CN105006519A - High-speed low-power-consumption Sn18Sb82-SnSe2 nanometer composite multilayer film, preparation method and application thereof - Google Patents

High-speed low-power-consumption Sn18Sb82-SnSe2 nanometer composite multilayer film, preparation method and application thereof Download PDF

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CN105006519A
CN105006519A CN201510413009.XA CN201510413009A CN105006519A CN 105006519 A CN105006519 A CN 105006519A CN 201510413009 A CN201510413009 A CN 201510413009A CN 105006519 A CN105006519 A CN 105006519A
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snse
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CN105006519B (en
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翟继卫
刘瑞蕊
沈波
何子芳
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Tongji University
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Abstract

The invention relates to a high-speed low-power-consumption Sn18Sb82-SnSe2 nanometer composite multilayer film, a preparation method and an application thereof. The high-speed low-power-consumption Sn18Sb82-SnSe2 nanometer composite multilayer film has a superlattice type structure which is obtained through alternatively arranging Sn18Sb82 films and SnSe2 films. The thickness of each Sn18Sb82 film is 2-8nm. The thickness of each SnSe2 film is 10nm. The total thickness of the composite multilayer film is 40-60nm. The Sn18Sb82 and the SnSe2 are used as sputtering target materials. In an Ar gas atmosphere, alternative sputtering is performed on a SiO2/Si100 substrate. Compared with the prior art, the high-speed low-power-consumption Sn18Sb82-SnSe2 nanometer composite multilayer film is advantageous in that the operation phase transition speed of the PCRAM device is improved from 100ns of GST to 5ns; the phase transition temperature is increased from about 160 DEG C to 200 DEG C; and crystallization activation energy is increased from 2.28eV to 3.61eV.

Description

Tin antimony-Xi selenium nano composite multiple layer the film of high-speed low-power-consumption and Synthesis and applications
Technical field
The present invention relates to technical field of microelectronic material, especially relate to a kind of preparation method and application with the tin antimony-Xi selenium nano composite multiple layer film of high-speed low-power-consumption.
Background technology
In the 21st century of information globalization, memory, as the core component of electronic equipment, causes the great attention of people.And phase transition storage because of have memory cell size little, have extended cycle life, good stability, low in energy consumption and embed the advantages such as function is strong be regarded as one of most promising three large electric resistance changing materials (G.I.Meijer:Science, 2008, p.1625).
Current Ge-Sb-Te system because having extraordinary composite characteristic, and is widely used in phase change memory field.But its lower phase transition temperature, phase velocity and stability but limit it and further apply.For this reason, researchers are devoted to the New-type phase change storage medium researching and developing a kind of alternative Ge-Sb-Te system.Research finds that rich Sb based phase-change material can rely on the precipitation of Sb element, is increased in forming core site, thus the phase velocity of raising material (Y.F.Hu and X.Y.Feng:Scripta, 2014, p.4).Meanwhile, research finds that Sn-Se base film has comparatively faster phase velocity because having Sn element; There is Se element can be with material to widen and improve its crystalline state and amorphous state resistance; By means of bond energy larger between Sn-Se, improve Sn-Se film stability (W.Welnic and A.Pamungkas:Nature Materials, 2006, p.56).And H.X.Yang etc. also point out, the film differed greatly by two kinds of phase-change characteristics carries out compound, both features effectively can be combined, thus obtain the good phase-change storage material of combination property (H.X.Yang and C.T.Chong:Applied Physics Letters, 2009, p 203110).
Chinese patent CN103762308A discloses Polymorphic gallium antimony-stannic selenide multi-layer nano composite phase-change material and Synthesis and applications thereof, is Ga 30sb 70/ SnSe 2multilayer nanocomposite phase transition film, by SnSe 2film and Ga 30sb 70film is alternately arranged into multi-layer film structure, wherein SnSe 2the thickness of film is 5 ~ 35nm, Ga 30sb 70the thickness of film is 5 ~ 35nm; Ga 30sb 70/ SnSe 2the gross thickness of multilayer nanocomposite phase transition film is 50-70nm, adopts magnetron sputtering method to prepare, can be applied in the high-density phase-change memory with polymorphic performance.But Ga used in the present invention 30sb 70and SnSe 2material all has higher amorphous state resistance thus have impact on the operating characteristics of its device, causes it and can only complete SET process (crystallization) in device detection, namely can not complete the complete procedure of Information Access simultaneously.And Sn used in the present invention 18sb 82because there is the generation that lower amorphous state resistance can avoid this phenomenon very well, with SnSe 2the thin-film material that compound obtains has good device being operative.In addition, the device operation speed in this invention is 1000ns, differs greatly compared with the 100ns of GST.And device operation speed of the present invention can rise to 5ns.
