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SYNTHESIS OF SILVER ELECTRODEPOSITED ON TITANIUM SUBSTRATE AND ITS ANTIMICROBIAL ACTIVITY. *Nor Zulfa binti Tahir *2009713131 *AS225 Bsc Applied Chemis Yusairie bin Mohd

Synthesis of silver electrodeposited onto titanium mesh

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a project to alternatively replace toxic cyanide bath to synthesize silver by using nitrate solution.

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Page 1: Synthesis of silver electrodeposited onto titanium mesh

SYNTHESIS OF SILVER ELECTRODEPOSITED ON TITANIUM SUBSTRATE AND

ITS ANTIMICROBIAL ACTIVITY.

*Nor Zulfa binti Tahir *2009713131 *AS225 Bsc Applied Chemistry *Dr Yusairie bin Mohd

Page 2: Synthesis of silver electrodeposited onto titanium mesh

BACKGROUND OF STUDIES

SILVER PROPERTIES

•Silver is slightly harder than gold. •It is very ductile and malleable, exceeded in these properties by gold and palladium.•Silver is stable in pure air and water, although it tarnishes upon exposure to ozone, hydrogen sulfide, or air containing sulfur.•Has ANTIMICROBIAL PROPERTIES

Page 3: Synthesis of silver electrodeposited onto titanium mesh

BACKGROUND OF STUDIES

TITANIUM PROPERTIES

•strong, •low-density, •highly corrosion-resistant metallic element•Used as medical mesh and plates in reconstructive surgery•holds numerous advantages compared to all other types of non-corrosive, body-compatible metals

Page 4: Synthesis of silver electrodeposited onto titanium mesh

BACKGROUND OF STUDIES

Preparation of Silver DepositsDeposition process

Electroless and

chemical depositio

n

Electrodeposition

Advantages of electrodeposition technique• Process is faster.• Low costs• Capable of producing high quality

material

Advantages of Electrodeposition

substrateSilver deposits

Disadvantages of other technique such as chemical deposition.• it is more expensive because the

reducing agent costs more than an equivalent amount of in the bulk of the solution

• it is less intensive because the metal deposition rate is limited by metal ion reduction

Page 5: Synthesis of silver electrodeposited onto titanium mesh

PROBLEM STATEMENTS

Electrodeposition condition and solution influence the formation of silver deposition on substrate.

The existing solution use toxic substances i.e AgCN thus encouraging the studies of environmentally precursor of silver solution required.

Titanium mesh implant cause bioaccumulation in medical surgery.

Page 6: Synthesis of silver electrodeposited onto titanium mesh

To replace toxic AgCN, the disadvantages and adverse effects caused by current method practise by industries to obtain silver deposits.

• To use material that can inhibit and prevent bioaccumulation of titanium implant for medical purposes.

SIGNIFICANCES OF STUDIES

Page 7: Synthesis of silver electrodeposited onto titanium mesh

OBJECTIVES OF STUDIES

1. To extract silver from silver nitrate and investigate the influence of potential applied during deposition of silver onto titanium mesh by electrodeposition technique.

2. To characterize the prepared silver coating with varies voltage by FESEM, and EDAX.

3. To study antimicrobial activity of titanium mesh coated with silver against Gram-negative bacteria Escherichia coli, and Gram-positive bacteria Staphylococcus aureus

Page 8: Synthesis of silver electrodeposited onto titanium mesh

LITERATURE REVIEW

YEAR AUTHOR JOURNAL FINDING

2005 G.M. ZarkadasA. StergioG. Papanastasio

Electrochimia Acta The production of smooth, compact, and coherent deposits is of greatest importance in the electrodeposition process and is much desired in the electrolytic refining of metals.

2006 Elvira GomezJose Garcia- TorresElisa Valles

Electroanalytical Chemistry

Silver were produced by electrodeposition process using cyanide baths because silver electrodeposits prepared from a simple salt do not lead to coherent deposits. Despite the high quality of the deposits obtained from the alkaline cyanide solutions, these plating baths are strongly toxic. Thus developing alternative baths, which could replace cyanide ones, is of important environmental and economical interest.

Page 9: Synthesis of silver electrodeposited onto titanium mesh

LITERATURE REVIEWYEAR AUTHOR JOURNAL FINDING

2010 Andrew BasileAnand I. BhattAnthony P. O’MullaneSuresh K. Bhargava

Electrochimia Acta

Several approaches have been taken to produce silver films including physical vapour deposition, chemical vapour deposition, chemical vapour deposition and sputtering, all of which have disadvantages including cost and slow deposition rates. Other approaches include electro and electroless plating, however this usually requires the use of toxic cyanide based plating baths that often contain additional organic additives which are both harmful and difficult to dispose off after the reaction completes.Therefore the development of alternative solvents that minimise the use of pollutant is of importance given the industrial and academic focus on green processes which aim to reduce the environmental impact of current industrial methods.

2004 Claudia Ramirez Elsa M. ArceMario Romero- RomoManuel Palomar- Pardave

Solid State Ionics

Considering that silver is the metal which has been largely used for coatings, exhibiting optimal physicochemical properties and fairly good corrosion resitance.

