CN102386327A - Preparation method of phase-change material - Google Patents

Preparation method of phase-change material Download PDF

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Publication number
CN102386327A
CN102386327A CN2011103769229A CN201110376922A CN102386327A CN 102386327 A CN102386327 A CN 102386327A CN 2011103769229 A CN2011103769229 A CN 2011103769229A CN 201110376922 A CN201110376922 A CN 201110376922A CN 102386327 A CN102386327 A CN 102386327A
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phase
change material
amorphous
annealing
crystallite
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宋志棠
夏梦姣
饶峰
刘波
封松林
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Shanghai Institute of Microsystem and Information Technology of CAS
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Shanghai Institute of Microsystem and Information Technology of CAS
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Abstract

The invention discloses a preparation method of a phase-change material. The method comprises the following steps of: forming an amorphous Si-Sb<x>Te<1-x> material layer on a semiconductor substrate, wherein x is more than or equal to 0.1 but less than or equal to 0.9; performing primary annealing treatment on the Si-Sb<x>Te<1-x> material layer at a temperature higher than the crystallization temperature of the Si-Sb<x>Te<1-x> composite material, to allow phase separation of amorphous Si and crystal Sb<x>Te<1-x>; performing secondary annealing treatment on the phase-split amorphous Si-Sb<x>Te<1-x> composite material in a hydrogen atmosphere after annealing, to transform amorphous Si into microcrystalline Si to form a microcrystalline Si-Sb<x>Te<1-x> composite phase-change material; and performing heating annealing dehydrogenation treatment on the microcrystalline Si-Sb<x>Te<1-x> composite phase-change material. Compared with the prior art, in the prepared microcrystalline Si-Sb<x>Te<1-x> composite phase-change material, the microcrystalline Si has a grain size of 3 nm to about 20 nm, has less defects than amorphous Si, can effectively inhibit oxidation and suppress mutual diffusion of Si and Sb<x>Te<1-x>, and has more sable properties.

Description

The preparation method of phase-change material
Technical field
The present invention relates to a kind of phase change memory technology, especially, more relate to a kind of preparation method who is applied to the phase-change material of phase transition storage.
Background technology
Along with consumer's increasingly high to the data memory requirement, the traditional data memory device can not satisfy the growing needs in market, and novel memory continues to bring out, for example, and phase transition storage, ferroelectric memory, RRAM (resistor random-access storage) etc.Phase transition storage (PC-RAM) is a kind of non-volatile semiconductor memory of rising in recent years, and it is based on Ovshinsky in late 1960s (Phys.Rev.Lett., 21; 1450～1453; 1968) beginning of the seventies (Appl.Phys.Lett., 18,254～257; 1971) phase-change thin film that proposes can be applied to that the conception of phase change memory medium sets up, and is the memory device of a kind of low price, stable performance.Phase transition storage can be made on the silicon wafer substrate, and its critical material is recordable phase change material film, heating electrode material, heat-insulating material and extraction electrode material etc.The basic principle of phase transition storage is to utilize electric impulse signal to act on the device cell; Make phase-change material between amorphous state and polycrystalline attitude, reversible transition take place; Low-resistance when high resistant during through the resolution amorphous state and polycrystalline attitude can realize writing, wipe and read operation of information.
Compare with present existing multiple semiconductor memory technologies, phase transition storage has low-power consumption, high density, anti-irradiation, non-volatile, read at a high speed, high erasable number of times (＞10 13Inferior), device size contractibility (nanoscale); High-low temperature resistant (55 ℃ to 125 ℃), low in energy consumption, anti-vibration, anti-electronic jamming and manufacturing process advantages such as simple (can and prior integrated circuit process be complementary); Be at present by the strongest competitor in the extensively good memory of future generation of industrial quarters, have vast market prospect.
