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Chapter 2 Memory characteristics of Co nanocrystals memory device

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

the CoSi nanocrystals by Fowler-Nordheim tunneling. In addition, the CoSi

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. The inset was the

cross-section TEM of CoSi nanocrystals memory structure. It presents the structure of

Si substrate/ tunneling oxide/ CoSi nanocrystals/ HfO2 blocking oxide. The

well-separated and spherical Ni nanocrystals are observed.

In Fig.4-4, the charge retention characteristics of the CoSi nanocrystals were

measured at room temperature. If there are some leakage paths for the trapping

charges, the memory effect will gradually decrease. In Fig.4-4, 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 33.33% after 104 s. The inset was

threshold voltage shift versus time. It is clearly shown that the CoSi nanocrystals

memory has excellent retention characteristic.

The reliability of memory is major issue for nonvolatile memory devices. The

endurance of CoSi nanocrystals memory were studied by stressing samples with a

pulse voltage of ±7 V and a pulse width of 5 ms. Figure 4-5 shows the endurance

characteristics of CoSi nanocrystals memory after different stressing cycles. The

threshold voltage shift versus stressing cycles shows superior endurance. There was

no significant degradation (only 17.1%) of the threshold voltage shift observed even

after 106 P/E cycles.

4.4 Conclusions

In conclusion, the nonvolatile memory device with CoSi nanocrystals exhibits

1.6 V threshold voltage shift under 9 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.

Fig. 4-1. The process flow proposed in this work.

Fig. 4-2. The electron diffraction pattern corresponding to CoSi nanocrystals.

Fig. 4-3. The capacitance-voltage (C-V) hysteresis of CoSi nanocrystals memory device after bidirectional sweeps between 9V/(-9V) and 12V/(-12V). The inset is cross-section TEM micrographs of an HfO2/CoSi/SiO2/Si stacked structure.

Gate Voltage (V)

Fig. 4-4. Data retention characteristics of the CoSi nanocrystals memory device.

Fig. 4-5. Endurance characteristics of the CoSi nanocrystals memory device.

Chapter 5

Nickel silicide nanocrystals embedded in SiO

2

and HfO

2

for Nonvolatile Memory Application

5.1 Motivation

Nonvolatile memory is a necessary indispensable component of modern

electronic systems. Nonvolatile memory is used in personal computers, cellular

phones, digital cameras, global positioning systems, etc. Conventional floating-gate

(FG) devices have their limitations, because of continued scaling of the device

structure. The tunnel oxide is thinner with the continued scaling down. So the

retention characteristics of memory devices may be degraded [5.1]. 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 [5.2-5.3]. Nanocrystals memory devices employing distributed

nanodots as storage elements have exhibited great potential in device applications

[5.4-5.10]. 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 [5.3]. 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 a high-k dielectric as the blocking oxide leads to lower

program and erase voltage [5.11].

5.2 Experimental procedures

(100) oriented p-type silicon wafers were chemically cleaned by a standard

Radio Corporation of America cleaning, followed by formation of a 3-nm tunnel

oxide layer which was thermally grown at 1000℃ in a vertical furnace system.

Subsequently, a 3-nm amorphous silicon layer and a 3-nm-thick nickel layer were

deposited onto the tunnel oxide by electron beam evaporation, respectively. In

addition, a 10-nm amorphous silicon layer was deposited on some of the samples.

Oxidation at 800℃ 700℃ and 600 ℃ was performed at 5min, 10min and 10min

respectively to form nickel silicide nanocrystals. The 30-nm-thickness blocking oxide

(HfO2) layer was deposited by sputtering. Finally, an Al gate electrode was

patterned and sintered. Figure 5-1 presents the process flow. 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 nickel silicide nanocrystals.

5.3 Results and discussions

Figure 5-2 shows the forward and reverse sweep C-V characteristics, indicating

the electron charging and discharging effects of nickel silicide 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 an electron

charging effect. In Fig. 5-2, with the voltage swept from 8 to -8V and back to 8 V, an

outstanding threshold voltage shift of 0.7 V was observed. As the whisked voltage

was increased to 10V, a more obvious C-V shift of 1.3 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 resulting C-V shift indicates that the charging effects of nickel silicide

nanocrystals are more significant than that seen for 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. When the device is written or programmed, the

electrons directly tunnel from the Si substrate through the tunnel oxide, and are

trapped in the nickel silicide nanocrystals. On the other hand, as the device is erased,

the electrons may tunnel back to the deep accumulation layer of the Si substrate. The

blocking oxide is utilized to prevent the carriers from the gate electrode from being

injected directly into the nickel silicide nanocrystals by Fowler-Nordheim tunneling.

In addition, the nickel silicide nanocrystals do not exhibit a voltage drop from the gate

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

tunnel oxide and control oxide and this provides an advantage over their

semiconductor counterparts. Figure 5-3 presents the cross-section TEM micrographs

of an HfO2/nickel silicide /SiO2/Si stacked structure with dry oxidation at 600℃. As

illustrated in Fig. 5-3, well-separated and spherical nickel silicide nanocrystals were

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

be a NiSi2 phase through analysis of the diffraction ring pattern shown in Fig. 5-4.

Figure 5-5 shows the capacitance-voltage (C-V) hysteresis of sample with

α-Si/Ni/α-Si structure after dry oxidation at 700℃. It was found that as the voltage

swept from 8 to -8V and back to 8 V, significant threshold voltage shift of 1.7 V was

observed. When the whisked voltage was increased to 10V, a more obvious C-V shift

of 2.1 V was seen. For samples oxidized at 600℃, these voltages were larger shift. In

figure 5-6, the voltage swept from 3 to -3V and back to 3 V, a threshold voltage shift

of 0.4 V was observed. When the whisked voltage was increased to 5V, a more

obvious C-V shift of 2 V was seen. Figure 5-7 presents the threshold voltage vs.

operation voltage for samples oxidized at different temperature. The sample which

used α–Si/Ni/α-Si structure had improved memory characteristics. As shown in

figure 5-1, the nickel silicide nanocrystals of α–Si/Ni/α-Si structure had random

distribution between SiO2 and HfO2. It was different from the α–Si/Ni conventional

device(distribution of plane) [5.10][5.12]. It shows that more charges were injected

into deep nickel silicide nanocrystals under programming mode. The charges which

were injected into deep nickel silicide nanocrystals resulted in the higher threshold

voltage. The operating voltage of the memory devices with a conventional floating

gate or semiconductor nanocrystals embedded in SiO2 is above 7V [5.13-5.14]. In our

approach to fabricate the nickel silicide nanocrystals embedded in SiO2 and HfO2, a

lower programming voltage of 4V and erasing voltage of -4 V realizes a significant

threshold voltage shift, 1.3 V, which is sufficient to be defined as “1” and “0” by a

typical sensing amplifier for a memory device.

5.4 Conclusions

A nonvolatile memory device with NiSi2 nanocrystals embedded in the SiO2 and

HfO2 layer has been fabricated. A significant memory effect is observed through the

electrical measurements. When a low operating voltage, 4V, is applied a significant

threshold-voltage shift, 1.3V, is observed. The processing of the structure is

compatible with the current manufacturing technology of semiconductor industry.

Fig. 5-1 The process flow of nickel silicide nanocrystals.

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