CN106410025A - Oxygen-doped Sb nanometer phase change thin-film materials and preparation method thereof and application thereof - Google Patents
Oxygen-doped Sb nanometer phase change thin-film materials and preparation method thereof and application thereof Download PDFInfo
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N70/00—Solid-state devices without a potential-jump barrier or surface barrier, and specially adapted for rectifying, amplifying, oscillating or switching
- H10N70/801—Constructional details of multistable switching devices
- H10N70/881—Switching materials
- H10N70/883—Oxides or nitrides
- H10N70/8833—Binary metal oxides, e.g. TaOx
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N70/00—Solid-state devices without a potential-jump barrier or surface barrier, and specially adapted for rectifying, amplifying, oscillating or switching
- H10N70/011—Manufacture or treatment of multistable switching devices
- H10N70/021—Formation of the switching material, e.g. layer deposition
- H10N70/026—Formation of the switching material, e.g. layer deposition by physical vapor deposition, e.g. sputtering
Abstract
The present invention belongs to the semiconductor material field, and discloses the oxygen-doped Sb nanometer phase change thin-film materials. The chemical composition general formula is expressed by SbOx, wherein the Sb represents the Sb element, the O represents the nitrogen atom, the x represents different oxygen doping amount marks, and x=1,2,3 or 4. A magnetron sputtering method is employed for preparation, the substrate employs SiO2/Si(100) substrate, the target of sputter is the Sb target, the sputtering gas is high-purity Ar gas and the high-purity O2 gas, and the total flow of the argon and the oxygen is maintained to 30 sccm in the sputtering process. The oxygen-doped Sb materials can solve the defects and deficiencies of the pure Sb materials. Different oxygen atoms are doped to allow the Sb crystallization temperature to be obviously improved, the data maintenance capacity is enhanced, and the stability is improved. The RESET power consumption is reduced while the crystalline state resistance is improved.
Description
Technical field
The present invention relates to a kind of semi-conducting material of microelectronics technology and in particular to a kind of for phase transition storage
Sb oxide nano film material and its preparation and application.
Background technology
Phase transition storage (PCRAM) core the most is phase-change material based on chalcogen compound, this phase-change material
It is respectively provided with low resistance and high resistance in crystalline state and amorphous state.By the use of the obvious resistance value of gap as " 0 " of data storage
And one state, rely on the joule thermal induction that electric pulse produces to realize repeating between high-impedance state and low resistance state and change, letter can be reached
The purpose of breath storage.Due to advantages such as the unit size of PCRAM chip is little, storage speed is fast, operating voltage is low, small power consumptions, with
Semiconductor process technique and develop into nanometer scale so that the technical advantage of PCRAM is more and more substantially it is considered to be most potential
Non-volatility memorizer of future generation (Song Zhitang etc., nano-composite phase-changing material, preparation method and its method for optimizing authorize specially
Profit number 2010101634769).
Ge2Sb2Te5It is the phase-change material of current most study, but Ge2Sb2Te5The heat stability of material is not high, crystallization
Temperature only has 160 DEG C about, and the temperature that data keeps 10 years is only had 85 DEG C by it.Additionally, Ge2Sb2Te5The transformation time of material
Longer it is impossible to meet the design requirement of following high-speed PCR AM.Therefore, get more and more and there is more high thermal stability, faster change speed
The phase-change material of degree is continuously developed out.The phase-change material of rich Sb due to having phase velocity faster, by more and more
Attention.In recent years, (the Sun Zhimei that is reported successively such as phase-change material Sb-Te, Sb-Se, Si-Sb and Ge-Sb of rich Sb
Deng, a kind of preparation method of Ge-Sb-Te ternary phase change material film, granted patent number 2012100588048；Lv Ye just etc., phase
Become storage material and preparation method thereof, there is memorizer of phase-change storage material and preparation method thereof, granted patent number
2010105811885).
