CN107768518B - A kind of Al/Ge for phase transition storage10Sb90Class superlattices phase change film material and preparation method - Google Patents
A kind of Al/Ge for phase transition storage10Sb90Class superlattices phase change film material and preparation method Download PDFInfo
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Abstract
The invention belongs to microelectronic field phase-change materials and preparation method thereof, more particularly to a kind of Al/Ge for phase transition storage10Sb90Class superlattices phase change film material and preparation method.A kind of Al/Ge for phase transition storage10Sb90Class superlattices phase change film material, the Al/Ge10Sb90Class superlattices phase change film material is MULTILAYER COMPOSITE membrane structure, by Al layers and Ge10Sb90Layer alternating deposit is combined, by Al layers and Ge10Sb90Layer is used as an alternate cycle, and the Al layer of the latter alternate cycle is deposited on the Ge of previous alternate cycle10Sb90Layer top.The present invention uses the Al/Ge for phase transition storage10Sb90Class superlattices phase change film material is a kind of novel phase-change material, and not only thermal stability is good, while retaining the advantage that its speed is fast, low in energy consumption again.
Description
Technical field
The invention belongs to microelectronic field phase-change materials and preparation method thereof, are used for phase transition storage more particularly to one kind
Al/Ge10Sb90Class superlattices phase change film material and preparation method.
Background technique
Memory occupies an important position in semi-conductor market, only DRAM (dynamnicRandamAccessMemory)
Just occupy the 15% of whole market with two kinds of FLASH, with gradually popularizing for portable electronic device, nonvolatile memory
Market is also increasing, and FLASH accounts for the mainstream of nonvolatile memory, about 90% at present.But with the progress of semiconductor technology,
FLAH meets more and more technical bottlenecks, and the floating gate of storage charge first cannot be unlimited with the development of integrated circuit technology
System is thinned, and furthermore some other disadvantage of FLASH technology also limits his application.
Phase change memory technology be based on Ovshinsky late 1960s (Phys.Rev.Lett, 21,1450
~1453,1968) phase-change thin film that the beginning of the seventies (Appl.Phys.Lett, 18,254-257,1971) proposes can be applied to
What the conception of phase change memory medium was set up, be a kind of memory device cheap, performance is stable.Phase transition storage can be with
It is made in silicon wafer substrate, critical material is recordable phase-change thin film, heating electrode material, heat-insulating material and extraction electrode
The research hotspot of material is also just unfolded around its device technology: the physical mechanism research of device includes how to reduce device material etc..Phase
The basic principle of transition storage is acted on device cell using electric impulse signal, makes phase-change material in amorphous state and polycrystalline state
Between reversible transition occurs, by high resistant when differentiating amorphous state and low-resistance when polycrystalline state, the write-in of information may be implemented, wipe
It removes and read operation.
High speed reading, high erasable number, non-volatile, component size is small, low in energy consumption, anti-due to having for phase transition storage
Strong motion and it is anti-radiation the advantages that, thought that current flash memories is most possibly replaced to form by International Semiconductor Industry Association
For future memory main product and at first as the device of commercial product.
Voltage or electricity that operation is exactly application different in width and height on device cell are wiped in the reading and writing of phase transition storage
Signal pulse stream: operation (RESET) is wiped, when adding a short and strong pulse signal to make the phase-change material temperature liter in device cell
After more than height to fusion temperature, then through the rapid cooling to achieve phase-change material polycrystalline state to amorphous conversion, i.e. one state
To the conversion of 0 state；Write operation (SET) is raised to phase-change material temperature when applying long and moderate strength a pulse signal
Under fusion temperature, on crystallization temperature after, and keep a period of time promote nucleus growth, to realize amorphous state to polycrystalline state
Conversion, i.e. the conversion of 0 state to one state；Read operation, when add one the state of phase-change material will not be had an impact it is very weak
Pulse signal after, its state is read by the resistance value of measurement device unit.
As the phase-change thin film of phase transition storage core, physical characteristic is of crucial importance.In order to real simultaneously
Existing high stability, the cycle life of length and ultrafast reading speed, phase-change material must simultaneously have biggish amorphous state/crystalline state
Good stability, preferable chemical stability and lower fusing point and thermal conductivity under resistance ratio, amorphous state.
There are three types of methods for regulation currently with GeSb material to phase transformation GeSb alloy phase change performance: one is changing GeSb
Atom composition realize the change (YifengGu etc., Applied Physics A, 2009,99:205-209) of phase transition performance；
The second is by the doping of other elements, such as N mix GeSb (Audery Bastard, MRS proceedings, 2010,
1251:03-22)；The third is to prepare superlattices (multilayer) phase-change material, such as GeSb/Ge (Pengzhi Wu, SPIE
Proceeding, 2016,9818).The third technique study is also fewer, while also not over the conductive metal films such as Al reality
The research of existing superlattices regulation.
