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Combining the strengths of UMIST and The Victoria University of Manchester Making and Using Nanoparticles Paul O Paul O Brien Brien The School of Chemistry The School of Chemistry and The Manchester Materials Science Centre and The Manchester Materials Science Centre

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Page 1: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

Making and Using Nanoparticles

Paul O Paul O’ ’Brien Brien The School of Chemistry The School of Chemistry and The Manchester Materials Science Centre and The Manchester Materials Science Centre

Page 2: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

Structure of Talk

• Why now ? – Looking at some nanodimensional objects by way of introduction

• Synthetic approaches semiconductors • How nanoparticles grow and rods and tetrapods • Other materials a rogues gallery • What are some of the opportunities

– The Nanoco Technologies Ltd perspective

• Closing remarks

Page 3: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

Electronics, Volume 38, Number 8, April 19, 1965

Page 4: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

350 nm

250 nm

180 nm

Page 5: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

10 nm

1850

1980 2004

Industrial Development and a History of Precise Size Control

What are lost dimensions?

Ball Bearings for the 21 st Century!

Page 6: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

Quantum Dot and nano Particle Structures I

SeCd P O C

‘Metal Organic Dot’

Crystalline core e.g CdS

Organic Capping Agent

Page 7: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester Chem Commun., 1999, 1573­1574

Page 8: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

More CdSe

Page 9: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

Sample of PbS Coated with TOPO

J. Materials Chemistry, 1997, 7, 1011

Page 10: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

Uniform Microscopic NH 4 TiOF 3 or TiO 2 Mesocrystals by a Room Temperature Self-assembly Process

Water in

Water out

Brij Series Surfactants

H 3 BO 3 (NH 4 ) 2 TiF 6

35 o C

Schematic of Experiment

Incomplete hydrolysis of Ti complex:

[TiF 6 ] 2­ + nH 2 O [TiF 6­n (OH) n ] 2­ + nHF (n ≦ 3)

Formation of NH 4 TiOF 3 :

[TiF 3 (OH) 3 ] 2­ + H + + NH 4 + → NH 4 TiOF 3 $ + 2H 2 O

Removal of HF:

H 3 BO 3 + 4HF → HBF 4 + 3H 2 O

e.g. 15 g of Brij 58 is added into the

50 ml bath solution containing

(NH 4 ) 2 TiF 6 (0.1 mol∙dm ­3 ) and

H 3 BO 3 (0.2 mol∙dm ­3 ).

Page 11: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

Impact of sintering [NH 4 ][TiOF 3 ] to TiO 2

SEM images of samples before and after sintering. a, b, top view and cross­ section of an as­prepared sample. c, ultrahigh resolution image of a broken point. d, e, top view and cross­section of after a sintered sample. f, ultrahigh resolution image of surface .

a

e d

b c

f

Page 12: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

TEM analysis of as­prepared samples

TEM images and SAED Pattern of as­prepared samples.

Page 13: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

16nm

Particles Prepared with 30% Brij58, after sintering

12nm

18nm

TEM:

Page 14: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

Page 15: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

Page 16: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

Anatase

001

100

110

Page 17: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

Structure of Talk

• Why now ? – Looking at some nanodimensional objects by way of introduction

• Synthetic approaches semiconductors • How nanoparticles grow and rods and tetrapods • Other materials a rogues gallery • What are some of the opportunities

– The Nanoco Technologies Ltd perspective

• Closing remarks

Page 18: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

Page 19: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

(I) Rapid Nucleation (II) Growth

of Nuclei

Driven by decomposition

Interaction with coordinating solvent

(III) Growth Terminates Coated Particle

Requirements for Nanoparticulate Synthesis

Precursors

Page 20: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

. Cd(Se 2 CNRR’) 2 CdSe O’Brien et al Chem Comm, 1998 1849, ibid 1999, 1573.

Me 2 Cd + TOPSe CdSe

The NanoCo Process

Patent Family UK patent application No. 9518910.6 PCT application WO 97/10175.

US patent No. 09/043,258 (Granted) EP patent application No. 96927134.5

Page 21: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

New strategies for the synthesis of nanoparticulates

X­Ray single crystal structure of Cd(E 2 CNCH 3 (CH 2 CH 2 Ph)] 2

Page 22: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

350 400 450 500 550 600

0.0

0.2

0.4

0.6

0.8

1.0

Absorbance (a.u.)