By mixing appropriate O atom or N atom in phase-change material, the higher oxide of stability or oxygen can be formed
Compound amorphous particle, is distributed in around phase-change material, on the one hand stops the crystallization of phase-change material, improves the overall heat of phase-change material
Stability；On the other hand, by reducing crystallite dimension, increase number of grain boundaries, thus increasing crystalline resistance, device can be reduced and exist
Power consumption during RESET.Jang etc. have studied in Ge2Sb2Te5Material phase transformation performance after middle incorporation O atom, result
Show that the oxide of the Ge generating can stop growing up of crystal grain, thus improving Ge2Sb2Te5Crystallization temperature (Jang, M.H. etc.,
Applied Physics Letters, 95 (1), 012102,2009).Zhu, M. etc. are in Sb2Mix N atom in Te, not only carry
High Sb2The heat stability of Te, and reduce operation power consumption (Zhu, M. etc., the Journal of of its RESET process
Alloys and Compounds, 509,10105,2011).
Content of the invention
It is an object of the invention to preparing a kind of sb oxide nano thin-film for phase transition storage, provide a kind of simultaneously
The method that phase-change material phase velocity and heat stability can be changed.
Pure metal Sb material itself does not have phase transition performance, because its heat stability is poor, by magnetically controlled sputter method
The Sb material of deposition is crystalline state, therefore cannot meet the technical requirements of phase transition storage.But, Sb material has based on growth
Crystallization Mechanism, this makes its crystallization rate very fast, is very favorable for accelerating the Information Access speed of PCRAM.This
The bright Sb material mixing oxygen preferably resolves the shortcoming and defect of pure Sb material.By mixing different oxygen atoms, make Sb's
Crystallization temperature is significantly improved, and data holding ability is strengthened, thus improves its stability.Simultaneously by crystalline state electricity
The raising of resistance is so that its RESET lower power consumption.Sb material is made to become a kind of high speed, high stability, low-power consumption by mixing oxygen
Phase-change material, thus having preferable market application foreground.
For achieving the above object and other related purposes, the present invention adopts the following technical scheme that：
A kind of Sb nano phase change thin-film material mixing oxygen, its chemical composition formula SbOx represents, wherein Sb represents and do not mix
The material of oxygen, O represents oxygen atom, and x represents and different mixes oxygen amount labelling, x=1,2,3 or 4.Measure through EDS, x=in the present invention
1st, 2,3 and 4 correspond to the oxygen atom percentage mixing respectively for 10.3%, 16.7%, 21.2%and 25.2.%.
Preferably, described x is preferably 2 or 3.Preferably go out two kinds of compositions that x is 2 or 3, it mixes oxygen Sb material heat stability relatively
Good, can respectively data be kept 10 years at 113 DEG C and 127 DEG C respectively, therefore data reliability is preferable.Crystallization temperature is respectively
185 and 194 DEG C, there is phase velocity faster, disclosure satisfy that the requirement of high stability and high speed.
Preferably, the described gross thickness mixing oxygen Sb nano phase change thin-film material is 45-60nm；It is preferably 50nm.
The oxygen Sb nano phase change thin-film material of mixing of the present invention adopts magnetically controlled sputter method to prepare, by radio frequency sputtering deposition
It is passed through argon and oxygen during Sb thin film simultaneously, and be prepared from nanometer scale.
The present invention mixes oxygen Sb nano phase change thin-film material, according to the difference mixing oxygen amount, keeps argon in sputter procedure
Total flow with oxygen is 30sccm, if oxygen flow is y sccm, corresponding argon flow amount is (30-y) sccm.
The above-mentioned SbOx nano phase change thin-film material of the present invention, works as x=1, all show when 2,3,4 obvious amorphous state-
The phase transition process of crystalline state, and its stability is in monotone increasing trend with the increase of x.Pure Sb material does not have in heating process
Significantly sudden change of resistivity process, and it is held in low resistance state, show that its deposited is crystalline state.Phase-change material heat stability
Higher, phase velocity is slower.So, need to consider both variation relations when preferred phase-change material.At this
In bright, work as X>When 4, the phase-change characteristic mixing oxygen Sb material becomes very inconspicuous.
