CN109935687A - A kind of multi-level phase change V2O5Thin-film material and its preparation method and application - Google Patents
A kind of multi-level phase change V2O5Thin-film material and its preparation method and application Download PDFInfo
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Abstract
The present invention relates to a kind of multi-level phase change V2O5Thin-film material and its preparation method and application.Vanadium and O occur during magnetron sputtering using reactive deposition method2Reaction and be deposited on substrate, pass through control Ar gas and O2Throughput and sputtering pressure generate V2O5, rather than other oxides of vanadium.Obtained V2O5Occur amorphous state, intermediate state and crystalline state three different phases during reversible transition of the film under 200~300nm thickness, shows 3 different resistance values, stored compared to traditional binary states, multi-level phase change V of the invention2O5Thin-film material has higher storage density；And multi-level phase change V of the invention2O5Thin-film material has faster phase velocity, and 10 annual datas keep temperature to reach 200 DEG C, is much larger than tradition Ge2Sb2Te585 DEG C of material have preferable thermal stability.Multi-level phase change V of the invention2O5Thin-film material industry application value with higher.
Description
Technical field
The present invention relates to technical field of information storage, and in particular to a kind of multi-level phase change V2O5Thin-film material and its preparation side
Method and application.
Background technique
The performances such as high speed, high density, low-power consumption are needed to have as novel information memory, just adapt to the following big data
The requirement of information processing.Phase transition storage (PCRAM) is to be quickly converted to realize between crystalline state-amorphous state using material
A kind of novel non-volatility memorizer of information storage.There is high resistance when phase-change material is in amorphous state, when crystalline state has
Phase-change material interior atoms are resequenced or are upset using the Joule heat that electric pulse generates, to realize high-impedance state by low resistance
Repetition conversion between low resistance state, achievees the purpose that information stores.It has reading speed is fast, stability is strong, it is low in energy consumption, deposit
Store up the advantages that density is high, compatible with traditional CMOS technology, thus the concern by more and more researchers.
Ge2Sb2Te5(GST) phase-change material is that the phase transformation that current research is most, most widely used is deposited because of its excellent combination property
Material is stored up, but since its lower crystallization temperature and poor thermal stability make the data retention of GST less desirable,
So the purpose in order to realize more high stability, faster phase velocity, more and more New-type phase change storage materials are not turned off
It issues.Zhu Min et al. has developed Ti-Sb-Te phase-change material, specific fast nearly 10 times of the service speed (6ns of comparison GST device
Set speed, 500ps Reset speed), low 80% operation power consumption, the resistance drift coefficient of small an order of magnitude, and it is reversible
Operation is more than 107It is secondary that (particular content is detailed in Shanghai Inst. of Microsystem and Information Technology, Chinese Academy of Sci's doctorate in 2014
Paper third page).Lu etc. has developed the Ga with ultra-long data holding capacity14Sb86Alloy, 10 annual datas keep temperature
Reach 162 DEG C, (particular content is detailed in the Journal Of of volume 109 of the 6th phase in 2011 for the data storage that can be used under hot environment
Physics 064503-1 to 064503-3 pages of Applied).In addition, the phase-change materials such as Si-Sb-Te, Ni-Ti, Cu-Sb-Te
Also it is studied, there is preferable storage performance.
But the above material only shows the transformation of amorphous state to crystalline state, i.e., traditional binary states storage, storage density has
Limit.
Summary of the invention
The limited technical problem of its storage density is stored based on above-mentioned traditional binary states, the present invention provides a kind of multi-level phase change
Vanadic anhydride (V2O5) thin-film material.
The multi-level phase change V2O5The reversible transition process with a thickness of 200~300nm, under the thickness of thin-film material
In have apparent amorphous state-intermediate state-crystalline state reversible transition, occur amorphous state, intermediate state and crystalline state in phase transition process
Three different phases, and show 3 different resistance values.
The present invention also provides a kind of multi-level phase change V2O5The preparation method of thin-film material, the preparation method is that reactive deposition
Method.
Further, the reactive deposition method be occur vanadium and oxygen using magnetron sputtering react and be deposited on substrate,
Pass through control Ar gas and O2Gas flow and sputtering pressure, generate V on substrate2O5Method, rather than vanadium other oxidation
Object.