Wavelength (nm)

T6 200C T6 250C T6 300C

UV­Vis spectra of aliquots T6 (20 min), of runs CdS 200°C,

CdS 250°C and CdS 300°C fitted to a direct transition.

Cd(E 2 CNCH 3 (CH 2 CH 2 Ph)] 2

300 °C 200 °C

250 °C

Page 23: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

Page 24: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

Quantum Dot Structures I

SeCd P O C

‘Metal Organic Dot’

Crystalline core e.g CdS

Organic Capping Agent

Page 25: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

CdSe core

ZnS shell

Ligand coating

Quantum Dots II

H 2 N

O P

Core Shell Structures •Broadband excitation •Narrow bandwidth emission •Emit light of high intensity •Available in many colours •Resistant to quenching •Photochemically stable

Page 26: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

Page 27: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

350 400 450 500 550 600 0.00

0.05

0.10

0.15

Intens

ity

Wavelength(nm)

QDs in chloroform QDs­tuftsin aqueous solution (a)

400 450 500 550 600 650 0.0

0.2

0.4

0.6

0.8

1.0 Intens

ity

Wavelength (nm)

QDs in Chloroform QDs­tuftsin aqueous solution

(b)

UV Vis and PL of QDs

Page 28: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

Structure of Talk

• Why now ? – Looking at some nanodimensional objects by way of introduction

• Synthetic approaches semiconductors • How nanoparticles grow and rods and tetrapods • Other materials a rogues gallery • What are some of the opportunities

– The Nanoco Technologies Ltd perspective

• Closing remarks

Page 29: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

b

Page 31: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

N = 2

Total atoms = 4 Surface atoms = 4

N = 3

Tetrahedron Cube N = 2

Total atoms = 8 Surface atoms = 8

Total atoms = 10 Surface atoms = 10

N = 3

Total atoms = 27 Surface atoms = 26

Page 32: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

Shape Total atoms Surface atoms

Cube Bcc packing (N+1) 3 +N 3 6N 2 +2

Cube Fcc packing 4N 3 +6N 2 +3N+1 12N 2 +2

Octahedron Fcc packing 3

N 3

2N 3

+ 4N 2 ­8N+6

Tetrahedron Fcc packing 3

N 2 N

6 N 2 3

+ + 2N 2 ­4N+4

Cuboctahedron triangular faces, fcc packing 1

3 11N 5N

3 10N 2

3

− + − 10N 2 ­20N+12

Relationship between the number of shells N and the total number of atoms and surface atoms for different shapes

P. John Thomas and P. O’Brien J. Amer. Chem. Soc., 128, 2006 5615­5615

Page 33: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

1000 2000 3000 4000 5000

30

40

50

60

70

80

90

Fraction of surface atoms %

Number of atoms

Tetrahedron BCC cube Octahedron FCC cube Cuboctahedron

Page 34: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

D=(N+2)/3

N = 4

D=2

D=(N+2)/3

N = 4

D=2

750 1500 2250 3000

36

40

44

48

52

56

60

7

6

5

Fraction of surface atoms %

Number of atoms

Page 35: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

1000 1500 2000 2500 3000

40 42 44 46 48 50 52 54 56

b a

b a b

SAP

T a Plot showing the changes in the surface atom percentage (SAP) accompanying the growth of four hexagonal branches. The dotted line represents the SAP profile that the seed would have adopted if branching had not taken place.

Page 36: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

2 4 6 8 10 12

1

2

3

4

5 2 4 6 8 10 12 14 16 18

∆SAP m

ax

Edge length (nm)

Base length (nm)

:Plot showing changes in the maximum difference in the surface atom percentage (∆SAPmax) between the tetrahedron and the corresponding structures with four

hexagonal branches grown from a CdSe seed.

Page 37: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

Sample mmol CdAc2 Final Molarity

λem (nm) % rods Diam ** (nm) (std)

A 1.3 0.011 465 <5 3.5 (0.7) B 2.2 0.018 489 <5 4.0 (1) C 21.7 0.181 499 ~15 6.5 (1) D 31.6* 0.198 504 72 7.0 (1)

Chem. Comm. 2005 2817­2819

Page 38: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

Powder XRD showing hexagonal phase of A and the cubic phase of B. Inset at higher resolution.

