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The advanced nonvolatile memory devices were fabricated and investigated for

solving the problem of conventional nonvolatile memory. This dissertation is divided

into eight chapters. The contents in each chapter are described as follows.

In chapter 1, general background of nonvolatile memory devices is introduced.

In chapter 2, the memory characteristics of Co nanocrystals memory device with

HfO2 as blocking oxide is investigated.

In chapter 3, the nickel nanocrystals with HfO2 blocking oxide for nonvolatile

memory application is studied.

In chapter 4, the fabrication and electrical characteristics of CoSi nanocrystals

nonvolatile memory with HfO2 blocking oxide for memory device applications is

presented.

In chapter 5, the nickel silicide nanocrystals embedded in SiO2 and HfO2 for

nonvolatile memory application are demonstrated.

In chapter 6, the using double layer CoSi2 nanocrystals to improve the memory

effects of nonvolatile memory devices are presented.

In chapter 7, comparison electric characteristics with metal and metal-silicide

nanocrystals memory device with HfO2 as blocking oxide

Finally, the summarization of all experimental results in this dissertation and the

suggestions for the future work are presented in chapter 8.

Fig. 1-1 The structure of the conventional floating gate nonvolatile memory device. Continuous poly-Si floating gate is used as the charge storage element and ONO sandwiched structure is used as the control oxide.

Fig. 1-2 The structure of the SONOS nonvolatile memory device. The nitride layer is used as the charge-trapping element.

Fig. 1-3 The structure of the nanocrystal nonvolatile memory device. The semiconductor nanocrystals or metal nano-dots are used as the charge storage element instead of the continuous poly-Si floating gate.

Nano-Dots

Fig. 1-4 The development of the gate stack of SONOS EEPROM memory devices. The optimization of nitride and oxide films has been the main focus in recent years.

Fig. 1-5 The energy band diagrams of the write/erase operation for a SONOS device.

Chapter 2

Memory characteristics of Co nanocrystals memory device with HfO

2

as blocking oxide

2.1 Motivation

Nonvolatile memory devices with floating-gate structure are being used widely, for

example, in mp3 players, digital cameras and integrated circuit cards at present. The

most prominent one is the limited potential for continued scaling of the device

structure. When the tunnel oxide is thinner, the retention characteristics may be

degraded, and when the tunnel oxide is made thicker to take the isolation into account,

the speed of the operation will be slower. There is, therefore, a tradeoff between speed

and reliability and the thickness of the tunnel oxide is compromised to about 8-11 nm,

which is barely reduced over more than five generations of the industry [2.1].

Recently, memory-cell structure using discrete traps as the charge storage media has

received much attention as the promising candidate to replace conventional dynamic

random access memory or flash memories for future high speed and low power

consuming memory devices [2.2-2.4]. Nanocrystals memory devices employing

distributed nanodots as storage elements have exhibited great potential in device

applications [2.5-2.11]. Among the different materials of nanocrystals, the metal

nanocrystals memory possesses several advantages, such as stronger coupling with

the conduction channel, a wide range of available work functions, higher density of

states around the Fermi level, and smaller energy perturbation due to carrier

confinement [2.3]. Besides, using the high-k dielectric as the blocking oxide

concentrates and releases the electric fields across the tunnel oxide and the blocking

oxide, respectively, under the program/erase mode. Using the high-k dielectric as the

blocking oxide leads to lower program and erase voltage [2.12].

In this study,we demonstrated the electron charging and discharging effects of

Co nanocrystals embedded in SiO2 and HfO2, which is desirable for applications of

the nonvolatile memory technology. The characteristic of Co metal was its high work

function about 4.41eV. Once the charge trapping in the Co nanocrystals, it was more

difficult go back from nanocrystals during retention. Also, the Co metal was

compatible with the current manufacturing technology of semiconductor industry.