The multi-level phase change V2O5The preparation method of thin-film material, specifically includes the following steps:
(1) SiO is cleaned2/ Si (100) substrate；
(2) V is prepared2O5Preparation before film: vanadium target target to be sputtered is installed, magnetron sputtering chamber is vacuumized；If
Determine sputtering power；Set sputter gas Ar gas and O2Gas gas flow simultaneously adjusts sputtering pressure；
(3) multi-level phase change V is prepared2O5Thin-film material:
A) space base support is rotated into vanadium target target position, opens the AC power source on target, sputtering time is set 1., to the target of vanadium target
Material surface is sputtered to clean target material surface；
B) after the completion of target surface cleaning, the shutter above vanadium target target position is closed；By the cleaned substrate in step (1)
It is placed in space base support, substrate to be sputtered is rotated to above vanadium target target position, shutter above vanadium target target position is opened, according to setting
Sputtering time 2. and sputter rate, start sputtering and generate V2O5Film.
Further, sputtering power described in step (2) is 100~200W, sputtering pressure 0.20Pa.
Preferably, the sputtering power is 150W.
Further, sputter gas described in step (2) is Ar gas and O2The mixed gas of gas, the volume hundred of the Ar gas
Divide >=99.999%, gas flow is 60~80sccm；The O2Volume basis >=99.999% of gas, gas flow be 5~
15sccm。
Preferably, the gas flow of the Ar gas is 70sccm, O2The gas flow of gas is 10sccm.
Further, 1. the sputtering time is 200s, 2. the sputtering time is 500~3750s, sputter rate 2
~15s/nm.
Preferably, 2. the sputtering time is 1000~2000s, and sputter rate is 5~10s/nm.
Further, the purity of the atomic percent of the vanadium target is greater than 99.999%, and shape is cylinder, and diameter is
50.5mm, with a thickness of 4mm, back end copper thickness is 2mm.
The present invention finally provides a kind of multi-level phase change V2O5Application of the thin-film material in multi-level phase change memory.
Advantageous effects: occurred during magnetron sputtering using reactive deposition method vanadium and oxygen react and deposition
In substrate, pass through control Ar gas and O2Gas flow and sputtering pressure, generate V on substrate2O5, rather than other oxygen of vanadium
Compound.Obtained V2O5There is amorphous state, intermediate state during reversible transition of the thin-film material under 200~300nm thickness
The phase different with crystalline state three shows 3 different resistance values, stores compared to traditional binary states, multistage phase of the invention
Become V2O5Thin-film material has higher storage density；And multi-level phase change V of the invention2O5Thin-film material has faster phase transformation
Speed, 10 annual datas keep temperature to reach 200 DEG C, are far longer than traditional Ge2Sb2Te585 DEG C of material have preferable heat
Stability.Multi-level phase change V of the invention2O5Thin-film material industry application value with higher.
Detailed description of the invention
Fig. 1 is multi-level phase change V prepared by the embodiment of the present invention 12O5The In-situ resistance and temperature profile of thin-film material are surveyed
Heating rate during examination is 20 DEG C/min.
Fig. 2 is the 1 multi-level phase change V of the embodiment of the present invention for calculating crystallization activation energy2O5Thin-film material is in different isothermal temperature
Normalized resistance versus time curve under degree；Upper right corner illustration is crystallization activation energy fitted figure.
Fig. 3 is based on multi-level phase change V of the invention2O5Thin-film material is applied to the electrical property figure of PCRAM device, and wherein PCL is
V of the invention2O5Film.
Specific embodiment
The present invention is further described below in conjunction with drawings and the specific embodiments, but is not limited the scope of the invention.
Embodiment 1
In the present embodiment multi-level phase change thin-film material the preparation method is as follows:
(1) SiO is cleaned2/ Si (100) substrate, clean the surface, the back side remove dust granule, organic and inorganic impurity；
A) it is cleaned by ultrasonic by force in ethanol solution 40~60 minutes, surface and the back side is dried up after flushing；
B) in 120 DEG C of drying in oven steam, until silicon chip surface is dry；
(2) V is prepared2O5Preparation before film:
A) high purity vanadium target sputtering target material is installed, and base vacuum is evacuated to 1 × 10-4Pa；
B) sputtering power 150W is set；
C) high-purity Ar and O are used2Mixed gas as sputter gas, set Ar throughput as 70sccm, O2Throughput is
10sccm, and sputtering pressure is adjusted to 0.20Pa.