Page 39: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

Page 40: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

002 0.31 nm

The low temperature (140 ºC) growth of hexagonal ZnS nanorods in a mixture of hexadecylamine and octylamine from sulfur and zinc acetate

J. Experimental Nanoscience 2006, in press.

Page 41: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

ZnS as before but at 180 º C

Page 42: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

25 30 35 40 45 50 55 60 65

Counts (a.u.)

2­theta (degree)

XRPD of ZnS (a) rods grown at 140 o C and (b)dots grown at 180 o C. Also shown are the bulk indices for hexagonal (below) and cubic (top).

Page 43: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

Structure of Talk

• Why now ? – Looking at some nanodimensional objects by way of introduction

• Synthetic approaches semiconductors • How nanoparticles grow and rods and tetrapods • Other materials a rogues gallery • What are some of the opportunities

– The Nanoco Technologies Ltd perspective

• Closing remarks

Page 44: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

Some Oxides…………..

Page 45: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

Precursor Solvent Reaction T m

Time (hour)

Product and Size

Fe(acac) 3 HDA 250 o C 2 Fe 3 O 4 10.5 nm

Mn(acac) 2 HDA 270 o C 1 MnO 17.5 nm

Co(acac) 2 HDA 240 o C 3.5 CoO 20.0 nm

Ni(acac) 2 HDA+TOPO (2:1 w/w)

220 o C 2 NiO 14.0 nm

Cr(acac) 3 HDA 340 o C 3 No Reaction

Generic routes to metal oxides J. Mater Chem in press 2006

Page 46: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

(A)TEM image, (B) Selected area electron

diffraction (SAED) pattern acquired from

the corresponding Fe 3 O 4 nanoparticles,

(C) HRTEM image of a 10 nm diameter of Fe 3 O 4 nanoparticle, (insert) FFT of the HRTEM,

(D) XRD pattern of Fe 3 O 4

20 40 60 80 0

5000

10000

15000

20000

25000

30000

35000

40000

(440)

(311)

(311)

(311)

(311)

(311) Intensity (a

rb)

2θ (deg)

D (311)

Page 47: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

30 40 50 60 70 80

1000

2000

3000

4000

(220)

(200)

Intensity (arb)

2θ (deg)

D

(111) Fig. 3 (A) TEM image, (B) SAED pattern acquired from the corresponding MnO nanoparticles, (C)HRTEM image of a 18 nm diameter of MnO nanoparticle, (insert) FFT of the HRTEM, (D) XRD pattern of MnO

Page 48: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

Some Cobalt Phosphide………..

Page 49: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

TEM images of CoP nanowires prepared with different weight ratios of HDA to TOPO:

1:2 1:1

However, the reaction of [Co(acac) 2 ]with TOPO as the only solvent did not give any wires of CoP even at 360 o C over three hours. Similar experiment in HDA alone gave only CoO nanoparticles.

J. Amer. Chem. Soc., 2005, 127, 16020­16021

Page 50: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

20 40 60 80 0.0

0.2

0.4

0.6

0.8

1.0

(203)

(301) (020)

(103)

(211)

(112)

(200)

(111)

(011)

Intensity

2θ (Degree)

(101)

Page 51: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

EuS and EuSe…………..

Page 52: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

NaCl type structures

Eu(II) chalcogenide nanocrystals

Page 53: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

Preparation of EuS using photo-irradiation

Energy levels of EuS-complex

Photo-reduction

Eu(III) complex Eu(II)S

Excitation spectrum from ‘T. Yamase et al, Chem. Lett., 907 (1997)

in acetonitrile (r.t) Solid(4.2 K)

LMCT (S - Eu)

Phonon-assisted electron transitions 4f-4f transition

400 450 500 550 600 650 700 750 Wavelength / nm

[Eu(dtc) 4 ] ­

Page 54: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

0

0.2

0.4

0.6

0.8

1

300 400 500 600 700 Wavelength / nm

White LED for excitation light source

Em of White LED Ex of Eu complex

Na[Eu(S 2 CEt 2 ) 4 ]∙5H 2 O in acetonitrile (1 mM)

Absorbance ~ 0.4 / cm (440 nm) for 3 days

White LED

Glass plate

solution

shield

Page 55: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

EuS nanoparticles from single-source precursor

Y. Hasegawa, M. Afzaal, P. O’Brien, Y. Wada, S. Yanagida, Chem. Commm., 2005 242­244

Page 56: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

TEM observations

Page 57: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

Sulfides by CVD………..