Summary of the invention
Object of the present invention be exactly in order to overcome above-mentioned prior art exist defect and utilize the difference of resistance and the difference of crystallization temperature before and after two kinds of phase-change material crystallization, by the method for compound, the performance of bi-material is carried out comprehensively, obtaining the Sn of high phase velocity high stability low-power consumption 18sb 82-SnSe 2multilayer nanocomposite phase transition film material.
Foundation of the present invention is mainly the phase velocity being improved phase-change thin film by rich Sb sill, and is kept the phase velocity of the material of film by the element S n contained in target.In addition according to having larger to be with and combination larger between Sn-Se can improve the stability of thin-film material containing the material of Se element, the mode eventually through compound obtains characteristics such as simultaneously having the power consumption of phase velocity, suitable crystallization temperature, higher stability and lower PCRAM operation faster.
Object of the present invention can be achieved through the following technical solutions:
Tin antimony-Xi selenium nano composite multiple layer the film of high-speed low-power-consumption, it is characterized in that, this film is Sn 18sb 82film and SnSe 2film is alternately arranged and forms class superlattice structure,
Described Sn 18sb 82film thickness is 2-8nm, described SnSe 2the thickness of film is 10nm, and the gross thickness of complex multi layer films is 40-60nm.
Preferably, described Sn 18sb 82-SnSe 2a=2nm, 4nm in nano composite multiple layer film; B=4.
Optimum, described Sn 18sb 82-SnSe 2the chemical composition of nano composite multiple layer film is [Sn 18sb 82(2nm)-SnSe 2(10nm)] 4.
Sn of the present invention 18sb 82-SnSe 2nano composite multiple layer thin-film material has phase velocity and stability faster compared to traditional phase-change storage material.And compared to individual layer Sn 18sb 82thin-film material has higher phase transition temperature and stability; Compared to individual layer SnSe 2thin-film material has lower amorphous state resistance, is conducive to the operability of PCRAM device.
Sn of the present invention 18sb 82-SnSe 2nano composite multiple layer film adopts magnetically controlled sputter method to obtain, at SiO 2on/Si (100) substrate, with Sn 18sb 82and SnSe 2for sputtering target material, take Ar as sputter gas, alternating deposit Sn 18sb 82and SnSe 2film.
Preferably, described Sn 18sb 82and SnSe 2target purity is all more than 99.999%, and vacuum degree is higher than 2 × 10 -4pa.
Preferably, described Sn 18sb 82and SnSe 2target all adopts DC power supply, and sputtering power is 15-25W, and optimum is 20W.
Preferably, the gas flow of described Ar gas is 25-35SCCM, and optimum is 30SCCM; Sputtering pressure is 0.15-0.25Pa, and optimum is 0.2Pa.
Described each layer film thickness is by Sn 18sb 82and SnSe 2the sputtering time of target controls.
Sn of the present invention 18sb 82-SnSe 2the preparation method of nano composite multiple layer film, specifically comprises the following steps:
1. by SiO 2/ Si (100) substrate is cut into suitable size, and in absolute alcohol, carry out Ultrasonic Cleaning removal dust, organic-inorganic impurity;
2. in sputter cavity, install hired target and substrate to be sputtered, shut cavity, chamber internal gas pressure is extracted into 2 × 10 -4below Pa, the parameters such as setting power, gas flow and sputtering pressure;
3.Sn 18sb 82-SnSe 2the preparation of nano composite multiple layer film
A substrate is rotated to Sn by () 18sb 82target position, opens DC power supply, by setting sputter thickness certain hour, after, close Sn 18sb 82dC power supply;
B substrate is rotated to SnSe by () again 2target position, opens SnSe 2dC power supply, after, close SnSe 2dC power supply.
C () repeats above-mentioned steps (a) and (b), until obtain film desired thickness.
This tin antimony-Xi selenium nano composite multiple layer film is applied in phase transition storage.
The Sn that the present invention prepares 18sb 82-SnSe 2nano composite multiple layer film is compared with conventional phase change material, and PCRAM device operation phase velocity rises to 5ns by the 100ns of GST; Phase transition temperature brings up to about 200 DEG C by about 160 DEG C; Crystalline active energy brings up to 3.61eV by 2.28eV; Ten annual data hold facilities rise to 112 DEG C by 85 DEG C; And crystalline resistance improves 10 3above, also illustrate that PCRAM operates the reduction greatly of power consumption.Its faster phase velocity mainly come from Sb 18sn 82layer defines more Sb precipitated phase, and Sb compares strong metallicity, reduces the amorphous state resistance of material, improves the device being operative of material.In addition, research shows SnSe 2there is chain structure and stronger Sn-Se key can be formed, thus enhancing the stability of material; SnSe 2larger band structure adds the crystalline resistance of this complex multi layer films, thus reduces the power consumption of material.