2.2 Experimental procedures

Figure 2-1 presents process flow of an HfO2/Co/SiO2/Si stacked structure. (100)

oriented p-type silicon wafers were chemically cleaned by a standard Radio

Corporation of America cleaning, followed by a 3-nm tunnel oxide was thermally

grown at 1000℃ in vertical furnace system. Subsequently, a 3-nm-thick cobalt layer

was deposited onto the tunnel oxide by electron beam evaporation. The Co

nanocrystals were formed by rapid thermal annealing in the N2 ambient at 500℃ for

60 s [2.13]. The 30-nm-thick blocking oxide (HfO2) was capped by sputtering. Finally,

Al gate electrode was finally patterned and sintered. The structural analyses were

performed by transmission electron microscopy (TEM). The capacitance-voltage

(C-V) measurements were performed by an HP 4284A precision LCR meter to study

the electron charging and discharging effects of the Co nanocrystals.

2.3 Results and discussions

AFM analyses of Co thin film are listed in Table 2-1. Mean roughness of the Co

metal film before and after thermal treatment are 0.230nm and 0.471nm, respectively.

It shows that the Co nanocrystals are formed after thermal treatment. Figure 2-2

presents typical bright-field, cross-section TEM images. It shows the structure of

HfO2/Co/SiO2/Si. As illustrated in Fig. 2-2, the well-separated and spherical Co

nanocrystals embedded between the SiO2 layer and HfO2 layers were observed. The

aerial density and mean size of the Co nanocrystals are measured to be

2.13×1012/cm2.and 2 nm, respectively.

Figure 2-3 shows the forward and reverse sweep C-V characteristics, indicating the

electron charging and discharging effects of Co nanocrystals embedded between the

SiO2 and HfO2 layers. The bidirectional C-V sweeps were performed from deep

inversion to deep accumulation and in reverse, which exhibited electron charging

effect. In Fig. 2-3, with the voltage swept from 5 to -5V and back to 5 V, an

outstanding threshold voltage shift of 1 V was observed. As the whisked voltage was

increased to 7V, a more obvious C-V shift of 1.8 V was seen. It is perceived that the

hysteresis is counterclockwise which is due to injection of electrons from the deep

inversion layer and injection of holes from the deep accumulation layer of Si substrate.

The result of C-V shift indicates that the charging effects of Co nanocrystals are more

significant than the semiconductor nanocrystals. The high-k blocking oxide

concentrates the electric fields across the tunnel oxide and releases it across the

blocking oxide under program and erase mode. This effect leads to lower program and

erase voltage. Figure 2-4 presents gate voltage dependence of the memory window.

The threshold voltage shift is increased with gate voltage. Figure 2-5 shows the band

diagrams of “program” and “erase” operations with different gate polarities of the

memory device. When the device is written or programmed, the electrons directly

tunnel from the Si substrate through the tunnel oxide, and are trapped in the Co

nanocrystals. On the other hand, as the device is erased, the electrons may tunnel back

to the deep accumulation layer of Si substrate. The blocking oxide is utilized to

prevent the carriers of gate electrode from injecting into the Co nanocrystals by

Fowler-Nordheim tunneling. In addition, the Co nanocrystals do not bear a voltage

drop from gate voltage, which means that all the voltages provided from control gate

are dropped to the tunnel oxide and control oxide and gain advantage over their

semiconductor counterparts. The operating voltage of the memory devices with

conventional floating gate or semiconductor nanocrystals embedded in SiO2 is above

7V. In our approach to fabricate the Co nanocrystals embedded in SiO2, a lower

programming voltage of 5V and erasing voltage of -5 V realize a significant threshold

voltage shift, 1 V, which is sufficient to be defined as “1” and “0” by a typical sensing

amplifier for a memory device.

The retention characteristics of the Co nanocrystals were measured at room

temperature, as shown in Fig. 2-6. If there are some leakage paths for the trapping

charges, the memory effect will gradually decrease. In Fig. 2-4, the good retention

characteristics and the memory effect without significant decreasing up to 104 s can be

founded. The charge loss rate only decreases to 21.95% after 104 s. The inset shows

that the threshold-voltage shift does not significantly decrease after long time (104 s).

It is clearly shown that the Co nanocrystals memory has excellent retention

characteristic.

In addition, the reliability of the memory device was also investigated. As shown in

Fig.2-7, the data endurance of the Co nanocrystals memory device retains an obvious

memory window of 0.86 V after 106 cycles and write/erase voltage was 5/(-5) V. The

good endurance behavior of the Co nanocrystals memory device can be founded.