GeSb series storage material occupies an important position in phase-change material, however its thermal stability is not able to satisfy large number of rows
The needs of industry restrict always its development.Therefore, seek a kind of GeSb storage material that thermal stability is good become information technology into
The road of the certainty of step.
Summary of the invention
It is an object of the invention to overcome the prior art to take the undesirable defect of thermal stability of GeSb series storage material,
A kind of Al/Ge for phase transition storage is provided10Sb90Class superlattices phase change film material and preparation method.
The present invention provides a kind of Al/Ge for phase transition storage10Sb90Class superlattices phase change film material, it is described
Al/Ge10Sb90Class superlattices phase change film material is MULTILAYER COMPOSITE membrane structure, by Al layers and Ge10Sb90Layer alternating deposit it is compound and
At by Al layers and Ge10Sb90Layer is used as an alternate cycle, and the Al layer of the latter alternate cycle is deposited on previous alternate cycle
Ge10Sb90Layer top.
The Al/Ge10Sb90The membrane structure of class superlattices phase change film material general formula [Al (a)/Ge10Sb90 (b)]xTable
Show, the thickness that wherein a is single layer Al layers, 1nm≤a≤50nm；B is single layer Ge10Sb90The thickness of layer, 1nm≤b≤50nm；X is
Al layers and Ge10Sb90The alternate cycle number of layer, x is positive integer.
Further, the Ge10Sb90Contain two kinds of elements of Ge and Sb in layer, the atomic ratio of Ge and Sb are 1: 9.
Further, the 6nm≤(a+b) * x≤80nm.
Further, the 30nm≤(a+b) * x≤70nm.
A kind of Al/Ge for phase transition storage10Sb90The preparation method of class superlattices phase change film material, including it is following
Step:
①SiO2It is stand-by to be cleaned drying by the preparation of/Si (100) substrate for substrate；
2. the preparation of magnetron sputtering, by step, 1. clean substrate to be sputtered is placed on base, by Al alloy and
Ge10Sb90It is separately mounted in magnetron RF sputtering system target as sputtering target material, and by the sputtering chamber of magnetron sputtering coating system
It is vacuumized, uses high-purity argon gas as sputter gas；
3. magnetron sputtering prepares [Al (a)/Ge10Sb90(b)]xMulti-layer compound film；
A, Ge is cleaned first10Sb90Alloy target material and Al target material surface；
B, after target material surface cleaning, by SiO to be sputtered2/ Si (100) substrate rotates to Al alloy target position, opens
Target baffle starts Al layers of sputtering and closes Al alloy target position target baffle after the completion of Al layers of sputtering；
C, the substrate for having sputtered Al layers is rotated into Ge10Sb90Target position opens Ge10Sb90Baffle on target position, sputtering
After obtain Ge10Sb90Layer；
D, repeat the above steps b and c, and number of repetition is x-1 times, and sputtering terminates to obtain for high-speed low-power-consumption phase change memory
The Ga of device40Sb60/ Sb class superlattices phase change film material.
Further, the step 2. in high-purity argon gas percent by volume >=99.999%, Ar throughput be 25~
35SCCM, argon sputter air pressure are 0.15Pa~0.35Pa.
Al layers of sputter rate is 3~5s/nm, the Ge in the step 3. c in the step 3. b10Sb90Layer sputtering
Rate is 2~4s/nm.
Beneficial effects of the present invention: (1) present invention is using the Al/Ge for being used for phase transition storage10Sb90Class superlattices phase transformation
Thin-film material is a kind of novel phase-change material, and not only thermal stability is good, while retaining the advantage that its speed is fast, low in energy consumption again；
(2) at that same temperature, resistance variations rate is bigger, then crystallization is fast, and crystalline rate is faster, the operating time of high resistant to low-resistance
Shorten, to improve the service speed of device.(3) under the action of external energy, can smoothly realize high-impedance state and low resistance state it
Between reversible transition, the storage of data is realized using the difference of low resistance high before and after reversible transition.Due to the addition of Al, improve
Al/Ge10Sb90The data retention of class superlattices phase change film material, enhances the stability of device.
