Summary - Experiment Procedures and Principle

Chapter 2 Experiment Procedures and Principle

3.4 Summary

We have demonstrated experimentally the effects of low-temperature treatments on the dielectric characteristics of HfO2 film. The preliminary improvement in HfO2

dielectrics is obtained by H2O vapor immersion at 150 °C, due to the deactivation of defects inside low-temperature deposited HfO2 films and replacing these defects by the formation of Hf-O-Hf bonds. A further study also showed that the efficiency of passivating defects can be maximized via the SCCO2 treatment which mixed with H2O and additive alcohol. Basing on the gas-like and high-pressure properties, the supercritical CO2 fluids can affinity with H2O molecules and infiltrate into HfO2 films to effectively deactivate these defects (or dangling bonds). After SCCO2 treatment, the amount of oxygen and the intensity of Hf-O-Hf bonds obviously rise, and the superior resistance to leakage current is gained as a result of the conduction mechanism transform into Schottky emission. The properties of SCCO2-treated HfO2

film, such as larger dielectric constant, lower density of interface states, higher breakdown voltage of HfO2 film and excellent reliability under high electric field are presented in addition. These results indicate that the low-temperature SCCO2 fluids technology is greatly beneficial to enhance the dielectric properties of low-temperature deposited HfO2 films by reducing defects, and performs better electrical reliability. We have successful fabrication OTFTs with low-temperature treatments on the dielectric characteristics of HfO2 insulator after. The characteristic of mobility, threshold voltage and on/off current ratio have better OTFT of PECVD SiO2 insulator. The DC bias and current stress characteristics decay is nearly.

Chapter 4 Conclusion

In this study, we successfully employ the supercritical CO2 fluids technology to carry H2O molecule into sputter-deposited HfO2 film for passivating the defects at low temperature and successfully obtained characteristics of OTFTs .The mobility of 0.05cm²/Vs, threshold voltage of -0.1V, on/off current ratio of 2x10⁵ and sub-threshold swing of 2.2 V/Dec. .

With this proposed treatment, the HfO2 films present the more completed higher oxygen content and Hf-O-Hf binding. In the investigation on the electrical characteristics of treated-HfO2 films, the excellent performances of dielectric property are achieved, including the ultra-low leakage current, the ideal capacitance-voltage curve, the higher dielectric constant, the better resistance to breakdown and the more stable reliability under high electric field. From these experimental results, the efficiency of applying supercritical CO2 fluids to deactivate defects is proved.

Therefore, this technology agrees to fabricate the high quality dielectric films at low-temperature.

This proposed technology is also used to fabrication organic thin film transistors (OTFTs) at 150 °C. After supercritical CO2 treatment, we successfully obtained characteristics of OTFTs are better than SiO2 insulator of OTFTs ,including the better sub-threshold swing, lower off-current, higher on/off current ratio and higher mobility. The DC bias and current stress characteristics were nearly SiO2 insulator of OTFTs. Such that the supercritical CO2 treatment provide a novel method to fabricated OTFTs at low-temperature.

Fig. 1-1 Phase diagram for CO

Fig. 1-2 Density-pressure-temperature surface for pure CO

Table 1-1 Critical temperature and pressure for some common fluids.

Table 1-2 Comparison of physical properties of CO

150℃

High-pressure Syringe Pump B (Co-solvent)

Co-solvent Syringe CO₂Syringe

Reaction

Fig. 2-1 The supercritical fluid system.

High-pressure Syringe Pump B (Co-solvent)

Co-solvent Syringe CO₂Syringe

Reaction

( b ) H

₂

O-Vapor Treatment Process

150℃

High-pressure Syringe Pump B (Co-solvent)

Co-solvent Syringe CO₂Syringe

Reaction

Co-solvent Syringe CO₂Syringe

Reaction

( b ) H

₂

O-Vapor Treatment Process

150℃

( a ) SCCO

₂

Treatment Process

High-pressure Syringe Pump B (Co-solvent)

Co-solvent Syringe CO₂Syringe

Reaction

Co-solvent Syringe CO₂Syringe

Reaction

C3H7OH& H2O SCCO2SCCO2SCCO2

C3H7OH& H2O

( a ) SCCO

₂

Treatment Process

Si Wafer

Deposited by DC magnetron sputtering at room temperature under Ar/O2 ambient

HfO₂

1. Baking-only treatment :

only baked on a hot plate at 150 °C for 2 hrs.

2. H2O vapor treatment :

immersed into a pure H2O vapor ambience at 150 °C for 2 hrs.

3. 3000psi-SCCO2 treatment :

was placed in the supercritical fluid system at 150°C for 2 hrs.