2.4 Conclusions

In summary, the memory effects of the Co nanocrystals using tunneling and control

oxide, SiO2 and HfO2, were demonstrated in this letter. A significant C-V hysteresis of

Vt shift of 1V is observed under low operating voltage of 5V. The retention

characteristics are tested to be robust. Also, the endurance of the memory device is not

degraded up to 106 write/erase cycles.

Fig. 2-1 Process flow of an HfO2/Co/SiO2/Si stacked structure

Table 2-1 AFM analyses of Co thin film(scan area: 5 × 5 μm )

Fig. 2-2 The Cross-section TEM micrographs of an HfO2/Co/SiO2/Si

Fig. 2-3 The capacitance-voltage (C-V) hysteresis of Co nanocrystals memory device after bidirectional sweeps between 5V/(-5V) and 7V/(-7V).

Fig. 2-4 Gate voltage dependence of the memory window.

Gate Voltage (V)

0 1 2 3 4 5 6 7 8 9 10 11 12

T hr eshol d vol tage shi ft ( V )

0

1

2

3

4

5

6

7

Fig. 2-5 The band diagrams of the operation of the distributed charge storage with Co nano-dots.

Fig. 2-6. Data retention characteristics of the Co nanocrystals memory device.

Fig. 2-7. Endurance characteristics of the Co nanocrystals memory

Chapter 3

Nickel nanocrystals with HfO

2

blocking oxide for nonvolatile memory application

3.1 Motivation

The commercial products contain poly-Si floating gate (FG) structure which is

taken as charge storage layer. Because of continued scaling of the device structure,

the tunneling oxide must thinner. Once the tunnel oxide is thinner, the electrical

characteristics such as endurance and retention may be degraded. Therefore

memory-cell structures which use discrete traps as the charge storage media have

received much attention. These memories can replace conventional dynamic random

access memory or flash memories for future high speed and low power consuming

memory devices [3.1-3.3]. Nanocrystal memory devices employing distributed

nanodots as storage elements have exhibited great potential in device applications

[3.4-3.10]. Among the different materials of nanocrystals, the metal nanocrystal

memory possesses several advantages: (1) stronger coupling with the conduction

channel; (2) a wide range of available work functions; (3) higher density of states

around the Fermi level; (4) smaller energy perturbation due to carrier confinement

[3.11]. Besides, we use the high-k dielectric as the blocking oxide. Its concentrates

and releases the electric fields across the tunnel oxide and the blocking oxide,

respectively, under the program/erase mode. At the same time, using the high-k

dielectric as the blocking oxide leads to lower program and erase voltage [3.12].In

this study,we demonstrated the memory characteristics of Ni nanocrystals embedded

in SiO2 and HfO2. Because Ni metal has higher work function (~ 4.96eV) than Co

metal(~ 4.41eV). It causes the retention different. Also Ni is compatible with the

current manufacturing technology of semiconductor industry.

3.2 Experimental procedures

Metal-oxide-silicon (MOS) capacitors were fabricated using silicon p-type wafers

[(100) orientation]. Figure 3-1 illustrates the process flow of fabricating Ni

nanocrystals. First, the wafers were chemically cleaned by a standard Radio

Corporation of America cleaning. The thin tunnel oxide (3nm) was thermally grown

at 1000℃ in vertical furnace system. Subsequently, a 3-nm-thick nickel layer was

deposited onto the tunnel oxide by electron beam evaporation. The Ni wetting layer

transformed the Ni nanocrystals after the Rapid thermal annealing (RTA) in the N2

ambient at 500℃ for 60 sec. A 30-nm-thickness blocking oxide (HfO2) was capped

by sputter. The parameter of the high-k sputtering is 0.3 Å/sec as rf power sputter in

150W under the working pressure of 20 mTorr. The flow rate of Ar/O2 is 20/5 SCCM

(SCCM denotes cubic centimeter per minute at STP). The dielectric constant of HfO2

is 20. Finally, Al gate electrode was patterned and sintered. The structural analyses

were performed by transmission electron microscopy (TEM). The capacitance-voltage

3.3 Results and discussions

(C-V) measurements were performed by a precision LCR meter HP 4284A to

study the electron charging and discharging effects of the Ni nanocrystals.

