1
Anodic Formation of TiO 2 Dielectric Films B.Chou, D. McGervey, U. Landau, and G. Welsch Department of Materials and Engineering, Case Western Reserve University, Cleveland, U.S. The aim if this research is a capacitor with an energy density comparable to that of batteries. When titanium of high purity is anodized a TiO 2 film with high dielectric strength (0.75Volt/nm) and high charge density is obtained. The energy density is of the order of 100 to 200 Wh per kg of dielectric. Titanium oxide films were grown at voltages from 1 to over 400V. Film thickness was measured from interference colors in diffuse daylight, Figure 1, and on cross sections by electron microscopy. Experimental parameters were (a) purity of the titanium substrate, (b) surface preparation by chemical cleaning, etching and electro-polishing, (c) anodizing solutions and (d) solution modifiers. The parameters during anodization included temperature, voltage, current density, and anodizing time. A number of anodizing solutions were tried, including phosphoric acid and sodium silicate. Their effectiveness was studied by evaluating breakdown voltage, charge density and leakage current. The mechanisms responsible for leakage current are not fully understood. The experimental work on surface preparation, anodization parameters and evaluation of the dielectric properties and microstructure will be discussed. mixed with small amount organic solvent, like ethylene glycol can give oxide higher charge density and lower leakage current density. It is suggested the organic solvent can cover the defects of the titanium surface before the oxide grows, it may reduce the leakage current. Fig 1. Titanium anodized at different voltages in 1% H 3 PO 4 , at room temperature. Current limit at 8mA/cm 2 Fig2. Anodizing formation time verse voltage. High purity titanium was anodized at 18mA/cm 2 . Fig 3 Charge density and leakage current density of high purity titanium anodized to 30V at temperatures between 20 and 80 o C in H 3 PO 4 . 5V 10V 15V 20V 25V 30V 35V 40V 45V 50V 60V 70V 80V 90V 100V110V 120V 140V160V180V 200V 250V300V 350V400V Color chart @ diffuse daylight 0 10 20 30 40 50 60 70 80 90 20 40 60 80 100 120 140 160 charge density (uC/cm 2 ) Temperature ( o C) 100 200 300 400 500 600 700 leakage current density (uA/cm 2 ) 0 50 100 150 200 250 300 350 400 0 100 200 300 400 500 D C B A voltage (volt) Time (sec)

Color chart @ diffuse daylight The aim if this research is ... oxide films were grown at voltages from 1 to over 400V. ... effectiveness was studied by evaluating breakdown voltage,

  • Upload
    lyhanh

  • View
    215

  • Download
    2

Embed Size (px)

Citation preview

Anodic Formation of TiO2 Dielectric Films

B.Chou, D. McGervey, U. Landau, and G. Welsch

Department of Materials and Engineering, Case Western Reserve University, Cleveland, U.S.

The aim if this research is a capacitor with an energy density comparable to that of batteries. When titanium of high purity is anodized a TiO2 film with high dielectric strength (0.75Volt/nm) and high charge density is obtained. The energy density is of the order of 100 to 200 Wh per kg of dielectric. Titanium oxide films were grown at voltages from 1 to over 400V. Film thickness was measured from interference colors in diffuse daylight, Figure 1, and on cross sections by electron microscopy.

Experimental parameters were (a) purity of the titanium substrate, (b) surface preparation by chemical cleaning, etching and electro-polishing, (c) anodizing solutions and (d) solution modifiers. The parameters during anodization included temperature, voltage, current density, and anodizing time.

A number of anodizing solutions were tried,

including phosphoric acid and sodium silicate. Their effectiveness was studied by evaluating breakdown voltage, charge density and leakage current. The mechanisms responsible for leakage current are not fully understood. The experimental work on surface preparation, anodization parameters and evaluation of the dielectric properties and microstructure will be discussed. mixed with small amount organic solvent, like ethylene glycol can give oxide higher charge density and lower leakage current density. It is suggested the organic solvent can cover the defects of the titanium surface before the oxide grows, it may reduce the leakage current. Fig 1. Titanium anodized at different voltages in 1% H3PO4, at room temperature. Current limit at 8mA/cm2

0 50 100 150 200 250 300 350 400

0

100

200

300

400

500

D

C

B

A

volta

ge (

volt)

Time (sec)

Fig2. Anodizing formation time verse voltage. High purity titanium was anodized at 18mA/cm2.

Fig 3 Charge density and leakage current density of high purity titanium anodized to 30V at temperatures between 20 and 80oC in H3PO4.

5V 10V 15V 20V 25V 30V 35V 40V 45V 50V 60V 70V 80V 90V 100V110V 120V 140V160V180V 200V 250V300V 350V400V

Color chart @ diffuse daylight

0 10 20 30 40 50 60 70 80 90

20

40

60

80

100

120

140

160

ch

arg

e d

en

sit

y (

uC

/cm2 )

Temperature (oC)

100

200

300

400

500

600

700

� � � � � � � � � � � � � � � � � � � � � � � � � � � � � � � � � � � � � � � � � �

le

ak

ag

e c

urr

en

t d

en

sit

y (

uA

/cm

2 )