Fundamentals of Nanotechnology
Cornelia Cretiu Vasiliu
12-01-2007
1
Motivation
Methods of synthesis
Characterization of structure
Morphology and particle size distribution
Properties & Applications
2
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Bone: 2nd most implanted tissue after blood
Protein matrix containing type 1 collagen and
minerals
Calcium as:
(Ca 2+)10-x(H3O+)2x*(PO4)6(OH-)2
Synthetic vs. homo-, allo-, xeno-geneic implants
Properties: biocompatibility, biodegradability,
mechanical integrity, vascularization
inductivity, osteoconductivity, and
osteoinductivity
http://www.uabhealth.org/16313
3
HA
Wet methods5
Solid-state reactions6
Sol-gel7
Ellectrocrystallization8
Spray pyrolysis9
Emulsion processing10
Hydrothermal treatment11
nHA
Chemical precipitation1
Hydrothermal treatment12
Microwave synthesis2
To be considered:
stoichiometry, pH, rate of addition, ionic strength
4
nHA Methods of synthesis
Co precipitation 1)
Ca(OH)2 + H3 PO4
nHA
Aqueous, pH 8, 38oC
•
•
Microwave synthesis 2)
10 Ca(OH)2+6 (NH4)2HPO4
850W, 20 min.
Ca10(PO4)6(OH)2+6H2O+12NH4OH
13)Aq.
Sol. NaNO3, Ca(NO3)2·4H2O and KH2PO4
precursor
600W, 5 min.
stirred in H2O ( room temperature , 1 h) nHA particles.
5
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XRD(1
Powder XRD of the HA precipitate: (a) as-prepared, (b) calcined at
700 °C, (c) calcined at 800 °C, (d) calcined at 900 °C and (e) calcined at
1200 °C. [specific peaks :(H) HAP; (b) β-TCP; (a) α-TCP].( 1
6
IR(1 spectra of the nHA
precipitates:
 (a) as-dried,
 (b) calcined at
700 °C,
 (c) calcined at
800 °C,
 (d) calcined at 900 °C
and
 (e) calcined at
1200 °C.
7
SEM micrograph of the as-prepared nHA(1
TEM micrograph of as-synthesized nano
HA crystals(14
8
 DLS: Histogram
representation of the
mean diameters of asprepared nHA
suspended in aqueous
solution. (1
9
Coatings
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(2
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Cell morphology after
being cultured for 15
min on the different
nHA coated(G2) and
uncoated(G1H)
titanium surfaces.
Surface roughness
decreased(2
Fibers, tubes
nHA doped PLGA
composite (30% nHA)
hollow fiber membrane
fabricated using wet phase
inversion technique (13
(13
10
Bone filler(4
(A) Preoperative axial CT
(B) Lateral preoperative view
(C) After reduction, the remaining
defect was filled with nHA paste.
(D) Postoperative radiograph
(E) 6 weeks after surgery . The patient
progressed to full weight bearing at
this point in time.
(F) 12 months postoperatively, only a
marginal loss of correction could be
measured.
11
CT scan
Computer file
Choose customized design
Print, sinter implant
Seed cells, growth factors
Implant
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http://www.sciencedirect.com/science/article/B6THV-4JVK5671/2/501b2d84c7d81d8e9dc5771941065db1 Phase
Xiaolong Zhu et al 2006 Nanotechnology 17 2711-2721
http://www.sciencedirect.com/science/article/B6TWH-4KY88TT3/2/2a01537a8d0b528852bb67f079d7e91a Rapid densification
F. Huber, J. Hillmeier, N. McArthur, H. Kock and P. J. Meeder, The Use of Nanocrystalline
Hydroxyapatite for the Reconstruction of Calcaneal Fractures: Preliminary Results, J. of Foot
and Ankle Surgery Vol. 45/ 5, 2006, pp. 322-328.
C. Liu, Y. Huang, W. Shen and J. Cui, Biomaterials 22 (2001), pp. 301–306.
X. Yang and Z. Wang, J. Mater. Chem. 8 (1998), pp. 2233–2237
W. Feng, L. Mu-sen, L. Yu-peng and Q. Yong-xin, Mater. Lett. 59 (2005), pp. 916–919
S.K. Yen and C.M. Lin, Mater. Chem. Phys. 77 (2003), pp. 70–76.
K. Itatani, T. Nishioka, S. Seike, F.S. Howell, A. Kishioka and M. Kinoshita, J. Am. Ceram. Soc.
77 (1994), pp. 801–805
C.-W. Chen, R.E. Riman, K.S. TenHuisen and K. Brown, J. Cryst. Growth 270 (2004), pp. 615–
623
G.Z. Hui, Z. Qingshan and H.X. Zhao, Mater. Res. Bull. 40 (2005) (8), pp. 1326–1334.
W.L. Suchanek, K. Byrappa, P. Shuk, R.E. Riman, V.F. Janas and K.S. TenHuisen, J. Solid State
Chem. 177 (2004), pp. 793–799
N. Zhang et al. / Materials Science and Engineering C 27 (2007) 599–606
S. Ramesh et al. / Ceramics International 33 (2007) 1363–1367
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HA:βTCP
60:40
1270oC/4h
HA:βTCP
60:40
1100oC/4h
14