Page 10: Synthesis of silver electrodeposited onto titanium mesh

LITERATURE REVIEWYEAR AUTHOR JOURNAL FINDING

2007 M. SaitouT. OtaA. NakanoS.M Asadul

Hossain

Surface and Coating Technology

Cyanide free compounds such as silver nitrate, silver sulfate, silver ionide and silver thiosulfate have not been reported to produce silver thin films shiny appearances. In most experiments, the surface appearances are white, yellow or white bright tints that are not accepted for decorative and technological application.

In spite of cyanide toxisity, silver electrodeposition has been carried out from cyanide electrolytes because the cyanide processes are easy to chemically control a broad range of silver cyanide concentrations.

2008 Woo Kyung Jung Hye Cheong KooKi Woo KimSook ShinSo Hyun KimYong Ho Park

Applied and Environmental Microbiology

Since ancient times, the silver ion has been known to be effective against a broad range of microorganisms. Today, silver ions are used to control bacterial growth in a variety of medical applications, including dental work, catheters, and the healing of burn wounds.

Page 11: Synthesis of silver electrodeposited onto titanium mesh

LITERATURE REVIEWYEAR AUTHOR BOOK/JOURNAL FINDING

2007 Felix Bronner Mary C.F. Antonios G.M

Engineering of Functional Skeletal Tissues.

The advantages of using the mesh material for tissue engineering purposes are its flexibility, strength, porosity, and interconnectivity. Strength allows the implant to bear the mechanical load. Flexibility eliminates focal stresses by distributing the stresses between implant and tissue over a larger area. Finally porosity and interconnectivity allow tissue in growth and stabilisation of the implant.

2010 Liao JuanZhu ZhiminMo AnchunLi LeiZhang Jingchao

International journal nanomedicine

Implanted devices such as artificial hip or knee joints, and dental implants are suitable substrates for microbial colonization and biofilm formation, which is a recurrent complication in implant surgery.

Page 12: Synthesis of silver electrodeposited onto titanium mesh

METHODOLOGY

SYNTHESIS OF

SILVER ELECTRODEPOSITED ON

TITANIUM

SUBSTRATE AND

ITS ANTIMICROBIAL

ACTIVITY.

Antimicrobial

Testing

Preparation of silver

particles

Electrodeposition:CV

Electrodeposition:Chronoamperometric

Characterisation.

1

2

3

FESEM

EDAX

ADHESION

GRAM+VE

GRAM -VE

Page 13: Synthesis of silver electrodeposited onto titanium mesh

METHODOLOGY

Material and Chemicals Instruments

1. Silver nitrate,AgNO3 solutions 2. Nitric acids, HNO3 pH adjustment3. Silver nitrate (AgNO3 )4. Mueller Hinton Agar5. Mueller Hinton Broth 6. Escherichi coli Broth culture7. Staphylococcus aureus bacteria culture.

1. Field Emission Scanning Electron Microscopy (FESEM)

2. Autolab pentiostat3. EDAX (energy dispersive

Xray)4. Tape

Page 14: Synthesis of silver electrodeposited onto titanium mesh

METHODOLOGYSurface Preparation of Substrate Titanium Mesh

To obtain desired deposits optimumly,

Page 15: Synthesis of silver electrodeposited onto titanium mesh

Cyclic Voltammetry (determination of deposition potential)

Chronoamperometry ( to deposit the silver films on Ti mesh)

Electrodeposition of Silver Onto Titanium mesh

METHODOLOGY

Page 16: Synthesis of silver electrodeposited onto titanium mesh

METHODOLOGYCharacterization of Silver Deposits

EDAX

Field Emission Scanning Electron Microscopy (FESEM) – surface morphology

Adhesion test

Page 17: Synthesis of silver electrodeposited onto titanium mesh

METHODOLOGYAntimicrobial Testing

Page 18: Synthesis of silver electrodeposited onto titanium mesh

METHODOLOGYAntimicrobial Testing

Page 19: Synthesis of silver electrodeposited onto titanium mesh

METHODOLOGYAntimicrobial Testing

Page 20: Synthesis of silver electrodeposited onto titanium mesh

RESULTS AND DISCUSSIONCyclic Voltammetric

Ag+ (aqueous) + e Ag (solid)

Low potential chosen: -0.5VHigh potential chosen: -1.5V

faraday process involves the transfer of electrons across the electrode-electrolyte interface

Starts here

Page 21: Synthesis of silver electrodeposited onto titanium mesh

RESULTS AND DISCUSSIONChronoamperometric

• Ag/Ti AT -0.5V(LOW VOLTAGE)

• bright shining silver +very little

precipitation of white pale powder

• Ag/Ti AT -1.5V (HIGH VOLTAGE)

• bright shining silver + abundant precipitation of white pale powder.

Page 22: Synthesis of silver electrodeposited onto titanium mesh

RESULTS AND DISCUSSIONChronoamperometric Factor

influenced

deposition.Quantity

SAMPLE NO.

CONDITION AVERAGE(g)MASS OF

DEPOSITION

ADHESION

1 Cronoamperometry at -0.5V with solution 0.20M silver nitrate

1.1135Very weak adherence and exfoliates from substrates.