Accompanying drawing explanation
Fig. 1 is [Sn 18sb 82(a)-SnSe 2(10nm)] bthe relation curve of nano composite multiple layer film resistance and temperature under different heating rate and matching gained activation energy thereof.
Fig. 2 is [Sn 18sb 82(2nm)-SnSe 2(10nm)] 4nano composite multiple layer film out-of-service time at different temperatures, and matching the data obtained hold facility and Avrami index n.
Fig. 3 is [Sn 18sb 82(2nm)-SnSe 2(10nm)] 4nano composite multiple layer film reflectivity change curve before and after crystallization under picopulse effect.
Fig. 4 is [Sn 18sb 82(2nm)-SnSe 2(10nm)] 4i-V, R-V characteristic curve of the PCRAM device cell of nano composite multiple layer film.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Illustrate embodiments of the present invention below by way of particular instance, those skilled in the art can by content described in this specification convenient understand phase-change material of the present invention other a little and characteristic.The present invention can also be implemented by other different modes or be applied, and its every details also can based on different viewpoints and purposes, carries out various modification or change not deviating under thought of the present invention.
Embodiment 1
Sn prepared by this example 18sb 82-SnSe 2nano composite multiple layer film, gross thickness is about 50nm, and general structure is [Sn 18sb 82(a)-SnSe 2(10nm)] b, concrete structure has:
[Sn 18Sb 82(2nm)-SnSe 2(10nm)] 4，[Sn 18Sb 82(4nm)-SnSe 2(10nm)] 4,
[Sn 18Sb 82(6nm)-SnSe 2(10nm)] 3，[Sn 18Sb 82(8nm)-SnSe 2(10nm)] 3。
1. clean SiO 2/ Si (100) substrate:
A substrate is placed in deionized water by (), with ultrasonic cleaning 20 minutes, remove substrate surface dust granule;
B substrate is placed in absolute ethyl alcohol by (), with ultrasonic cleaning 20 minutes, remove substrate surface dust granule and inorganic impurity;
C () again by step (b) in triplicate;
D () takes out substrate, do with pure Ar air-blowing, stand-by.
2. sputter [Sn 18sb 82(a)-SnSe 2(10nm)] bthe early-stage preparations of nano composite multiple layer film:
A () is by Sn 18sb 82and SnSe 2target is placed on 1 respectively, on No. 2 target position, and is fixed on sample stage by the substrate handled well, closes sealed vacuum room;
B () opens mechanical pump, and by molecular pump preheating 5min, when vacuum reaches 5Pa or be following, start molecular pump, be evacuated to 2 × 10 -4below Pa.
(c) setting Sn 18sb 82and SnSe 2the direct current power of target is 20W.
D () leads to argon gas (sputter gas), flow is set to 30SCCM, and sputtering pressure is 0.2Pa.
3. carry out plated film by plated film monitoring program, required sputtering thickness, can be changed by sputtering time, wherein Sn 18sb 82the sputtering rate of target is 20s/7nm, SnSe 2the sputtering rate of target is 0.9s/nm:
A substrate is rotated to Sn by () 18sb 82target position, opens DC power supply, by setting sputter thickness certain hour, after, close Sn 18sb 82dC power supply;
B substrate is rotated to SnSe by () 2target position, opens SnSe 2dC power supply;
C () repeats above-mentioned (a), (b) two step, until film thickness reaches about 50nm.
Comparative example 1
The individual layer Sn prepared in this comparative example 18sb 82phase-change thin film, gross thickness is 50nm.
1. clean SiO 2/ Si (100) substrate:
A substrate is placed in deionized water by (), with ultrasonic cleaning 20 minutes, remove substrate surface dust granule;
B substrate is placed in absolute ethyl alcohol by (), with ultrasonic cleaning 20 minutes, remove substrate surface dust granule and inorganic impurity;
C () again by step (b) in triplicate;
D () takes out substrate, do with pure Ar air-blowing, stand-by.
2. sputtering for Sn 18sb 82film early-stage preparations:
A () is by Sn 18sb 82target is placed on No. 1 target position, and is fixed on sample stage by the substrate handled well, closes sealed vacuum room;
B () opens mechanical pump, and by molecular pump preheating 5min, when vacuum reaches 5Pa or be following, start molecular pump, be evacuated to 2 × 10 -4below Pa.