(3) multi-level phase change V is prepared2O5Thin-film material:
A) space base support is rotated to the target position of vanadium target, the AC power source applied on vanadium target is opened, according to the sputtering of setting
Time 1. 200s, sputters the target surface of vanadium target to clean target material surface；
B) after the completion of target surface cleaning, the shutter above vanadium target target position is closed；Substrate to be sputtered is rotated into vanadium target
Above target position, the shutter above vanadium target target position is opened, according to the sputtering time 1250s of setting, sputter rate 5s/nm, is started
Sputtering generates V2O5The multi-level phase change V that film thickness is 250nm is finally made in film2O5Thin-film material.
Obtained film passes through the measurement of energy disperse spectroscopy EDS, and the group of film is divided into V2O5。
The prepared V of detection2O5Film performance:
Fig. 1 is V obtained by the embodiment of the present invention 12O5Its In-situ resistance of thin-film material and temperature curve figure, test
Heating rate in the process is 20 DEG C/min.
From figure 1 it appears that at the beginning, with the raising of heating temperature, the resistance of film is gradually decreased, at 318 DEG C
Film is all in amorphous structure (including in figure beforeWithIt is shown), discoverySlope ratioSteeper, this may be
Caused by being oxidized due to the material on film portion surface in heating process；When temperature reaches 318 DEG C of its first time phase transition temperature,
Film resistor is rapidly from amorphous 2.0 × 108Ω is reduced to intermediate state2.3 × 107Ω；As temperature further increases
When to 346 DEG C, telomutation is had occurred in resistance, from the 2.2 × 10 of intermediate state7Ω drops to crystalline state9.1 × 105Ω.More than
Show that film has occurred by amorphous state to intermediate state, then arrives the diauxic shift of crystalline state.Therefore, obtained V2O5Thin-film material exists
Occur three amorphous state, intermediate state and crystalline state different phases in phase transition process, and shows 3 different resistance values, compared to
Traditional binary states storage, multi-level phase change V of the invention2O5Thin-film material has higher storage density.
It is the reason of in order to further analyze resistance variations, rightThe conductivity activation energy of this 4 states is fitted.
From the upper right corner illustration interpretation of result of Fig. 1,Conductivity activation energy be respectively 0.63,0.51,0.41 and
0.23eV, in reduced trend, smaller conductivity activation energy will make free electron be easier to occur the transition from valence band to conduction band, from
And show lower resistivity.
Fig. 2 is V made from the embodiment of the present invention 12O5Normalized resistance of the thin-film material under different isothermal temperatures is at any time
Between change curve, conclusion shows multi-level phase change V obtained by the present invention2O5Nano film material can 200 DEG C at a temperature of will
Data are kept for 10 years, this temperature is far longer than Ge2Sb2Te585 DEG C, obtained multi-level phase change V as a result,2O5Nanometer thin membrane material
Material has preferable data retention.
Fig. 3 (a) is the structural schematic diagram of PCRAM device cell, wherein V of the present invention used in PCL2O5Film；Fig. 3 (b) is base
In V2O5The I-V curve of the PCRAM device of film.By Fig. 3 (b) it is found that obviously observed electric current in voltage increase process
Secondary change process, threshold transition voltage are respectively 0.5V and 1.12V.It is 8ns in Voltage Pulse Width with (d) in Fig. 3 (c)
Under the conditions of R-V curve in SET and RESET this pair of of reversible process, the visible increase with voltage, resistance are first in two figures
After there is mutation process twice, this shows that phase transition process twice has occurred in thin-film material；And applied voltage pulse width is
8ns, this shows that the material has faster phase velocity.
Embodiment 2
The preparation method of multi-level phase change thin-film material is same as Example 1 in the present embodiment, and difference is: step (2)
In sputtering power be 100W, Ar throughput be 63sccm, O2Throughput is 9sccm；B in step (3)) sputtering time be
3750s, sputter rate 15s/nm, film thickness 250nm.