When SbOx nano phase change thin-film material of the present invention adopts magnetically controlled sputter method to prepare, substrate adopts SiO2/
Si (100) substrate, sputtering target material is Sb, and sputter gas are high-purity Ar gas and high-purity O2Gas.
Preferably, the purity of described Sb target is in atomic percent more than 99.999%, background vacuum is not more than 1 ×
10-4Pa.
Preferably, described Sb target all adopts radio-frequency power supply, and sputtering power is 25-35W；Sputtering power is preferably
30W.
Preferably, the purity of described Ar gas is percent by volume more than 99.999%, sputtering pressure is 0.3-0.5Pa；Excellent
Choosing, the total gas flow rate of described argon and oxygen is 30sccm, and sputtering pressure is 0.4Pa.
The thickness of SbOx nano phase change thin film of the present invention can be regulated and controled by sputtering time.
The preparation method of SbOx nano phase change thin-film material of the present invention, specifically includes following steps：
1) clean SiO2/ Si (100) substrate；
2) install sputtering target material；Set sputtering power, set sputtering Ar gas and O2The gas flow of gas and sputtering pressure；
3) room temperature magnetically controlled sputter method is adopted to prepare SbOx nano phase change thin-film material；
A) space base support is rotated to Sb target position, open the radio-frequency power supply on Sb target, according to the sputtering time setting (such as
100s), start Sb target material surface is sputtered, clean Sb target material surface；
After the completion of Sb target position surface cleaning, the radio-frequency power supply being applied is closed on Sb target position, by substrate rotation to be sputtered
To Sb target position, open the radio-frequency power supply on Sb target position, according to the sputtering time setting, start to sputter SbOx thin film；Sputtering finishes
What acquisition was described afterwards mixes oxygen Sb nano phase change thin-film material；
4) repeat step 2) and 3) two steps, change Ar gas and O2The flow proportional of gas, divides on SiO2/Si (100) substrate
Do not prepare SbOx (x=1,2,3,4) nano phase change thin-film material.
What the present invention was above-mentioned mixes oxygen Sb nano phase change thin-film material, can be by the Ar gas in preparation method and O2The gas stream of gas
Amount than controlling the content of the O atom mixed in oxygen Sb nano phase change thin-film material being obtained, other in certain preparation process
Condition is also very important, temperature in such as sputter procedure, air pressure, rotary speed of sample etc., to final obtain mix oxygen Sb
The content size of the O atom in nano phase change thin-film material also plays a role.
The present invention mixes oxygen SbOx nano film material and can be applied to phase transition storage, with traditional phase change film material
Compare and have the advantage that：First, SbOx nano phase change thin-film material has crystallization rate faster, can greatly improve
The storage speed of PCRAM；Secondly, SbOx nano phase change thin-film material there is higher crystallization temperature and activation energy such that it is able to
Greatly improve the stability of PCRAM；Again, compare the Sb thin-film material not mixing oxygen, SbOx nano phase change thin-film material has
Higher amorphous state and crystalline resistance, reduce PCRAM operation power consumption such that it is able to effective.
Brief description
Fig. 1 is SbOx (x=1,2,3 or 4) nano phase change thin-film material and the Sb thin film phase for comparative example 1 of the present invention
Become the In-situ resistance of material and the relation curve of temperature.
Fig. 2 is the right of SbOx (x=1,2,3 or 4) nano phase change thin-film material out-of-service time and the inverse temperature of the present invention
Answer relation curve.
Fig. 3 is the SbO based on the present invention3The cycle fatigue properties curve of the PCRAM device of material.
Specific embodiment
Below by way of specific instantiation, embodiments of the present invention are described, those skilled in the art can be by this specification
Disclosed content understands other advantages and effect of the present invention easily.The present invention can also be by addition different concrete realities
The mode of applying is carried out or applies, and the every details in this specification can also be based on different viewpoints and application, without departing from
Carry out various modifications and changes under the spirit of the present invention.
Embodiment 1
In the present embodiment, the oxygen Sb nano phase change Thin Films of mixing of preparation are embodied as SbO1.