1.Fourier transformation infrared spectroscopy (FTIR).

2.Thermal desorption spectroscopy (TDS).

3.X-ray Photoelectron Spectroscopy (XPS).

4.Transmission Electron Microscopy (TEM).

Si Wafer HfO2

Al metal, deposited by thermally evaporating

1.Current density-electric field (J-E) characteristics.

2.Capacitor-voltage (C-V) characteristics.

3.Breakdown voltage 4.Gate bias stress

Defect passivation process:

Fig. 2-2 The experiment processes of thin HfO film with various treatments.

Si Wafer

Deposited by E-beam evaporation at room temperature

HfO₂

Defect passivation process:

1. Baking-only treatment : only baked on a hot plate at 150 °C for 2 hrs.

2. H2O vapor treatment : immersed into a pure H2O vapor ambience at 150

°C for 2 hrs.

3. 3000psi-SCCO2 treatment : was placed in the supercritical fluid system at 150°C for 2 hrs.

1. Current density-electric field (J-E) characteristics.

2. Capacitor-voltage (C-V) characteristics.

3. Secondary Ions Mass Spectrometer (SIMS) Analysis.

Si Wafer HfO₂

Al metal, deposited by thermally evaporating

1. Current-Voltage characterization.

2. DC bias stress analysis 3. Current stress analysis

Au metal, deposited by thermally evaporating Pentacene, deposited by thermally evaporating

Fig. 2-3 The experiment processes of OTFTs with HfO

film of various

treatments .

Fig. 2-4 The energy band diagram of pentacene. The optical energy gap and adiabatic energy gap are determined.

Fig. 2-5 Energy band diagrams (a) for a p-channel (pentacene) and (b)

for a n-channel (NTCDA) OTFTs. The left side shows the

devices at zero gate bias, while in the centre and in the right

parts the accumulation and depletion mode operation regimes

Electric field (MV/cm)

0.0 0.5 1.0 1.5 2.0 2.5 3.0

J (Amp./cm2 )

10^-9 10^-8 10^-7 10^-6 10^-5 10^-4 10^-3 10^-2 10^-1

10⁰ Baking-only treatment H₂O vapor treatment 3000psi-SCCO₂ treatment

Fig. 3-1 The leakage current densities of HfO

films after different treatments (The negative bias is applied on gate electrode)

Al HfO

₂

Silicon

e

-“+” bias common

Fowler-Nordheim tunneling

Schottky-Richardson emission

Frenkel-Poole emission

Al HfO

₂

Silicon

e

-“+” bias common

Fowler-Nordheim tunneling

Schottky-Richardson emission

Frenkel-Poole emission

Fig. 3-2 Conduction mechanism for Al/HfO

/Si MIS structure

E^1/2(MV/cm)^1/2

E_applied > 0.7 MV/cm.

(a)

the baking-only treated HfO

₂

film, and a schematic energy

band diagram accounting for trap-assisted tunneling shown in

the inset. (b) Leakage current density versus the square root of

electric field (E

^1/2

) plot for the 3000 psi-SCCO

₂

treated HfO

₂

film. The inset shows the energy band diagram of

Schottky-type conduction mechanism.

Electric field (MV/cm) H₂O vapor treatment 3000 psi-SCCO₂ treatment

Al H₂O vapor treatment 3000 psi-SCCO₂ treatment

Fig. 3-4 The leakage current densities of HfO

films after different treatments (The positive bias is applied on gate electrode).

1 MHz

3000 psi-SCCO₂, reverse

ΔV 3000 psi-SCCO₂, forw ard

Reverse

Forward

Fig. 3-5 The capacitance-voltage characteristics of HfO

films after

different treatment, measuring at 1M Hz with gate bias swing

from negative voltage to positive voltage (forward) and from

positive voltage to negative voltage (reverse)

attract H₂O part

attract CO₂part

HO – C – C – C –H

Fig. 3-6 The mechanism of extracting of fixed charge with SCCO

₂

fluids.

Removing negative charge

-by SCCO₂fluids

Removing positive charge

+

by SCCO₂fluids

+

-Dipole, which could attract negative/positive charge Oxygen molecule

Hydrogen molecule

+

-Dipole, which could attract negative/positive charge

Gate Si

Fig. 3-7 The equivalent capacitance models of MOS structure (a) without C

_it

, (b) with C

_it

.

1M & 100K Hz (Forward)

V

_GS

(Volt.)

3000 psi-SCCO₂, 100K Hz

Fig. 3-8 The capacitance-voltage characteristics of HfO

₂

films after

different treatment, measuring at 1M Hz and 100k Hz with

forward gate bias swing.