Obtained film passes through the measurement of energy disperse spectroscopy EDS, and the group of film is divided into V2O5.Performance detection is carried out to the film, is surveyed
There is three kinds of amorphous state, intermediate state and crystalline state different phases during obtaining reversible transition of the material under the film thickness.
Embodiment 3
The preparation method of multi-level phase change thin-film material is same as Example 1 in the present embodiment, and difference is: step (2)
In sputtering power be 130W, Ar throughput be 80sccm, O2Throughput is 12sccm；B in step (3)) sputtering time be
3000s, sputter rate 12s/nm, film thickness 250nm.
Obtained film passes through the measurement of energy disperse spectroscopy EDS, and the group of film is divided into V2O5.Performance detection is carried out to the film, is surveyed
There is three kinds of amorphous state, intermediate state and crystalline state different phases during obtaining reversible transition of the material under the film thickness.
Embodiment 4
The preparation method of multi-level phase change thin-film material is same as Example 1 in the present embodiment, and difference is: step (2)
In sputtering power be 180W；B in step (3)) sputtering time be 750s, sputter rate 3s/nm, film thickness 200nm.
Obtained film passes through the measurement of energy disperse spectroscopy EDS, and the group of film is divided into V2O5.Performance detection is carried out to the film, is surveyed
There is three kinds of amorphous state, intermediate state and crystalline state different phases during obtaining reversible transition of the material under the film thickness.
Embodiment 5
The preparation method of multi-level phase change thin-film material is same as Example 1 in the present embodiment, and difference is: step (2)
In sputtering power be 200W；B in step (3)) sputtering time be 500s, sputter rate 2s/nm, film thickness 300nm.
Obtained film passes through the measurement of energy disperse spectroscopy EDS, and the group of film is divided into V2O5.Performance detection is carried out to the film, is surveyed
There is three kinds of amorphous state, intermediate state and crystalline state different phases during obtaining reversible transition of the material under the film thickness.
Comparative example 1
The preparation method of thin-film material is same as Example 1 in this comparative example, and difference is: the sputtering in step (2)
Power is 50W, and Ar throughput is 40sccm, O2Throughput is 20sccm；B in step (3)) sputtering time be 4500s, sputtering
Rate is 30s/nm, film thickness 150nm.
Obtained film passes through the measurement of energy disperse spectroscopy EDS, and the group of film is divided into V2O5.Performance detection is carried out to the film, is surveyed
It obtains the material and phase transition process is not present in temperature-rise period, therefore cannot function as the materials'use of PCRAM.
Comparative example 2
The preparation method of thin-film material is same as Example 1 in this comparative example, and difference is: the sputtering in step (2)
Power is 300W, and Ar throughput is 100sccm, O2Throughput is 30sccm；B in step (3)) sputtering time be 1050s, splash
Firing rate rate is 3s/nm, film thickness 350nm.
Obtained film passes through the measurement of energy disperse spectroscopy EDS, and the group of film is divided into V2O5.Performance detection is carried out to the film, is surveyed
It obtains the material and phase transition process is not present in temperature-rise period, therefore cannot function as the materials'use of PCRAM.
By above series of experiment it is found that film thickness has certain influence to multistage reversible transition process, when the film thickness of material
Material just has multistage reversible transition process when at 200~300nm, and there are three different phases for tool.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe
The those skilled in that art for knowing this technology all without departing from the spirit and scope of the present invention, repair above-described embodiment
Decorations change.Therefore, such as those of ordinary skill in the art without departing from disclosed spirit and skill
All equivalent modifications completed under art thought or change should be covered by the claims of the present invention.
Claims (9)
1. a kind of multi-level phase change V2O5Thin-film material, which is characterized in that the V2O5Thin-film material is the thickness of 200~300nm,
Three kinds of amorphous state, intermediate state and crystalline state different phases are all had during reversible transition under the thickness, it is corresponding to be presented 3
Different resistance values.