2 Titanium mesh undergo cronoamperometry at -1.5V with solution 0.20M silver nitrate

0.01585Very weak adherence and exfoliates from substrates.

Page 23: Synthesis of silver electrodeposited onto titanium mesh

RESULTS AND DISCUSSION

Characterisation: FESEMMagnification 300X Magnification 500X

Blank Titanium mesh

Ag/Ti mesh: -0.5V

Ag/Ti mesh: -1.5V

Page 24: Synthesis of silver electrodeposited onto titanium mesh

RESULTS AND DISCUSSION

Characterisation: EDAX

Blank Titanium mesh Ag/Ti mesh: -0.5V Ag/Ti mesh: -1.5V

Page 25: Synthesis of silver electrodeposited onto titanium mesh

RESULTS AND DISCUSSIONANTIMICROBIAL TESTING

Gram negative bacteria

Titanium mesh only.

No inhibiton zone

Ag/Ti at -0.5V.

Inhibition zone 0.95cm

Average 1.0cm

Ag/Ti at -1.5v

Inhibition zone

Average 0.75cm

Penicillin antibioticInhibiton

zone 0.65cmAverage 0.65cm

Sterile Distilled Water

No inhibition zone

Escherichia coli

Page 26: Synthesis of silver electrodeposited onto titanium mesh

RESULTS AND DISCUSSIONANTIMICROBIAL TESTING

Gram negative bacteria

Titanium mesh only.

No inhition

zone

Ag-Ti at -0.5V.

Inhibition zone

1.05cmAverage 1.0cm

Ag-Ti at -1.5V

Inhibition zone

0.85cmAverage 0.75cm

Penicillin antibioticInhibition

zone 0.65cmAverage0.65cm

Sterile Distilled Water

No inhibition

zone

Escherichia coliDUPLICATED

Page 27: Synthesis of silver electrodeposited onto titanium mesh

RESULTS AND DISCUSSIONANTIMICROBIAL TESTING

Gram positive bacteria

Titanium mesh only.

No inhition

zone

Ag-Ti at -0.5V.

Inhibition zone

0.7cmAverage 0.8cm

Ag-Ti at -1.5V

Inhibition zone

0.7cmAverage 0.65cm

Penicillin antibioticInhibition

zone 0.7cm

Average0.7cm

Sterile Distilled Water

No inhibition

zone

Staphlococcus aureus

Page 28: Synthesis of silver electrodeposited onto titanium mesh

RESULTS AND DISCUSSIONANTIMICROBIAL TESTING

Titanium mesh only.

No inhition

zone

Ag-Ti at -0.5V.

Inhibition zone

0.9cmAverage 0.8cm

Ag-Ti at -1.5V

Inhibition zone

0.6cmAverage 0.65cm

Penicillin antibioticInhibition

zone 0.70cmAverage0.70cm

Sterile Distilled Water

No inhibition

zone

Staphlococcus aureusDUPLICATED

Page 29: Synthesis of silver electrodeposited onto titanium mesh

RESULTS AND DISCUSSIONANTIMICROBIAL TESTING

Page 30: Synthesis of silver electrodeposited onto titanium mesh

CONCLUSION AND RECOMMENDATIONSCO

NCL

USI

ON

Page 31: Synthesis of silver electrodeposited onto titanium mesh

CONCLUSION AND RECOMMENDATIONS

Study details the mechanism involved in the formation of silver on titanium subtrates by electrodeposition technique.

• The silver particles on titanium mesh can be further characterized in many other terms such as temperature and mechanical (stress test etc).

In addition that to improve analysis of elements obtained, EDAX can be analyzed at several different spot more on the surface giving more precise analysis that reducing the deviations between the analyzed sample.

• Adhesion between Ag-Ti can be further improved by studying the factor that influence strength of the adherence between Ag-Ti. Some of the factors are presence of additives in the solution bath, stability of the electrolyte etc.

And lastly, the application of Ag-Ti in its antimicrobial activity can further be investigated against various types of bacteria and microorganisms.

REC

OM

MEN

DAT

ION

S

Page 32: Synthesis of silver electrodeposited onto titanium mesh

REFERENCESClaudia Ramirez, et. al. (2004). The effect of temperature on the kinetics and mechanism

of silver electrodeposition. Journal of Solid State Kinetic; 81- 85

M. Saitou, et. al. (2007). Electrodeposition of silver films with shiny appearances from an electrolyte comprising silver ferrocyanide- thiocyanate and antimony potassium tartrate. Journal of Surface and Coating Technology 201 (2007) 6947-6952

G. M. Zarkadas, et. al. (2005). Influence of citric acid on the silver electrodeposition from aqueous AgNO3. Journal of Electrochimica Acta; 5022-5031.

Elvira Gomez, et al. (2006). Study and preparation of silver electrodeposits at negative potentials. Journal of Electroanalytical Chemistry; 89-95.

Andrew Basile, et al. (2010). Investigation of silver electrodeposition from ionic liquids; Influence of atmospheric water uptake on the silver electrodeposition mechanism and film morphology