Page 58: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

Substrate

Transport (1)

Adsorption (2)

Reaction (3)

Desorption (6)

Ligand

Ligand

Centered metal

Diffusion (4)

Nucleation and growth (5)

By­product (7)

The CVD Process

Page 59: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

The AA­CVD Process

Mixed Solution of Presursor and Solvent

Precursor and solvent Vapour Adsorbed

Presursor products Reaction

Delivery Vapourization Vapour Transport

Surface Reaction

(1) (2) (3) (4)

Adsorbed Precursor

Reaction Products

Substrate Droplets

Page 60: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

Page 61: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

J. Mat Chem., 2004

Page 62: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

A

A

B

B

A Route to Nanowire Superlattices

Growth of nanowire superlattice structures for nanoscale photonics and electronics: M.S.Gudiksen, L.J.Lauhon, J. Wang, D.C. Smith and C.F.Lieber, Nature 415, 2002, 617­620

Page 63: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

• Our previous studies on the growth of PbS thin films by AA and LP­MOCVD on glass and Si substrates, have lead to films comprising large (ca. 1 μm) cubic crystallites (Figure 2).

• Our present study, using Si substrates seeded with Au nanoclusters, via a custom made AP­MOCVD kit, has yielded films of radically different morphology

• (Figure 3).

PbS films deposited on glass.

SEM images of PbS deposited at (a) T prec = 325 o C, T subs = 350 o C,

1 μm

1 μm

M. Afzaal, K. Ellwood, N. L. Pickett, P.O’Brien, J.Raftery, J.Waters J. Mater. Chem., 2004, 14, 1310

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Combining the strengths of UMIST and The Victoria University of Manchester

Page 65: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

Chemical Route to Punctuation

?

Page 66: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

Silica coated PbS nanowires M. Afzaal and P.O’Brien

Journal of Materials Chemistry 2006 16, 113­115.

(a) (b)

100nm 50nm 50nm

(c) (d) (e) 200 400

511

Page 67: Making and Using Nanoparticles · Making and Using Nanoparticles ... PCT application WO 97/10175. ... ra c t i o n o f s u rfa c e a t o m s

Combining the strengths of UMIST and The Victoria University of Manchester

New Ways to Tellurides……..

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Pr P

N H

P i Pr

Se Se

i Pr i Pr

Pr P

Pr Cl

SiMe 3 N H

Me 3 Si

M Se P

N P Se

i Pr

i Pr

i Pr

i Pr

Se

M Se

M

Se M P

N P

Se

P N

P

Se

P N

P Se

i Pr i Pr

Pr i Pr

i Pr i Pr

Pr Pr

Pr

Pr

Pr i Pr

Se, toluene

NaOMe/MeOH

i

i

i

i

i

i

i i

i

CuCl 2 , Cu(OAc) 2 , AgNO 3 or AuCl

4 M = Cu 5 M = Ag 6 M = Au

Imino­bis(diisopropylphosphine chalcogenide)

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• Efficient synthesis of “air­stable”

M [N(SePR 2 ) 2 ] 2 (yields 95­99%).

• Reaction can be scaled up (~25g) without loss to quality/yield.

• “Dot” synthesis is convenient and efficient.

Se

M

Se P

N

P Se P

N

P Se

R

R R

R PO OP

P O

O P

MSe

PO OP

P O

O P

MSe TOP / TOPO

where R = i Pr or Ph and M = Cd, Zn or Hg

200 o C

PL of CdSe by Thermolysis of Cd[N(SeP i Pr 2 ) 2 ] 2

D.J.Crouch, P. O’Brien, M.A.Malik, P.J.Skabara and S.P. Wright, Chem. Commm., 2003 1454.

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T. Chivers, DJ. Eisler, JS Ritch, Dalton Trans. 2005, 2675.