Phase transition storage (PC-RAM) is storage medium with the chalcogenide compound, and in the phase transition storage research and development, phase-change material commonly used mainly contains Ge 2Sb 2Te 5, Si 2Sb 2Te 6Deng germanium-antimony-tellurium (Ge-Sb-Te, GST) serial phase-change material series.Particularly, the Joule heat that can utilize electric pulse or light pulse to produce makes phase-change material between amorphous state (high resistant) and crystalline state (low-resistance), reversible transition take place and realizes writing and wiping of data, and reading then of data realizes through the state of measuring resistance.As Granted publication number for CN100590903C Chinese invention patent document illustration a kind of Si-Te-Sb series phase change film material that is used for phase transition storage.
Yet, experiment showed, SiSb xTe 1-xThe phase-change material of series is the mutually compound of amorphous Si and SbTe crystal in crystallization (SET) attitude, owing to amorphous Si 500 ℃ to 600 ℃ still uncrystallizable, and there are many defectives (like room, microvoid hole, dangling bonds etc.) in amorphous state Si, makes SiSb xTe 1-xThe phase-change material of series is unstable, thereby causes the phase transition storage based on said phase-change material on stability and erasable number of times, to show not good enough.
Summary of the invention
The object of the present invention is to provide a kind of crystallite Si-Sb xTe 1-xThe preparation method of composite phase-change material is used for solving prior art Si-Sb xTe 1-xThe phase-change material of series is under the compound situation mutually that is amorphous Si and SbTe crystal, and phase-change material is unstable, makes phase transition storage on stability and erasable number of times, show not good enough problem.
The present invention provides a kind of preparation method of phase-change material, and Semiconductor substrate is provided, and on said Semiconductor substrate, forms amorphous Si-Sb xTe 1-xMaterial layer, wherein 0.1≤x≤0.9; At said amorphous Si-Sb xTe 1-xOn the crystallization temperature of composite material, to said Si-Sb xTe 1-xCarry out annealing process for the first time, feasible amorphous Si and Sb wherein xTe 1-xCrystal forms phase-splitting; Amorphous Si and Sb with annealing back phase-splitting xTe 1-xThe composite material of crystal places nitrogen atmosphere to carry out annealing process for the second time, makes amorphous Si wherein change crystallite Si into to form crystallite Si-Sb xTe 1-xComposite phase-change material; To said crystallite Si-Sb xTe 1-xComposite phase-change material is carried out the heating anneal dehydrogenating technology.
Alternatively, form said amorphous Si-Sb xTe 1-xThe method of material layer is a physical vapour deposition (PVD) PVD technology.
Alternatively, to said Si-Sb xTe 1-xLayer is carried out for the first time, and annealing process comprises: with said Si-Sb xTe 1-xBe placed in the blanket of nitrogen, annealing temperature is 250 degrees centigrade to 450 degrees centigrade, and annealing time is 3 minutes to 5 minutes.
Alternatively, with the said Si-Sb of annealing back phase-splitting xTe 1-xAnnealing process comprises material as for carrying out for the second time in the nitrogen atmosphere: annealing temperature is 200 degrees centigrade to 500 degrees centigrade, and annealing time is 10 minutes to 30 minutes.
Alternatively, said heating anneal dehydrogenating technology comprises: with said crystallite Si-Sb xTe 1-xComposite phase-change material is incubated dehydrogenation in 10 minutes to 30 minutes under 300 degrees centigrade to 600 degrees centigrade annealing temperature.
Alternatively, the crystallite dimension of said crystallite Si is 3 nanometer to 20 nanometers.
The preparation method who is applied to the phase-change material of phase transition storage provided by the invention, phase-change material wherein is by the Si of crystallite attitude and phase-change material Sb xTe 1-xBe composited.The Si crystallite dimension of crystallite attitude is about 3 nanometer to 20 nanometers, and is littler than amorphous state Si (a-Si) relatively, the atom more ordering of arranging, so defective lacks than amorphous state Si (c-Si), can effectively suppress oxidation, hinders Si and Sb xTe 1-xThe phase counterdiffusion, have more stable properties.