Preparation process is：
1. clean SiO2/Si (100) substrate, cleaning surface, the back side, remove dust granule, organic and inorganic impurity；
A) strong ultrasonic cleaning 3-5 minute, deionized water rinsing in acetone soln；
B) strong ultrasonic cleaning 3-5 minute, deionized water rinsing in ethanol solution, high-purity N 2 dries up surface and the back side；
C) in 120 DEG C of drying in oven steam, about 20 minutes.
2. adopt RF sputtering method to prepare SbO1Prepare before thin film：
A) install Sb sputtering target material, the purity of target all reaches 99.999% (atomic percent), and base vacuum is taken out
To 1 × 10-4Pa；
B) set sputtering power 30W；
C) high-purity Ar and high-purity O are used2As sputter gas (percent by volume all reaches 99.999%), set Ar air-flow
Measure as 29sccm, O2Flow is 1sccm, and sputtering pressure is adjusted to 0.4Pa.
3. adopt magnetically controlled sputter method to prepare SbO1Nano phase change thin-film material：
A) space base support is rotated to Sb target position, the radio-frequency power supply being applied is opened on Sb target, according to the sputtering time setting
(100s), start Sb target is sputtered, clean Sb target material surface；
B), after the completion of Sb target material surface cleaning, the radio-frequency power supply being applied is closed on Sb target, substrate to be sputtered is rotated to
Sb target position, opens Sb target position radio-frequency power supply, according to the sputtering time setting, starts sputtering and mixes oxygen Sb thin film.
The final SbO obtaining1Film thickness is 50nm, and film thickness is controlled by sputtering time, SbO1Sputter rate
For 2.5s/nm.
Embodiment 2
Prepare the SbOx nano phase change thin-film material of the present embodiment, its concrete structure is respectively SbO2And SbO3And SbO4, and
Described SbO2And SbO3And SbO4The thickness of nano phase change thin-film material is 50nm.
Above-mentioned SbO2And SbO3And SbO4The preparation method of nano phase change thin-film material is identical with example 1, simply prepares SbO2
The Ar throughput that nano phase change thin-film material sets is as 28sccm, O2Flow is 2sccm；Preparation SbO3Nano phase change thin-film material
The Ar throughput setting is as 27sccm, O2Flow is 3sccm；Preparation SbO4The Ar throughput that nano phase change thin-film material sets as
26sccm, O2Flow is 4sccm.
Comparative example 1
Monolayer Sb phase change film material is prepared, representation is Sb, thickness 50nm in this comparative example.
Preparation process is：
1. clean SiO2/ Si (100) substrate, cleaning surface, the back side, remove dust granule, organic and inorganic impurity；
A) strong ultrasonic cleaning 3-5 minute, deionized water rinsing in acetone soln；
B) strong ultrasonic cleaning 3-5 minute, deionized water rinsing in ethanol solution, high-purity N 2 dries up surface and the back side；
C) in 120 DEG C of drying in oven steam, about 20 minutes.
2. prepare before adopting RF sputtering method preparation Sb thin film：
A) install Sb sputtering target material, the purity of target all reaches 99.999% (atomic percent), and base vacuum is taken out
To 1 × 10-4Pa；
B) set sputtering power 30W；
C) high-purity Ar gas is used as sputter gas (percent by volume reaches 99.999%), set Ar throughput as
30sccm, and sputtering pressure is adjusted to 0.4Pa.
3. adopt magnetically controlled sputter method to prepare Sb nano phase change thin-film material：
A) space base support is rotated to Sb target position, the radio-frequency power supply being applied is opened on Sb target, according to the sputtering time setting
(100s), start Sb target is sputtered, clean Sb target material surface；
B) after the completion of Sb target material surface cleaning, the radio-frequency power supply being applied is closed on Sb target, will rotate to for sputtering substrate
Sb target position, opens Sb target position radio-frequency power supply, according to the sputtering time setting, starts to sputter Sb thin film.