Table 3-1 presents AFM analyses of Ni thin film. Mean roughness of the Ni

metal film before and after thermal treatment are 0.229nm and 0.457nm, respectively.

It shows that the Ni nanocrystals are formed after thermal treatment. Figure 3-2 shows

the cross-section TEM of Ni nanocrystal memory structure. The figure presents the

structure of Si substrate/ tunneling oxide/ Ni nanocrystals. The well-separated and

spherical Ni nanocrystals are observed. The higher-resolution image confirms the

presence of Ni nanocrystals of approximately 5 nm in diameter. The aerial density of

the Ni nanocrystals is measured to be 3.9×1012/cm2.

Figure 3-3 presents the C-V characteristics of Ni nanocrystals embedded

between the SiO2 and HfO2 layers. It is found that a low operating voltage, 4 V,

causes a significant threshold-voltage shift up to ~ 1 V, which is sufficient to be

defined as ‘‘1’’ or ‘‘0’’ for the logic-circuit design. The electrons of the deep

inversion layer and holes of the deep accumulation layer were injected from the Si

substrate into the nanocrystals, so that the C-V hysteresis is counterclockwise. The

high-k blocking oxide concentrates the electric fields across the tunnel oxide and

releases it across the blocking oxide under program and erase mode. This effect leads

to lower program and erase voltage. The blocking oxide is utilized to prevent the

carriers of gate electrode from injecting into the Ni nanocrystals by Fowler-Nordheim

tunneling. In addition, the Ni nanocrystals do not bear a voltage drop from gate

voltage, which means all the voltages provided from control gate are dropped to

tunnel oxide and control oxide and gains advantage over their semiconductor

counterparts. Figure 3-4 presents gate voltage dependence of the memory window.

The threshold voltage shift is increased with gate voltage.

The retention characteristics of the Ni nanocrystals were measured at room

temperature, as shown in Fig. 3-5. If there are some leakage paths for the trapping

charges, the memory effect will gradually decrease. In Fig. 3-5, the good retention

characteristics can be founded and the memory effect without significant decreasing

up to 104 s. The charge loss rate only decreases to 15.65% after 104 s. It is clearly

shown that the Ni nanocrystals memory has excellent retention characteristic.

The programming characteristics of Ni nanocrystals memory were studied by

stressing samples with a pulse voltage of ±5 V and a pulse width of 5 ms during

programming and erasing (P/E). Figure 3-6 shows the endurance characteristics of Ni

nanocrystals memory after different stressing cycles at room temperature. The

threshold voltage shift as a function of stressing cycles shows superior endurance.

There was no degradation of the threshold voltage shift observed even after 106 P/E

cycles.

3.4 Conclusions

In summary, the nonvolatile memory device with Ni nanocrystals exhibits 1 V

threshold voltage shift under 4 V write operation, which is sufficient for a memory

device to define the signal “0” and “1”. The device has a long retention time with a

small charge lose rate. Besides, the endurance of the memory device is not degraded

up to 106 write/erase cycles.

3.5 Retention characteristics different with Co and Ni nanocrystals memory device

This section discusses the retention different between Co and Ni nanocrystals

memory device. Fig. 3-7 shows the retention characteristic for Co and Ni nanocrystals

memory device. The charge loss rate of Co metal and Ni metal are 21.95% and

15.65% respectively after 104 s. The charge loss rate of Co metal is more than Ni

metal. Because Ni metal has higher work function (~ 4.96eV) than Co metal(~ 4.41eV)

as shown in Fig. 3-8. Fig. 3-8 presents band diagram of Ni and Co nanocrystals

nonvolatile memory during retention. The electrons tunnel from the Si substrate

through the tunnel oxide, and are trapped in the Co and Ni nanocrystals when device

metal nanocrystals. The band offset between SiO2 tunnel oxide and nanocrystals

become high due to high work function of metal. The higher band offset between

SiO2 tunnel oxide and nanocrystals, the more difficult electrons go back Si substrate

from nanocrystals. The work function of Ni metal is about 4.96eV. Its more than Co

metal(~ 4.41eV). Therefore the retention characteristic of Ni nanocrystals is better

than Co nanocrystals.