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HRTEM and FFT (inset) of the films grown at 475 ºC

J. Amer. Chem.Soc. 2006, 128, 3121­3122

TEM Pictures

of Sb 2 Te 3

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Just when you thought you understood!

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Mo Complex from Woollins’ Reagent R

P R

Cl Si R

R H N

R

Si

R

R

R

H N

P P

Se Se

R

R

R

R

Si R

R

Cl

R

2 + + 4

+ Se

R P

R

H N P

R

R

R P

R

H N P

R

R

2

70 o C

Reflux, 110 o C

3 h

6 h

NaOMe, MeOH

MoCl 5

N P

P

Se

Se

R R

R R

Mo

3

P Se

Se

Mo Se

Se P

R

R

R

R O

Obtained product

May not get Wollins Reagent, but the “Wrong Ligand”

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R P

R Cl Me Si

Me

Me

N Si

Me

Me

Me

R P

R N P

R

R

R P

R

H N P

R

R Se Se

Se +

MAIN PRODUCT

Relux

High Conc

H H

R P

R Cl Me Si

Me

Me

N Si

Me

Me

Me

R P

R Si

Me

Me

Me

R P

R Se P

R

R Se Se

Se +

BY­PRODUCT

Heat

Low Conc

H

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[Mo 2 O 2 Se 2 (Se 2 P i Pr 2 ) 2 ] MoCl 5 and[ i Pr 2 PSe] 2 Se

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DIALKYLDICHALCOGENOPHOSPHINATES

R P

R C l P

R

R C l

S e + S e

P R

R C l

S e P

R

R S H

S e + N a H S + N a C l

P R

R C l

S e P

R

R S e H

S e + N a H S e + N a C l

N a + S e

L iq u id N H 3 , ­ 7 8 o C

Not­reproducible with added difficulty of using NaHSe

Unstable, never isolated, used in situ to make metal complexes, no solid state characterization

References: (a) J. Inorg. Nucl. Chem. 1974, 36, 472­5; (b) Angw. Chem. 1969, 8, 89. (c) Polyhedron 1991, 10, 2641.

Previous Work

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Novel Synthetic Route (1)

R P

R Cl H Si

Cl

Cl

Cl N Et

Et

Et

R P

R Si Cl

Cl

Cl

H N

Et

Et

Et

Cl + + + Toluene, 6h

Room temp

STEP 1: BENKESER REACTION

STEP 2: INSERT Se

R P

R Si Cl

Cl

Cl

3 Se, reflux 6 h

4 Se, reflux 6 h

R P

R Si Cl

Cl

Cl

Se P

R

R Se Se

R P

R P

R

R Se Se

Si

Cl

Cl

Cl

Se Se Si Cl

Cl

Cl

Si

Cl

Cl

Cl

+

+

2

R= Isopropyl R = Isopropyl

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Novel Synthetic Route (2) • Alternatively, use excess Lewis Base NEt 3 to stabilize ionic species e.g. [( i Pr) 2 PSe 2 ] ­

• HSiCl 3 /NEt 3 : did not work due to the formation of [HNEt 3 + ][SiCl 3 ­ ]

• HSiEt 3 /NEt 3 : worked

R P

R Cl

H Si

Et

Et

Et N Et

Et

Et

R P

R Si Et

Et

Et

H N

Et

Et

Et

Cl

+ +

+ Toluene, 6h

Room temp

STEP 1: BENKESER REACTION

STEP 2: INSERT Se

R P

R Si Et

Et

Et

2 Se, reflux 20 h

Si Et

Et

Et

Si

Et

Et

Et R

P R

Se

Se

H Si

Et

Et

Et N Et

Et

Et

+ +

N Et

Et

Et

H +

R= Isopropyl; Phenyl

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Crystal Structures

[ i Pr 2 PSe 2 ][HNEt 3 ] Yield = ~ 85%

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Group 13 complexes

n [R 2 PX 2 ] ­ + M n+ [R 2 PX 2 ] n M MeOH

Room Temp. R = Ph; i Pr X = S; Se M n+ = In 3+ ; Ga 3+

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Cu ­ Precursor

C 24 H 56 Cu 4 P 4 Se 8 , Mr =1354.41, Monoclinic, space group P2(1)/n, a = 12.9380(16)Å, b = 17.527(2) Å, c = 18.617(2) Å, a = 90, b = 91.453(2), g = 90, V = 4220.3(9) Å 3 , Z = 4, rcalculated = 2.132 g cm­ 3, m = 9.056 mm ­1 , T = 100(2) K. Crystal size 0.35 x 0.30 x 0.2 mm, l = 0.71073 Å, R1= 0.0309, wR2 = 0.0590 .