(a)

(b)

Fig. 3-9 The breakdown characteristic curves of HfO

films after

various treatments (a) at positive and (b) at negative gate bias

region, individually.

Stress voltage V_GS = 5 Volt. ； E = 5 MV/cm

Fig. 3-10 The variation of leakage current of different-treated HfO

₂

films as a function of stress time at a high electric field = 5 MV/cm.

Wavenumber (cm^-1)

400 600 800 1000 1200 1400 1600 1800 2000

Intensity (arb. units)

400 600 800 1000 1200 1400 1600 1800 2000

Intensity (arb. units)

Fig. 3-11

The FTIR spectra of HfO

₂

films after various post-treatments,

including Baking-only, H

₂

O vapor and 3000psi-SCCO

₂

treatment.

Hf dangling bond Driving into HfO₂film by SCCO₂fluids

CO₂molecule

Fig. 3-12 The transporting mechanism for SCCO

₂

fluids taking H

₂

O molecule into HfO

₂

film.

Driving into HfO₂film by SCCO₂fluids

CO₂molecule

(a)

m/e = 32 (O

₂

)

Temperature (⁰C)

200 400 600 800

Intensity (arb. units)

Baking-only H2O vapor 3000psi-SCCO2

m/e = 44 (CO

₂

)

Temperature (⁰C)

(b)

Fig. 3-13 The thermal desorption spectroscopy (TDS) measurement, (a) m/e (mass-to-charge ratio) = 32 peak that is attributed to O

₂

, (b) m/e = 18 peak that is attributed to CO

₂

.

Baking-only H2O vapor 3000psi-SCCO2

Intensity (arb. units)

200 400 600 800

H₂O vapor treatment

3000 psi-SCCO₂ treatment

Bonding energy (eV)

H₂O vapor treatment

Bonding energy (eV) H₂O vapor treatment

Bonding energy (eV)

3000 psi-SCCO₂ treatment

Bonding energy (eV) 3000 psi-SCCO₂ treatment

Bonding energy (eV)

Fig. 3-14 The X-ray photoemission spectra of HfO

₂

films O 1s after

various post-treatments, including (a) Baking-only, (b) H

₂

O

vapor and (c) 3000psi-SCCO

₂

treatment.

Fig. 3-15 The TEM images show the MIS (Al/HfO

₂

/Si-Substrate) structure after various post-treatments: (a) Baking-only treatment (b) H

₂

O vapor treatment and (c) 3000psi-SCCO

₂

treatment.

( a ) Baking-only 5 nm

( b ) H

₂

O vapor

( c ) 3000 psi-SCCO

₂

Si

HfO ₂ , ~70 Å

Si

HfO ₂ , ~66 Å

Si

HfO ₂ , ~70 Å

SiO _X , < 5 Å

SiO _X , ~ 5 Å 5 nm

5 nm 5 nm ( a ) Baking-only 5 nm

( b ) H

₂

O vapor

( c ) 3000 psi-SCCO

₂

Si

HfO ₂ , ~70 Å

SiO _X , < 5 Å

Si

HfO ₂ , ~66 Å

Si

HfO ₂ , ~70 Å

SiO _X , < 5 Å

5 nm 5 nm

SiO _X , ~ 5 Å

5 nm

Electric field (MV/cm) H₂O vapor treatment 3000-psi SCCO₂ treatment

Fig. 3-16 The leakage current densities of HfO

films after different treatments

Fig. 3-17 The capacitance-voltage characteristics of HfO

films after different treatment, measuring at 1M Hz with gate bias swing from negative voltage to positive voltage (forward) and from positive voltage to negative voltage (reverse)

V_GS(Volt.)

Si atom 3000 psi SCCO₂ treatment

HfOx layer

Fig. 3-17 Secondary ion mass spectroscopy: (a) Si atom (b) Hf atom and (c) O atom in HfO

₂

film of Baking-only and 3000 psi-SCCO

₂

treatmen

.

Baking-only treatment 3000 psi SCCO₂ treatment

0 50 100 150 200 250 300 3000 psi SCCO₂ treatment

HfOx layer

Si substrate

W/L = 800 um / 600 um , V_D = - 10 volt

Vg (volt.)

-20 -15 -10 -5 0 5 10

Drain Current (ID, Amp.)

10^-8 10^-7 10^-6 10^-5 10^-4 10^-3 10^-2 10^-1

Drain current (I_D) Gate leakage (I_G)

(a)

(b)

W/L = 800 um / 600 um , V_D = - 10 volt

Vg (volt.)