SbO by above-described embodiment 1 and 21、SbO2、SbO3And SbO4Surveyed with the Sb phase change film material of comparative example 1
Examination, obtains the In-situ resistance of each phase change film material and relation curve Fig. 1 of temperature；SbO by above-described embodiment 1 and 21、
SbO2、SbO3And SbO4Phase change film material is tested, and obtains the out-of-service time of each phase change film material and the right of inverse temperature
Answer relation curve Fig. 2.It is prepared for the SbO based on above-described embodiment 23The PCRAM device of thin film, and test its cycle characteristics,
Result is as shown in Figure 3：
Fig. 1 is SbOx (x=1,2,3 or 4) nano phase change thin-film material and the Sb thin-film material for contrast of the present invention
In-situ resistance and temperature relation curve, the heating rate in test process is 10 DEG C/min.Result shows, with annealing temperature
The rising of degree, the resistance of pure Sb thin-film material does not change significantly, and shows that it has occurred and that crystalline polamer in deposited.
Additionally, all at low temperature oxygen thin film of mixing are in high-resistance amorphous state.With the continuous rising of temperature, film resistor slowly drops
Low, when reaching its phase transition temperature, film resistor reduces rapidly, substantially keeps this resistance constant, show thin after reaching a certain value
Film there occurs by the transformation of amorphous state to crystalline state.Test result shows, with the increase mixing oxygen amount, the crystallization temperature of thin film gradually carries
Height, SbO1Crystallization temperature be 160 DEG C, SbO2、SbO3And SbO4Crystallization temperature be respectively 185,194 and 205 DEG C, show phase
The heat stability of thinning membrane material is enhanced.Meanwhile, the crystalline resistance of phase change film material by do not mix during oxygen 201
Ω increases SbO4634 Ω, thus contribute to reduce RESET process power consumption.
Fig. 2 is the right of the out-of-service time of SbOx (x=1,2,3,4) nano phase change thin-film material and the inverse temperature of the present invention
Answer relation curve.According to one of unified judgment criteria in the industry, corresponding temperature when being kept data 10 years using phase-change material
To pass judgment on the data holding ability of material.As can be seen that the present invention's mixes oxygen Sb thin film with the raising mixing oxygen amount, data keeps
Power has and dramatically increases, i.e. SbO1、SbO2、SbO3And SbO4The temperature that data keeps 10 years is respectively 95,113 by phase-change thin film,
127 and 143 DEG C.That is, the SbOx (x=1,2,3,4) of the present invention has the data more excellent than traditional pure Sb thin-film material
Holding capacity.
In order to verify the practicality of the phase-change material of the present invention, it is prepared for the SbO based on embodiments of the invention3Thin film
PCRAM device, and test its cycle fatigue properties.Fig. 3 result shows, under the induction of current impulse, the resistance of device exists
Constantly switch between high resistant and low-resistance, the difference of binary states resistance more than two orders of magnitude, thus ensure that the effectiveness of information Store.
Secondly, the cycle-index of this device has reached 3.3 × 105, show that this material has preferable reliability, meet functional need.
Above-described embodiment only principle of the illustrative present invention and its effect, not for the restriction present invention.Any ripe
The personage knowing this technology all can carry out modifications and changes without prejudice under the spirit and the scope of the present invention to above-described embodiment.Cause
This, those of ordinary skill in the art is complete with institute under technological thought without departing from disclosed spirit such as
All equivalent modifications becoming or change, must be covered by the claim of the present invention.
Claims (10)
1. a kind of Sb nano phase change thin-film material mixing oxygen it is characterised in that：Its chemical composition formula represents for SbOx, wherein Sb
Represent antimony element, O represents nitrogen-atoms, x represents and different mixes oxygen amount labelling, x=1,2,3 or 4；Measure through EDS, mix during x=1
Nitrogen percent be that during 10.3%, x=2, the nitrogen percent that mixes is 16.7%；The nitrogen-atoms hundred mixing during x=3
Divide ratio for 21.2%；The nitrogen percent mixing during x=4 is 25.2%.
2. a kind of Sb nano phase change thin-film material mixing oxygen according to claim 1 it is characterised in that：Described x=2 or 3.
3. a kind of Sb nano phase change thin-film material mixing oxygen according to claim 1 it is characterised in that：The described Sb mixing oxygen
Nano phase change thin-film material thickness is 45-65nm.