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CuInSe CuInSe 2 – Tetragonal – 40­1478

Intensity (a

.u)

2 Theta (degree)

5 10 20 30 40 50 60 70 80 90

CuInSe2 (JCPDS 40­1487)

T= 400

T= 450

T= 500

(112)

(220) (312) (400) (316) (424) (512)

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SEM

2.09 P

50.92 Se

23.36 In

23.63 Cu

% Atom

Eleme nt

EDX

T = 500 o C T = 400 o C

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Micrograph of rhobohedral Sb 2 Se 3 grown on glass at

(a)400 o C (b) 425 o C (c) 450 o C (d) 475 o C from

(b) [Sb(Se 2 P i Pr 2 ) 3 ] with an Ar flow rate of 180 sccm

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Structure of Talk

• Why now ? – Looking at some nanodimensional objects by way of introduction

• Synthetic approaches semiconductors • How nanoparticles grow and rods and tetrapods • Other materials a rogues gallery • What are some of the opportunities

– The Nanoco Technologies Ltd perspective

• Closing remarks

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illuminating the future

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§ World leading technology company – Produce fluorescent semiconductor nanoparticles "quantum dot“ and quantum dot

products

§ Patented technology solves problem of producing high quality quantum Dots on a large scale

§ Strategic partnerships with Application Developers – Tailored solutions to incorporate quantum dots into commercial applications

§ Quantum Dots are a “platform technology” with many applications in different industry sectors

§ Developed a range of quantum dots acceptable for commercial use

§ Nanotechnology Spin­out company from University of Manchester, UK

Company overview

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What are Quantum Dots? § Semiconductor material 100,000 x smaller than the width of a human hair § Size gives unique electronic and optical properties § Platform technology with many applications across different industry sectors

Why use them? § Replacement for luminescent dyes and inorganic materials § Better optical and electronic efficiencies

– More stable – More versatile

§ True platform technology which can be utilized in a range of applications across different industries

A True Platform Technology

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Nanoco Solves “Scale up” Problem The Problem The existing quantum dot ‘manufacturers’ processes are § Complex

– Hazardous and used banned substances § Costly § Low manufacturing yield

– No­one can produce a 1g batch

Without stable, cost effective supply of larger quantities of quality QD, developers are unable to bring there applications to market

The Solution Nanoco’s patented technology can § Using a ‘simple’ and controlled process § At a low cost § Now regularly produce r+d batches of 100g

Nanoco also has world leading patent technology to unlock the market

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Nanoco’s Technology

Dilute solution QD excited by UV light

High resolution electron microscope Image of single QD (5nm across)

Electron microscope image showing QD In very ordered patern

30 grams of 560nm QD. No other company in the world can produce this quantity. Market value in today’s bio applications greater than $10Million. Competitors can only produce 100 milligrams, 300X less material per batch. Nanoco will soon be producing 1 kilo batches

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O P O P

O

P

O

P

O P O P

O

P

O

P

The size of both core and shell of the particle can be changed

The capping agent can be changed

The organic groups on the capping agent can be functionalized for further chemical synthesis

O P O P

O

P

O

P

O P O P

O

P

O

P

O P O P

O

P

O

P

O P O P

O

P

O

P

The size of both core and shell of the particle can be changed

The capping agent can be changed

The organic groups on the capping agent can b further chemical synthesis

High­resolution transmission electron microscopy image showing the lattice plans of a nano­crystalline Quantum Dot, measuring 5nm

across (80,000 times smaller than the width of a human hair)

What are Quantum Dots?

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• Quantum dots absorb light over a wide wavelength range but have narrow emission spectra.

• The solutions, all contain the same semiconductor material (CdSe) but are different colours because unlike bulk CdSe, when below a certain size limit, we can control the electrical properties of the particles, by simply changing their size.