In addition, with the Si-Sb after the phase-splitting xTe 1-xPlace nitrogen atmosphere annealing can effectively reduce the temperature of Si crystallization.Because the crystallization temperature of common Si is more than 1000 ℃, and phase-change material promptly volatilizees at 660 ℃, H combines with the dangling bonds of Si, makes it more be prone to crystallization, reduces crystallization temperature to guarantee the intact of phase-change material.
Have again, with said crystallite Si-Sb xTe 1-xComposite phase-change material is applied in the phase transition storage, and the Si of crystallite attitude has changed the distribution of electric current in the phase transformation, has improved phase velocity, helps reducing power consumption and improves useful life, improves the operational stability of phase transition storage.
Description of drawings
Fig. 1 has shown crystallite Si-Sb provided by the invention xTe 1-xThe preparation method of phase-change material schematic flow sheet in one embodiment.
Fig. 2 has shown it is the crystallite Si-Sb to preparation 2Te 3The X-ray diffraction test XRD figure of composite phase-change material sample.
Fig. 3 uses has crystallite Si-Sb 2Te 3The effect sketch map of the performance test of the phase transition storage of composite phase-change material.
Embodiment
Inventor of the present invention finds: in existing phase transition storage, when compound mutually the Si-Te-Sb series phase-change material that adopts by amorphous Si and SbTe crystal, owing to there are many defectives in amorphous state Si, make SiSb xTe 1-xThe phase-change material of series is unstable, thereby causes the phase transition storage based on said phase-change material on stability and erasable number of times, to show not good enough.
Therefore, inventor of the present invention improves prior art, has proposed a kind of preparation method of novel phase-change material, forms amorphous Si-Sb earlier xTe 1-xMaterial is in the phase-splitting through annealing, with the SiSb after the annealing phase-splitting xTe 1-xMaterial places nitrogen atmosphere, makes SiSb xTe 1-xThe amorphous state Si that exists in the material SET attitude is converted into crystallite attitude Si, forms novel crystallite Si and Sb xTe 1-xComposite phase-change material, the Si crystallite dimension of crystallite attitude is about 3 nanometer to 20 nanometers, and defective is less, can effectively suppress oxidation, can hinder Si and Sb xTe 1-xThe phase counterdiffusion, help reducing power consumption and improve useful life, improve the operational stability of phase transition storage.
Below in conjunction with the more complete description the present invention of diagram, preferred embodiment provided by the invention, but should not be considered to only limit in the embodiment of this elaboration.In the drawings, for clearer reaction structure, suitably amplified the thickness of layer, but should not be considered to the proportionate relationship that strictness has reflected physical dimension as sketch map with the zone.Reference diagram is a sketch map of the present invention, and the expression among the figure is an illustrative nature, should not be considered to limit scope of the present invention.
Fig. 1 has shown that promptly the present invention is applied to the crystallite Si and the Sb of phase transition storage xTe 1-xThe preparation method of composite phase-change material schematic flow sheet in one embodiment.As shown in Figure 1, said preparation method comprises:
Step S11 provides Semiconductor substrate, on said Semiconductor substrate, forms amorphous Si-Sb xTe 1-xMaterial layer, wherein 0.1≤x≤0.9;
Step S13 is at said amorphous Si-Sb xTe 1-xOn the crystallization temperature of composite material, to said Si-Sb xTe 1-xCarry out annealing process for the first time, feasible amorphous Si and Sb wherein xTe 1-xCrystal forms phase-splitting;
Step S15 is with the amorphous Si and the Sb of annealing back phase-splitting xTe 1-xComposite material place nitrogen atmosphere to carry out annealing process for the second time, make amorphous Si wherein change crystallite Si into to form crystallite Si-Sb xTe 1-xComposite phase-change material;
Step S17 is to said crystallite Si-Sb xTe 1-xComposite phase-change material is carried out the heating anneal dehydrogenating technology.
Below in conjunction with accompanying drawing content of the present invention is elaborated.
At first execution in step S11 provides Semiconductor substrate 100, on Semiconductor substrate 100, forms amorphous Si-Sb xTe 1-xMaterial layer, wherein 0.1≤x≤0.9.