Fig. 3-1 Process flow of an HfO2/Ni/SiO2/Si stacked structure

Table 3-1 AFM analyses of Ni thin film.

Fig. 3-2. Cross-section TEM micrographs of an Ni/SiO2/Si stacked structure.

Fig. 3-3. The capacitance-voltage (C-V) hysteresis of Ni nanocrystals memory device after bidirectional sweeps between 4V/(-4V) and 5V/(-5V).

Fig. 3-4 Gate voltage dependence of the memory window.

Gate Voltage (V)

0 1 2 3 4 5 6 7

T hr e s h ol d vol tage shi ft ( V )

0.0 0.5 1.0 1.5 2.0 2.5

Fig. 3-5. The retention characteristics of the Ni nanocrystals memory device at room temperature.

Fig. 3-6. The endurance characteristics of the Ni nanocrystals memory device at room temperature.

Fig. 3-7 Retention for Ni and Co nanocrystals nonvolatile memory.

Fig. 3-8 Band diagram of Ni and Co nanocrystals nonvolatile memory.

Chapter 4

Fabrication and electrical characteristics of CoSi nanocrystals nonvolatile memory with HfO

2

blocking oxide for memory device applications

4.1 Motivation

The lots produced nonvolatile memory devices are based on the concept of a

continuous layer of floating gate up to now [4.1]. Although many popular products are

made by nonvolatile memory devices, it still has the difficulties of continue scaling

down [4.2]. It must compromise between long-term nonvolatility and high operating

speed [4.3]. Therefore the concept of distributed storage of charge has caught a lot of

attention lately. Tiwari et al. [4.4] was the first time demonstrated the Si nanocrystal

floating gate memory device in the early nineties to solve the scaling limits of the

conventional FG structure. The nanocrystal memory device can not only maintain

good retention characteristics when tunnel oxide is thinner but also lower the power

consumption [4.4-4.13]. Direct forming of the metal nanocrystals from metal (Co,Ni)

films have many problems. For example, the size of metal nanocrystals cannot be

controlled. The metal nanocrystals have more active with other materials during the

processes. It may cause the devices failure. So we search the materials which are more

stable than metal. In this study, we demonstrated the fabrication and memory

desirable for applications of the nonvolatile memory technology.

4.2 Experimental procedures

Silicon p-type wafers [(100) orientation] were chemically cleaned by a standard

Radio Corporation of America cleaning. The 3-nm tunnel oxide was thermally grown

at 1000℃ in vertical furnace system. Subsequently, 3-nm a-Si layer and 3-nm Cobalt

layer were deposited onto the tunnel oxide by electron beam evaporation. As shown in

figure 4-1, the stacked structure was oxidized at 700℃ for 5 minutes to form CoSi

nanocrystals. The nanocrystals were identified to be CoSi phase by the analysis of

electron diffraction pattern shown in figure 4-2 [4.14]. A 30-nm-thickness blocking

oxide (HfO2) was capped by sputter. Finally, Al gate electrode was finally patterned

and sintered. The structural analyses were performed by transmission electron

microscopy (TEM). The capacitance-voltage (C-V) measurements were performed by

a precision LCR meter HP 4284A to study the electron charging and discharging

effects of the CoSi nanocrystals.

4.3 Results and discussions

Figure 4-3 shows the capacitor-gate voltage(C-V) characteristics of CoSi

nanocrystal embedded between the SiO2 and HfO2 layers. The electrical C-V

measurements are performed by bidirectional voltage sweep. In Fig. 4-3, with the

voltage swept from 9 to (-9) V and back to 9 V, a significant threshold voltage shift of

1.6 V is observed. As the swept voltage is increased to 12V, a more pronounced C-V

shift is observed. The electrons of the deep inversion layer and holes of the deep

accumulation layer were injected from the Si substrate into the nanocrystals, so that

the C-V hysteresis is counterclockwise. The high-k blocking oxide concentrates the

electric fields across the tunnel oxide and releases it across the blocking oxide under

program and erase mode. This effect leads to lower program and erase voltage. The

blocking oxide is utilized to prevent the carriers of gate electrode from injecting into

blocking oxide is utilized to prevent the carriers of gate electrode from injecting into

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