Fig. 3-18 Current vs Voltage plots (I

-V

) of OTFTs characteristics on HfO

film: (a) Baking-only treatment and (b) H

O vapor treatment.

-20 -15 -10 -5 0 5 10

10^-8 10^-7 10^-6 10^-5 10^-4 10^-3 10^-2 10^-1

Drain Current (ID, Amp.)

Drain current (I_D) Gate leakage (I_G)

W/L = 800 um / 600 um , V_D = - 10 volt

Vg (volt.)

-20 -15 -10 -5 0 5 10

Drain Current (ID, Amp.)

10^-12 10^-11 10^-10 10^-9 10^-8 10^-7 10^-6 10^-5

Drain current (I_D) Gate leakage (I_G)

(a)

W/L = 800 um / 600 um , V_D = - 10 volt

Vg (volt.)

(b)

Fig. 3-19 Current vs Voltage plots (I

-V

) of OTFTs characteristics: (a) HfO

film of 3000 psi-SCCO

treatment and (b) PECVD SiO

film.

-20 -15 -10 -5 0 5 10

10^-11 10^-10 10^-9 10^-8 10^-7 10^-6

Drain current (I_D) Gate leakage (I_G)

Drain Current (ID, Amp.)

Out-put characteristic

V_D = - 10 volt

Vg (volt.)

Fig. 3-21 Normailzed Current vs Voltage plots (I

-V

) of OTFTs characteristics of HfO

film with 3000 psi-SCCO

treatment and PECVD SiO

₂

film.

-20 -15 -10 -5 0 5 10

10^-5 10^-4 10^-3 10^-2 10^-1 10⁰ 10¹ 10²

HfO2 film of 3000 psi-SCCO2 treatment PECVD SiO2 film

Normalized Drain current

(a)

Fig. 3-22 Current vs Voltage (I

-V

) characteristics of a OTFTs deposited on HfO2 film with 3000 psi-SCCO2 treatment : (a) DC bias stress of V

= -20V, (b) DC bias stress of V

= -20V and V

= -20V and (c) DC bias stress of V

= -20V and current stress of V = -200nA

V_G= -20V V_D= -20V

Δμ

-200nA (OTFTs deposited on HfO2 film with 3000 psi-SCCO2 treatment)

Fig. 3-24 Threshold voltage shift vs. bias stress time for DC bias stress

of V

= -20V, DC bias stress of V

= -20V and V

= -20V and

DC bias stress of V

= -20V and current stress of V

=

-200nA (OTFTs deposited on HfO2 film with 3000

psi-SCCO2 treatment)

(a)

Fig. 3-25 Current vs Voltage (I

-V

) characteristics of a OTFTs

deposited on PECVD SiO

film : (a) DC bias stress of V

=

Δμ

SECOND

0 200 400 600 800 1000

Δμ

0.90 0.92 0.94 0.96 0.98 1.00

V_G= -20V

V_G= -20V;V_D= -20V V_G= -20V;I_D= -200nA

Fig. 3-26 Mobility shift vs. bias stress time for DC bias stress of V

= -20V, DC bias stress of V

= -20V and V

= -20V and DC bias stress of V

= -20V and current stress of V

= -200nA (OTFTs deposited on PECVD SiO

₂

film)

Fig. 3-27 Threshold voltage shift vs. bias stress time for DC bias stress of V

= -20V, DC bias stress of V

= -20V and V

= -20V and DC bias stress of V

= -20V and current stress of V

= -200nA (OTFTs deposited on PECVD SiO

film)

ΔV_TH

SECOND

0 200 400 600 800 1000

ΔVTH

0.0 0.2 0.4 0.6 0.8 1.0 1.2

1.4 V_G= -20V

V_G= -20V;V_D= -20V V_G= -20V;I_D= -200nA

0.1 - 1.6

- 3.2

29.4 24.8

20.4 SCCO

₂

-3000psi H

₂

O vapor

Baking-only

Table 3-1 The extracted parameters from C-V curves of HfO

₂

films after different treatment, measuring at 1M Hz with gate bias swing from negative voltage to positive voltage (forward).

The V

_fb

means the flat-band voltage, and defined as C/C

_max

= 50%. The change of flat-band voltage of different- treated HfO

₂

films under forward swing is label as ΔV.

~ 0 0.1

ΔV (volt.) 0.9

V

_0.5

(volt.), C/C

_max

= 50%

Dielectric const.

~ 0 0.1

0.9 0.1 - 1.6

- 3.2

29.4 24.8

20.4 SCCO

₂

-3000psi H

₂

O vapor

Baking-only

ΔV (volt.)

V

_0.5

(volt.), C/C

_max

= 50%

Dielectric const.

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