C () setting direct current power is 20W.
D () leads to argon gas (sputter gas), flow is set to 30SCCM, and sputtering pressure is 0.2Pa.
3. carry out plated film by plated film monitoring program, required sputtering thickness, can be changed by sputtering time, wherein Sn 18sb 82the sputtering rate of target is 7nm/20s: substrate is rotated to Sn 18sb 82target position, opens DC power supply, by setting sputter thickness certain hour, after, close Sn 18sb 82dC power supply.
Comparative example 2
The individual layer SnSe prepared in this comparative example 2phase-change thin film, gross thickness is 50nm.
1. clean SiO 2/ Si (100) substrate:
A substrate is placed in deionized water by (), with ultrasonic cleaning 20 minutes, remove substrate surface dust granule;
B substrate is placed in absolute ethyl alcohol by (), with ultrasonic cleaning 20 minutes, remove substrate surface dust granule and inorganic impurity;
C () again by step (b) in triplicate;
D () takes out substrate, do with pure Ar air-blowing, stand-by.
2. sputtering for Sn Se 2film early-stage preparations:
A () is by SnSe 2target is placed on No. 1 target position respectively, and is fixed on sample stage by the substrate handled well, closes sealed vacuum room;
B () opens mechanical pump, and by molecular pump preheating 5min, when vacuum reaches 5Pa or be following, start molecular pump, be evacuated to 2 × 10 -4below Pa.
C () setting direct current power is 20W.
D () leads to argon gas (sputter gas), flow is set to 30SCCM, and sputtering pressure is 0.2Pa.
3. carry out plated film by plated film monitoring program, required sputtering thickness, can be changed by sputtering time, wherein SnSe 2the sputtering rate of target is 0.9nm/s: substrate is rotated to SnSe 2target position, opens DC power supply, by setting sputter thickness certain hour, after, close SnSe 2dC power supply.
To [the Sn described in example 1 18sb 82(a)-SnSe 2(10nm)] bphase-change thin film is tested, and obtains the variation relation curve of resistance and temperature under different heating rate, and carries out matching by the non-isothermal activation energy of Kissinger formula to non-crystaline amorphous metal, as shown in Figure 1; [the Sn best to performance 18sb 82(2nm)-SnSe 2(10nm)] 4nano composite multiple layer film carries out Isothermal Crystallization Kinetics test, the data holding ability obtaining thin-film material and the Avrami index n obtained by Johnson-Mehl-Avrami (JMA) equation model, as shown in Figure 2; To above-mentioned [Sn 18sb 82(2nm)-SnSe 2(10nm)] 4nano composite multiple layer film carries out device detection, obtains I-V and R-V indicatrix, as shown in Figure 3.
The testing result of above-mentioned Fig. 1-4 is as follows:
Fig. 1 is [Sn of the present invention 18sb 82(a)-SnSe 2(10nm)] bnano composite multiple layer film is respectively 10 DEG C/min, 20 DEG C/min, electrical resistance temperature variation curve under 30 DEG C/min and 40 DEG C/min at heating rate, and the crystalline active energy that matching obtains.As can be seen from the figure, [Sn 18sb 82(a)-SnSe 2(10nm)] bnano composite multiple layer film Sn 18sb 82thickness increased by 2nm and be followed successively by 151 DEG C, 153 DEG C, 170 DEG C and 183 DEG C to its phase transition temperature of 8nm; Activation energy is followed successively by 3.61eV, 2.52eV, 2.42eV and 2.26eV.And [Sn 18sb 82(2nm)-SnSe 2(10nm)] 4phase transition temperature and stability are put up the best performance.
Fig. 2 is crystallization temperature and the best [Sn of stability in the present invention 18sb 82(2nm)-SnSe 2(10nm)] 4nano composite multiple layer film out-of-service time at different temperatures and matching gained ten annual data hold facility and Avrami index n.As can be seen from the figure the out-of-service time of the higher film of temperature is shorter, and ten annual data hold facilities of matching gained are 112 DEG C, far above traditional material Ge 2sb 2te 5(GST) 85 DEG C; The mean value of gained Avrami index n is 1.05, illustrates that this film is a growth pattern of nucleation type, also predictive of its phase velocity faster.
Fig. 3 is the [Sn in the present invention 18sb 82(2nm)-SnSe 2(10nm)] 4nano composite multiple layer film reflectivity change curve before and after crystallization under picopulse effect.Can find out that its SET time be 5.9ns, RESET process is 6.2ns, also higher than traditional material GST.