4. a kind of Sb nano phase change thin-film material mixing oxygen according to claim 1 or 3 it is characterised in that：Described mix oxygen
Sb nano phase change thin-film material thickness be 50nm.
5. the preparation method of a kind of Sb nano phase change thin-film material mixing oxygen described in a kind of claim 1, using magnetron sputtering
Prepared by method, substrate adopts SiO2/ Si (100) substrate, sputtering target material is Sb target, and sputter gas are high-purity Ar gas and high-purity O2
Gas, keeps Ar gas and O in sputter procedure2Total flow be 30sccm；It is characterized in that：Specifically include following steps：
1) clean SiO2/ Si (100) substrate；
2) install sputtering target material；Set sputtering power, set sputtering Ar gas and O2The gas flow of gas and sputtering pressure；
3) room temperature magnetically controlled sputter method is adopted to prepare SbOx nano phase change thin-film material, including step a) and step b)：
A) space base support is rotated to Sb target position, open the radio-frequency power supply on Sb target position, the sputtering time 100～200s of setting, open
Begin Sb target material surface is sputtered, clean Sb target material surface；
B), after the completion of Sb target position surface cleaning, the radio-frequency power supply being applied is closed on Sb target position, substrate to be sputtered is rotated to
Sb target position, opens the radio-frequency power supply on Sb target position, starts to sputter SbOx thin film；Sputtering obtains the described Sb mixing oxygen after finishing and receives
Rice phase change film material.
6. a kind of Sb nano phase change thin-film material mixing oxygen according to claim 5 preparation method it is characterised in that：Sb
With atomic percentage more than 99.999%, background vacuum is not more than 1 × 10 to the purity of target-4Pa；Described Sb target
Using radio-frequency power supply, sputtering power is 25-35W.
7. a kind of Sb nano phase change thin-film material mixing oxygen according to claim 6 preparation method it is characterised in that：Institute
The Sb target stated adopts radio-frequency power supply, and sputtering power is 30W.
8. a kind of Sb nano phase change thin-film material mixing oxygen according to claim 5 preparation method it is characterised in that：Institute
State the purity of Ar gas with volume percentage more than 99.999%, sputtering pressure is 0.3-0.5Pa.
9. a kind of Sb nano phase change thin-film material mixing oxygen according to claim 8 preparation method it is characterised in that：Institute
Stating sputtering pressure is 0.4Pa.
10. described in a kind of claim 1, mix the purposes of the Sb nano phase change thin-film material of oxygen it is characterised in that：The described oxygen mixed
Sb nano phase change thin-film material is used for phase transition storage.
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| CN112786782A (en) * | 2021-01-11 | 2021-05-11 | 宁波大学 | Sb-Si for phase change memory3N4Thin film material and preparation method thereof |
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| CN106953006A (en) * | 2017-02-24 | 2017-07-14 | 江苏理工学院 | A kind of SiO2Doping Sb nano phase change thin-film materials and preparation method thereof and purposes |
| CN108365090A (en) * | 2018-01-05 | 2018-08-03 | 江苏理工学院 | A kind of SnSb nano phase change thin-film materials and preparation method thereof for mixing oxygen |
| CN108493337A (en) * | 2018-04-27 | 2018-09-04 | 江苏理工学院 | A kind of lanthanide series cerium dopping star antimony nano phase change material and preparation method thereof |
| CN112786782A (en) * | 2021-01-11 | 2021-05-11 | 宁波大学 | Sb-Si for phase change memory3N4Thin film material and preparation method thereof |
| CN112786782B (en) * | 2021-01-11 | 2022-09-20 | 宁波大学 | Sb-Si for phase change memory 3 N 4 Thin film material and preparation method thereof |
| CN113072915A (en) * | 2021-03-24 | 2021-07-06 | 华中科技大学 | Sb based on oxygen doping2Te3Phase change material, phase change memory and preparation method |
| CN113072915B (en) * | 2021-03-24 | 2022-03-11 | 华中科技大学 | Sb based on oxygen doping2Te3Phase change material, phase change memory and preparation method |
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