribution and to
composition comprising the nanocapsules.

41

Recent Patenting Trends in NanoParticle Manufacturing

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