Wherein, said Semiconductor substrate 100 is for the silicon that is formed with semiconductor device (for example being electrode), the silicon-on-insulator (SOI) that is formed with semiconductor device, or for being formed with the II-VI or the III-V compound semiconductor of semiconductor device.
In this execution mode, amorphous Si-Sb xTe 1-xThe method that material layer forms be physical gas-phase deposition (Physical Vapor Deposition, PVD).Particularly; For example can adopt magnetically controlled sputter method; Obtain the thin-film material layer of stoichiometric(al) through modulation process parameter (sputtering power, operating air pressure etc.), wherein adopt the technology of PVD technology growing film to be well known to those skilled in the art, so do not give unnecessary details at this.In step S11, the Si-Sb that utilizes PVD technology to form xTe 1-xMaterial layer, Si wherein exists with amorphous form.
Then, execution in step S13 is at said amorphous Si 2Sb 2Te 3On the crystallization temperature of composite material, said Si-SbxTel-x is carried out annealing process for the first time, feasible amorphous Si and Sb wherein xTe 1-xCrystal forms phase-splitting.
In step S13, said first time, annealing process comprised: with said Si-Sb xTe 1-xBe placed on blanket of nitrogen (N 2) in, annealing temperature be preferably 250 degrees centigrade (℃) to 450 degrees centigrade (℃), annealing time is preferably 3 minutes to 5 minutes.In fact, can do suitable adjustment to annealing temperature and annealing time, thereby select optimum technological parameter based on the difference of real material proportioning.
Then, execution in step S15 is with the amorphous Si and the Sb of annealing back phase-splitting xTe 1-xThe composite material of crystal places nitrogen atmosphere (H 2) the middle annealing process for the second time of carrying out, make amorphous Si wherein change crystallite Si into to form crystallite Si-Sb xTe 1-xComposite phase-change material.
Because the crystallization temperature of common Si is more than 1000 ℃, and phase-change material promptly volatilizees at 660 ℃, therefore, in the present invention, especially, with the Si-Sb after the phase-splitting xTe 1-xPlace nitrogen atmosphere to anneal, make H combine with the dangling bonds of Si, make it more be prone to crystallization, the temperature that reduces the Si crystallization is to guarantee the intact of phase-change material.
In this execution mode, said second time, annealing process comprised: annealing temperature is 200 degrees centigrade to 500 degrees centigrade, and annealing time is 10 minutes to 30 minutes.
In step S15, the annealing temperature in the said second time annealing process is a lower temperature, because the existence of H makes amorphous state Si form crystallite Si in this temperature in the nitrogen atmosphere, and does not cause phase-change material component segregation or performance change at high temperature.In addition, the crystallite dimension of said crystallite Si is that 3 nanometers (nm) are to 20 nanometers (nm).
Then, execution in step S17 is with said crystallite Si-Sb xTe 1-xComposite phase-change material is carried out the heating anneal dehydrogenating technology.
In this execution mode, said heating anneal dehydrogenating technology comprises: with said crystallite Si-Sb xTe 1-xComposite phase-change material is incubated dehydrogenation in 10 minutes to 30 minutes under 300 degrees centigrade to 600 degrees centigrade annealing temperature.
In step S17, crystallite Si and Sb xTe 1-xDo not influence the phase transformation performance of phase-change material after the composite material dehydrogenation.
Be elaborated with the preparation method of an instantiation at present to phase-change material in the above-mentioned execution mode.In following embodiment, be with Si 2Sb 2Te 3Material is that example describes, but not as limit, in other embodiments, still can adopt other phase-change materials.