Fig. 4 is [Sn 18sb 82(2nm)-SnSe 2(10nm)] 4i-V, R-V characteristic curve of the PCRAM device cell of nano composite multiple layer film.Can see that its threshold voltage is 2.46V by I-V, far below the threshold voltage (4.18V) of GST.In addition, [Sn as can be seen from R-V curve 18sb 82(2nm)-SnSe 2(10nm)] 4nano composite multiple layer film is under 5ns and 10ns impulse action, all can form complete SET and RESET process, its SET voltage is 2.5V (5ns) and 1.6V (10ns), and RESET voltage is 3.4 (5ns) and 2.5V (10ns), and [Sn is described 18sb 82(2nm)-SnSe 2(10nm)] 4film comparatively GST (100ns) has device operation speed faster; In addition according to publicity P=V 2/ R is known, and (after crystallization, resistance is 10 4-10 5Ω), illustrate that this material has low-down phase change memory power consumption.
Known [the Sn of complex chart 1-4 18sb 82(a)-SnSe 2(10nm)] bnano composite multiple layer film has good phase transition temperature and stability.Wherein [Sn 18sb 82(2nm)-SnSe 2(10nm)] 4film also has phase velocity faster, the features such as lower power consumption, describes its good composite characteristic.
Above-described embodiment is exemplary illustration principle of the present invention and effect thereof only, but not for limiting the present invention.Any person skilled in the art scholar all without prejudice under spirit of the present invention and category, can modify above-described embodiment or changes.Therefore, such as have in art and usually know that the knowledgeable modifies or changes not departing from all equivalences completed under the present invention says the spirit of announcement and technological thought, throw away and claim of the present invention should be had to contain.

Claims (8)

1. the tin antimony-Xi selenium nano composite multiple layer film of high-speed low-power-consumption, it is characterized in that, this film is Sn 18sb 82film and SnSe 2film is alternately arranged and forms class superlattice structure,
Described Sn 18sb 82film thickness is 2-8nm, described SnSe 2the thickness of film is 10nm, and the gross thickness of complex multi layer films is 40-60nm.
2. the tin antimony-Xi selenium nano composite multiple layer film of high-speed low-power-consumption according to claim 1, it is characterized in that, the chemical composition of nano composite multiple layer film is [Sn 18sb 82(a)-SnSe 2(10nm)] b, wherein a represents individual layer Sn 18sb 82the thickness of film, b represents Sn 18sb 82-SnSe 2the periodicity of nano composite multiple layer film.
3. the tin antimony-Xi selenium nano composite multiple layer film of high-speed low-power-consumption according to claim 2, it is characterized in that, periodicity b is 3 or 4.
4. the tin antimony-Xi selenium nano composite multiple layer film of high-speed low-power-consumption according to claim 1, is characterized in that, Sn 18sb 82film thickness is 2nm, 4nm, 6nm or 8nm.
5. the preparation method of the tin antimony-Xi selenium nano composite multiple layer film of high-speed low-power-consumption as claimed in claim 1, is characterized in that, adopts the method for magnetron sputtering, with Sn 18sb 82and SnSe 2for sputtering target material, under the environment of Ar gas, at SiO 2/ Si (100) substrate carries out alternating sputtering, prepares tin antimony-Xi selenium nano composite multiple layer film.
6. the preparation method of the tin antimony-Xi selenium nano composite multiple layer film of high-speed low-power-consumption according to claim 5, is characterized in that, Sn 18sb 82and SnSe 2all more than 99.999% (atomic percent), vacuum degree is higher than 2 × 10 for the purity of target 4pa, Ar gas purity (percent by volume) more than 99.999%.
7. the preparation method of the tin antimony-Xi selenium nano composite multiple layer film of high-speed low-power-consumption according to claim 5, is characterized in that, Sn 18sb 82and SnSe 2adopt DC power supply during target as sputter, sputtering power is 15-25W; The gas flow of Ar gas is 25-35SCCM; Sputtering pressure is 0.15-0.25Pa.
8. the application of the tin antimony-Xi selenium nano composite multiple layer film of high-speed low-power-consumption as claimed in claim 1, it is characterized in that, this tin antimony-Xi selenium nano composite multiple layer film is applied in phase transition storage.
CN201510413009.XA 2015-07-14 2015-07-14 The tin antimony of high-speed low-power-consumption-tin selenium nano composite multiple layer film and preparation and application Expired - Fee Related CN105006519B (en)

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CN109860388A (en) * 2019-01-09 2019-06-07 江苏理工学院 Multi-layer phase change film and preparation method and application
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