2. a kind of multi-level phase change V according to claim 12O5The preparation method of thin-film material, which is characterized in that the system
Preparation Method is reactive deposition method, reacts and be deposited on substrate using what vanadium and oxygen occurred for magnetron sputtering, by control Ar gas with
O2Gas flow and sputtering pressure generate V2O5, rather than the method for other oxides of vanadium；Specifically includes the following steps:
(1) SiO is cleaned2/ Si (100) substrate；
(2) V is prepared2O5Preparation before film: vanadium target target to be sputtered is installed, magnetron sputtering chamber is vacuumized；Setting is splashed
Penetrate power；Set sputter gas Ar gas and O2Gas gas flow simultaneously adjusts sputtering pressure；
(3) multi-level phase change V is prepared2O5Thin-film material:
A) space base support is rotated into vanadium target target position, opens the AC power source on target, sputtering time is set 1., to the target table of vanadium target
Face is sputtered to clean target material surface；
B) after the completion of target surface cleaning, the shutter above vanadium target target position is closed；Cleaned substrate in step (1) is placed in
In space base support, substrate to be sputtered is rotated to above vanadium target target position, shutter above vanadium target target position is opened, according to splashing for setting
2. and sputter rate it penetrates the time, starts sputtering and generate V2O5Film.
3. a kind of multi-level phase change V according to claim 22O5The preparation method of film, which is characterized in that institute in step (2)
Stating sputtering power is 100~200W, sputtering pressure 0.20Pa.
4. a kind of multi-level phase change V according to claim 32O5The preparation method of film, which is characterized in that institute in step (2)
Stating sputtering power is 150W.
5. a kind of multi-level phase change V according to claim 22O5The preparation method of film, which is characterized in that the vanadium target
The purity of atomic percent is greater than 99.999%；Sputter gas described in step (2) is Ar gas and O2The mixed gas of gas, it is described
Percent by volume >=99.999% of Ar gas, gas flow are 60~80sccm；The O2The percent by volume of gas >=
99.999%, gas flow is 5~15sccm.
6. a kind of multi-level phase change V according to claim 52O5The preparation method of film, which is characterized in that the Ar gas
Gas flow is 70sccm, O2The gas flow of gas is 10sccm.
7. a kind of multi-level phase change V according to claim 22O5The preparation method of film, which is characterized in that when the sputtering
Between be 1. 200s, 2. the sputtering time is 500~3750s, sputter rate is 2~15s/nm.
8. a kind of multi-level phase change V according to claim 72O5The preparation method of film, which is characterized in that when the sputtering
Between 2. be 1000~2000s, sputter rate be 5~10s/nm.
9. a kind of multi-level phase change V described in any item according to claim 1~82O5Thin-film material is in multi-level phase change memory
Using.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110456525A (en) * | 2019-07-11 | 2019-11-15 | 中国科学院上海光学精密机械研究所 | A kind of membrane structure with Multi-regulation function |
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| CN1800440A (en) * | 2005-04-30 | 2006-07-12 | 江苏工业学院 | Preparation method of polycrystalline vanadium dioxide film with room temperature resistance temperature coefficient higher than 10%K |
| CN102130295A (en) * | 2010-12-17 | 2011-07-20 | 天津理工大学 | Resistive random access memory based on vanadium oxide film and preparation method thereof |
| CN106992251A (en) * | 2017-05-12 | 2017-07-28 | 华中科技大学 | One kind is based on VOxThe phase-change memory cell of gate tube |
| CN206834207U (en) * | 2017-05-12 | 2018-01-02 | 华中科技大学 | A kind of phase-change memory cell based on VOx gate tubes |
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- 2019-02-27 CN CN201910146169.0A patent/CN109935687B/en active Active
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| CN1800440A (en) * | 2005-04-30 | 2006-07-12 | 江苏工业学院 | Preparation method of polycrystalline vanadium dioxide film with room temperature resistance temperature coefficient higher than 10%K |
| CN102130295A (en) * | 2010-12-17 | 2011-07-20 | 天津理工大学 | Resistive random access memory based on vanadium oxide film and preparation method thereof |
| CN106992251A (en) * | 2017-05-12 | 2017-07-28 | 华中科技大学 | One kind is based on VOxThe phase-change memory cell of gate tube |
| CN206834207U (en) * | 2017-05-12 | 2018-01-02 | 华中科技大学 | A kind of phase-change memory cell based on VOx gate tubes |
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| CN110456525A (en) * | 2019-07-11 | 2019-11-15 | 中国科学院上海光学精密机械研究所 | A kind of membrane structure with Multi-regulation function |
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