300 400 500 600 700 800

Wavelenght (nm)

Absorbance (a.u.)

PL UV

526

511

What are Quantum Dots?

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How Quantum Dots Work § UV light excites QD and kicks out electron creating electron and a vacant hole

§ As electron relaxes back into the hole a photon is emitted (visible light)

§ Size quantization effect – wavelength emitted depends on physical size of the quantum dot

e ­ e ­ e ­

UV light excites QD kicks out electron electron relaxes back into hole

UV light Visible light

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Quantum Dot Applications

• Biological screening

• Bio­Imaging

• Light emitting diodes

• Anti­counterfeiting

• Chemical\biological sensors

• Displays

• Solar cells

• Data storage

• Security application/ Bar coding

• Lighting

• Temperature sensors

• Single electron devices

• Quantum computing

10 – 30 years Current applications

1 – 5 years 6 – 10 years

QD Volum

e

Nanoco’s technology is allowing the QD market to grow rapidly

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QD Solar Cell Devices

Sun Light

§ Capture full spectrum of radiation § Quantum dots can be processed into inks § High efficiency of quantum dots § Tune the quantum dots to the radiation that you want to capture

Applications: Plastic solar cells, Gratzel cells, Solar roof tiles

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UV Light

Red

Green

Blue

Displays and QD­LED’s

Make full colour displays made by using quantum dots for each primary colour

§ Low energy consumption, § Same material for all colours, § High efficiency

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QD Biological Applications

Healthcare and Life Sciences Luminescent component in biological probes

2 nm 3 nm 4 nm

O P

O P

O P

O P

O P

O P

O P

O P

48 0 53 0 58 0 63 0 68 0

Count s, (a.u.)

Wavwlength (nm

)

O P O P

O P

O P

O P O P

O P

O P

O P O P

O P

O P

O P O P

O P

O P

0

0.05

0.1

0.15

0.2

0.25

0.3

0.35

0.4

400 450 500 550 600 650

Wavelengt h ( nm)

Absorbance (a.u.)

15nm

CdSe nanoparticle Encapsulated in a Polymer bead

Receptor Ligands Antibodies Antigens

Nucleic acid Proteins Enzymes

Narrow Emission Spectra Wide Absorption Spectra

Cell Virus DNA

Chemical agent

Cell

Cell Virus DNA

Chemical agent

Cell

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Confocal pictures of different size (A) 615nm, (B) 489nmCdSe/ZnS QDs labeling Lymphocyte Cells

Cell

Biocompatible polymer coating

Labelling cell

Affinity Ligand Quantum dot

Cell

Biocompatible polymer coating

Labelling cell

Affinity Ligand Quantum dot

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Quantum Dot Contain Beads

Quantum dot­containing polymer beads encoded beads

• High throughput screening • Anti­counterfeiting • Phosphors • Monitoring flow systems

Microscope image of a polymer bead containing three different sizes of quantum dots and the photoluminescent emission spectrum of 3 different bead encodings

Schematic of a polymer bead containing three different colours of quantum dots to

give an optical barcode

450 500 550 600 650 700 750 wavelength (nm)

450 500 550 600 650 700 750

wavelength (nm)

3125 5 5

256 4 4

27 3 3

4 2 2

N o of combinations

N o of intensities

N o of colours

400 450 500 550 600 650 700

Wavelength (nm)

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Identification of Beads by Fluorescence Profiles

4 types beads, 3 types QDs (532nm, 572nm & 628nm)

Chem. Commun, 2003, 2532 , J.Mater Chem., 2005,15,1238.

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Summary § World leading technology solution to existing problem – Scale up

§ Nanoco is de facto partner of choice to QD application developers

§ Large emerging market for QD based applications

§ World leading technology and management team

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www.nanocotechnologies.com

Nanoco Technologies Limited

48 Grafton Street

Manchester

M13 9XX

United Kingdom

Tel: +44 161 275 4606

[email protected]

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Structure of Talk

• Why now ? – Looking at some nanodimensional objects by way of introduction

• Synthetic approaches semiconductors • How nanoparticles grow and rods and tetrapods • Other materials a rogues gallery • What are some of the opportunities

– The Nanoco Technologies Ltd perspective

• Closing remarks

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