At first, utilize the PVD equipment amorphous Si-Sb that on sheet glass, grows xTe 1-xMaterial layer;
Then, with said amorphous Si-Sb xTe 1-xMaterial layer is at blanket of nitrogen (N 2) in, under 300 degrees centigrade annealing temperature, annealed 3 minutes, make it form amorphous state Si and crystalline state Sb 2Te 3Compound phase;
Then, with amorphous state Si after the phase-splitting and crystalline state Sb 2Te 3Composite material place nitrogen atmosphere (H 2) in, under 350 degrees centigrade annealing temperature, annealed 30 minutes;
At last, with said crystallite Si-Sb 2Te 3Composite phase-change material is incubated 30 to accomplish dehydrogenation under 400 degrees centigrade annealing temperature.
See also Fig. 2, demonstration be the crystallite Si-Sb to above-mentioned preparation 2Te 3X-ray diffraction test (X-ray Diffraction, XRD) figure of composite phase-change material sample.As shown in Figure 2, the characteristic peak of Si has appearred in the XRD figure, demonstrated (111), (220), (311) crystal orientation of silicon.The crystallite dimension of crystallite Si be 3 nanometers (nm) to 20 nanometers (nm), that explains that the inventive method can success prepares crystallite Si.
In addition, with the crystallite Si-Sb of above-mentioned preparation 2Te 3Composite phase-change material is applied in the phase transition storage, specifically comprises: utilize PVD equipment with Si 2Sb 2Te 3Material is grown in preparation to be had in the flow substrate of electrode; With said amorphous Si-Sb xTe 1-xMaterial layer is at blanket of nitrogen (N 2) in, under 300 degrees centigrade annealing temperature, annealed 3 minutes, make it form amorphous state Si and crystalline state Sb 2Te 3Compound phase; With amorphous state Si after the phase-splitting and crystalline state Sb 2Te 3Composite material place nitrogen atmosphere (H 2) in, under 350 degrees centigrade annealing temperature, annealed 30 minutes; With said crystallite Si-Sb 2Te 3Composite phase-change material is incubated 30 to accomplish dehydrogenation under 400 degrees centigrade annealing temperature; Continue to accomplish the subsequent step of flow, comprise growth titanium nitride (TiN), etching, growing metal (for example Al), complete phase transition storage is produced in corrosion etc.Phase transition storage to accomplishing is write, wiping, read operation, studies storage characteristics and the fatigue properties of said material etc.Fig. 3 is to use has crystallite Si-Sb 2Te 3The test result of the phase transition storage of composite phase-change material.As shown in Figure 3, with crystallite Si-Sb 2Te 3Composite phase-change material is applied in the phase transition storage, and the Si of crystallite attitude compares with amorphous Si, and defective is few, can effectively suppress oxidation, hinders Si and Sb xTe 1-xThe phase counterdiffusion, changed the distribution of electric current in the phase transformation operation simultaneously, help reducing power consumption, improve the life-span, improve phase velocity, improve the operational stability of phase transition storage.
In sum, the preparation method who is applied to the phase-change material of phase transition storage provided by the invention, phase-change material wherein is by the Si of crystallite attitude and phase-change material Sb xTe 1-xBe composited.The Si crystallite dimension of crystallite attitude is about 3 nanometer to 20 nanometers, and is littler than amorphous state Si (a-Si) relatively, the atom more ordering of arranging, so defective is than amorphous state Si) lack, can effectively suppress oxidation, hinder Si and Sb xTe 1-xThe phase counterdiffusion, have more stable properties.
In addition, with the Si-Sb after the phase-splitting xTe 1-xPlace nitrogen atmosphere annealing can effectively reduce the temperature of Si crystallization.Because the crystallization temperature of common Si is more than 1000 ℃, and phase-change material promptly volatilizees at 660 ℃, H combines with the dangling bonds of Si, makes it more be prone to crystallization, reduces crystallization temperature to guarantee the intact of phase-change material.
Have again, with said crystallite Si-Sb xTe 1-xComposite phase-change material is applied in the phase transition storage, and the Si of crystallite attitude has changed the distribution of electric current in the phase transformation, has improved phase velocity, helps reducing power consumption and improves useful life, improves the operational stability of phase transition storage.
