Brazilian Center for Physics Research

Dr. Elvis O. López M.

Wave resonance effect in a confined plasma by magnetron sputtering for increasing the plasma temperature and the production of

high quality biocompatible coatings of hydroxyapatite.

Laboratory of Surface and Nanostructures

Laboratory of Biomaterials Plasma Physics Laboratory

Work Team

Dr. Alexandre Mello

Dr. Alexandre Rossi

Dr. Ricardo Galvão

Carlo Mangano et al. (2006)

HA structures for medical application

Clinical phases of the 2-stepmaxillary sinus augmentationwith engineered porous ofhydroxyapatite applications.Hydroxyapatite

granules and its application

Hydroxyapatite (HA) application in bone regeneration

Orthopedic application

Coating in dental implants

Orthopedic implantsand medical devices

HA for future applications in orthopedics

Radio frequency magnetron sputtering (RFMS)

Sputteringdeposition process

Sputtering System

Structural Characteristics

• Lower deposition rate.• Control of thickness.• Low roughness.• Good adhesion (substrate – coating).

Terra, J.; Jiang, M.; Ellis, D.E. Philos Mag. A 2002, 82, 2357-2377.

Ca(I)4Ca(II)6[PO(I)O(II)2O(III)]6(OH)2HA structure

HA deposited by RFMS

Right angle magnetron sputtering (RAMS)

a) Diagram of the RAMS system and (b) comparison of simulatedB produced by the magnetrons and a picture of the confinedplasma.

RAMS system

XRD pattern of HA target

FTIR spectra of HA target

XPS spectra of the HA target sintered at 1150 °Cshown the a) full scan spectra and high resolutionspectra for: b) Ca2p, c) O1s and d) P2p

HA target characterization

GIXRD (λ = 0.13775 nm) patterns at θ =0.5° of HA films growth at RT, depositedat 3 nm/min in thickness of a) 90 nm, b)135 nm, c) 225 nm and d) 540 nm.

HA films characterization

TEM and HRTEM of HA film of 540 nm

Morphology of sputtered films.

Thornton 1986

Zone T (0.3 < Ts/Tm < 0.5)

TEM image of FHA film (540 nmof thick) showing: a) the sampleprepared by FIB and b) thestructure of the FHA film atnanoscale (TEM dark field image).

FHA films characterization

HRTEM image showingthe interface between FHAfilm and Si(100) substratein a) low magnification, b)high magnification of thereal image and its FFT onSi(100) substrate and FHAfilm, and c) the FFTinverse of the real image.

FHA films characterization

XRD pattern of a Ca deficient HA target

GIXRD patterns (over) and FTIRspectra (under) of the film depositedat 180 min at a) RT and b) afterannealing at 800 °C for 2 h.

Studies of RAMS plasma

14

2/1

0~

∈=Λ

se

eDes en

Tλ

( )BseeffisD unT

E2

≥Γ= ε

2/1

=

i

effB M

eTu

Discharge Processes

How Characterize the Plasma?

Langmuir Probe Measure electrons and ions

Measure ions

Measure the magnetic field

Measure ions

Faraday Probe

Hall Probe

Optical Emission Spectroscopy (OES)

Langmuir probe in Ar+Ag plasma sputtering

Typical circuit of Langmuir probe

Data obtained from Langmuir probe

Electron energy distribution function (EEDF)

Langmuir Probe Diagnostic

Grid Insolator

Collector

Data obtained from Faraday probe

Ion energy distribution function (IEDF)

Faraday Probe Diagnostic

Ionization Energies (eV):

OI = 13.61, CaI = 6.11,OII = 35.12, CaII = 11.87,

PI = 10.48, ArI = 15.76PII = 19.76, ArII = 27.63

HI = 13.6

Emission spectrum obtained by OES of the RAMS plasma bulk

Optical Emission Spectroscopy (OES)

Scheme of Hall sensor

a) Diagram of RAMS configuration; b) comparison of the absolute values ofB obtained from the Hall probe measurements and COMSOL simulation,along the Z direction; values of B simulated at Z = 32 mm along the c) Xʹ andd) Yʹ directions

Hall Probe

2/1

0

2

∈

=e

epe m

neω

2/1

0

2)(

∈

=i

iipi M

neZω

ee m

eB=Ω

i

ii M

eBZ=Ω

222peeUH ωω +Ω=

2/1|| eiLH ΩΩ≈ω

αωω

=Ω

=e

pz c

kk 22

222zkkk += ⊥

( )tmzki zeHE ωθ−+≈,

ωLH ωΩe

Plasma frequencies

Hybrid frequencies

Cyclotron frequencies

Helicon wave

0Bk ⊥

0// Bk

Frequencies in Magnetized Plasmas

Radial profiles of a) ne and b) Teffand Ti in the RAMS plasma

LH frequency calculated for differention species in the RAMS plasma

Radial variations of α, which appearsin the HW dispersion relation, and ne

Resonance effect in the RAMS plasma

Total energy delivered to thegrowing film by all incident ionsalong the plasma profile (Z).

GIXRD spectra at θ = 0.5° and Ca/P ratio determined by XPS measurements of HAfilms at 180 min of deposition, for: a) Z1 = 22 mm, b) Z2 = 26 mm, c) Z3 = 28 mm, d)Z4 = 30 mm, e) Z5 = 32 mm and f) Z6 = 36 mm.

Delivered Energy to HA Films Formation

23

a) B and b) E along the space (ȓ), generated by RAMS magnetrons, showing the regions oflower hybrid resonance (LHR) and helicon wave formation (HW) in the limit of magneticcusp. Down, magnification of region of the B and E showing the effect of plasma trappedinside magnetic cusp and the effect of plasma drift.

RAMS Plasma Model

Diagram of growth model of hydroxyapatite crystalline films by RAMS plasma

Growth Model of HA Films

GRACIAS SIMPOSIO PERUANO DE FÍSICA

2016

CBPF

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