The foregoing description is just listed expressivity principle of the present invention and effect is described, but not is used to limit the present invention.Any personnel that are familiar with this technology all can make amendment to the foregoing description under spirit of the present invention and scope.Therefore, rights protection scope of the present invention should be listed like claims.

Claims (6)

1. the preparation method of a phase-change material is characterized in that, may further comprise the steps:
Semiconductor substrate is provided, on said Semiconductor substrate, forms amorphous Si-Sb xTe 1-xMaterial layer, wherein 0.1≤x≤0.9;
At said amorphous Si-Sb xTe 1-xOn the crystallization temperature of composite material, to said Si-Sb xTe 1-xLayer is carried out annealing process for the first time, feasible amorphous Si and Sb wherein xTe 1-xCrystal forms phase-splitting;
Amorphous Si and Sb with annealing back phase-splitting xTe 1-xThe composite material of crystal places nitrogen atmosphere to carry out annealing process for the second time, makes amorphous Si wherein change crystallite Si into to form crystallite Si-Sb xTe 1-xComposite phase-change material;
To said crystallite Si-Sb xTe 1-xComposite phase-change material is carried out the heating anneal dehydrogenating technology.
2. the preparation method of phase-change material according to claim 1 is characterized in that, forms said amorphous Si-Sb xTe 1-xThe method of material layer is a physical vapour deposition (PVD) PVD technology.
3. the preparation method of phase-change material according to claim 1 is characterized in that, to said Si-Sb xTe 1-xLayer is carried out for the first time, and annealing process comprises: with said Si-Sb xTe 1-xBe placed in the blanket of nitrogen, annealing temperature is 250 degrees centigrade to 450 degrees centigrade, and annealing time is 3 minutes to 5 minutes.
4. according to the preparation method of claim 1 or 3 described phase-change materials, it is characterized in that, the said Si-Sb of annealing back phase-splitting xTe 1-xAnnealing process comprises material as for carrying out for the second time in the nitrogen atmosphere: annealing temperature is 200 degrees centigrade to 500 degrees centigrade, and annealing time is 10 minutes to 30 minutes.
5. the preparation method of phase-change material according to claim 1 is characterized in that, said heating anneal dehydrogenating technology comprises: with said crystallite Si-Sb xTe 1-xComposite phase-change material is incubated dehydrogenation in 10 minutes to 30 minutes under 300 degrees centigrade to 600 degrees centigrade annealing temperature.
6. the preparation method of phase-change material according to claim 1 is characterized in that, the crystallite dimension of said crystallite Si is 3 nanometer to 20 nanometers.
CN2011103769229A 2011-11-23 2011-11-23 Preparation method of phase-change material Pending CN102386327A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103811713A (en) * 2012-11-01 2014-05-21 三星Sdi株式会社 Winder for electrode assembly of rechargeable battery
US11271155B2 (en) 2020-03-10 2022-03-08 International Business Machines Corporation Suppressing oxidation of silicon germanium selenium arsenide material

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2004099835A1 (en) * 2003-05-09 2004-11-18 Hernan Miguez Method of laser writing refractive index patterns in silicon photonic crystals
CN102534479A (en) * 2010-12-16 2012-07-04 中国科学院上海微***与信息技术研究所 Microcrystalline Si-SbxTe1-x composite phase change material and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2004099835A1 (en) * 2003-05-09 2004-11-18 Hernan Miguez Method of laser writing refractive index patterns in silicon photonic crystals
CN102534479A (en) * 2010-12-16 2012-07-04 中国科学院上海微***与信息技术研究所 Microcrystalline Si-SbxTe1-x composite phase change material and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103811713A (en) * 2012-11-01 2014-05-21 三星Sdi株式会社 Winder for electrode assembly of rechargeable battery
CN103811713B (en) * 2012-11-01 2017-05-03 三星Sdi株式会社 Winder for electrode assembly of rechargeable battery
US11271155B2 (en) 2020-03-10 2022-03-08 International Business Machines Corporation Suppressing oxidation of silicon germanium selenium arsenide material

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