Detailed description of the invention
Fig. 1 is Al/Ge of the embodiment of the present invention 1 to embodiment 510Sb90Class superlattices phase change film material and comparative example
The In-situ resistance of phase change film material and the graph of relation of temperature；
Fig. 2 is the Ge of comparative example of the present invention10Sb90The resistance and time changing curve figure of phase change film material, illustration is phase
The Arrhenius curve answered；
Fig. 3 is [Al (8nm) Ge of the embodiment of the present invention 110Sb90(4nm)]5The resistance and time change of phase change film material are bent
Line chart, illustration are corresponding Arrhenius curve；
Fig. 4 is [Al (9nm) Ge of the embodiment of the present invention 210Sb90(3nm)]5The resistance and time change of phase change film material are bent
Line chart, illustration are corresponding Arrhenius curve；
Fig. 5 is [Al (10nm) Ge of the embodiment of the present invention 310Sb90(2nm)]5The resistance and time change of phase change film material
Curve graph, illustration are corresponding Arrhenius curve.
Specific embodiment
The present invention is further illustrated combined with specific embodiments below.
Al/Ge for phase transition storage of the invention10Sb90Class superlattices phase change film material is multilayer complex films knot
Structure, with a thickness of 48~72nm；By by Al layers and Ge10Sb90Layer alternating deposit be combined, i.e., in the film, according to Al layers-
Ge10Sb90- Al layers of-Ge of layer10Sb90The sequence of layer ... repeats to be alternately arranged.
By one layer Al layers and one layer of Ge10Sb90Layer is used as an alternate cycle, and the Al layer of the latter alternate cycle is deposited on
The Ge of previous alternate cycle10Sb90Layer top.Ge10Sb90Contain two kinds of elements of Ge and Sb in layer, the atomic ratio of Ge and Sb are 1:
9。
Al/Ge10Sb90The membrane structure of class superlattices phase change film material general formula [Al (a)/Ge10Sb90(b)]xIt indicates,
The thickness that middle a is single layer Al layers, 1nm≤a≤50nm；B is single layer Ge10Sb90The thickness of layer, 1nm≤b≤50nm；X is Al layers
And Ge10Sb90The alternate cycle number of layer, x is positive integer.
Embodiment 1
The Al/Ge of the present embodiment10Sb90Class superlattices phase change film material membrane structure is [Al (8nm) Ge10Sb90
(4nm)]5, i.e., each layer Al layers with a thickness of 8nm, each layer of Ge10Sb90Layer with a thickness of 4nm, Al layers and Ge10Sb90The friendship of layer
It is 5 for periodicity, [Al (8nm) Ge10Sb90(4nm)]5Superlattices phase change film material with a thickness of 60nm.
[Al (8nm) Ge of the present embodiment10Sb90(4nm)]5Superlattices phase change film material is made using magnetron sputtering method,
Specific preparation method, comprising the following steps:
1. the preparation of substrate.
Choose the SiO having a size of 5mm × 5mm2/ Si (100) substrate is first (pure in acetone by substrate in supersonic cleaning machine
Degree is 99% or more) middle ultrasonic cleaning 3~5 minutes, it washes complete taking-up and is rinsed with deionized water；Then by base in supersonic cleaning machine
Piece ultrasonic cleaning 3~5 minutes in ethyl alcohol (purity is 99% or more), wash complete taking-up and are rinsed with deionized water, after rinsing well
Use high-purity N2Dry up surface and the back side；Substrate after drying, which is sent into baking oven, dries moisture, and the substrate after drying is stand-by, wherein drying
Box temperature degree is set as 120 DEG C, drying time 20 minutes.
2. the preparation of magnetron sputtering.
In magnetron sputtering coating system (JGP-450 type), 1. SiO to be sputtered that step is prepared2/ Si (100) base
Piece is placed on base, by Ge10Sb90And Al (atomic percent alloy (purity 99.999%, atomic percent Ge: Sb=1: 9)
Than content 99.999%) it is separately mounted in magnetic control radio frequency (RF) sputtering target as sputtering target material, and by magnetron sputtering membrane system
The sputtering chamber of system vacuumize until vacuum degree reaches 1 × 10 in chamber-4Pa。
Use high-purity argon gas (percent by volume reaches 99.999%) as sputter gas, set Ar throughput as
25SCCM, and by argon sputter air pressure adjustment to 0.15Pa, the sputtering power of radio-frequency power supply is set as 30W.Set radio-frequency power supply
Sputtering power be 25W~35W (being 25W in the present embodiment).
3. magnetron sputtering prepares Al (8nm) Ge10Sb90(4nm)]5Multi-layer compound film；
A, Ge is cleaned first10Sb90Alloy target material and Al target material surface.Space base support is rotated into Ge10Sb90Target position is opened
Ge10Sb90DC power supply on target position sets sputtering time 100s, starts to Ge10Sb90Alloy target material surface is sputtered, clearly
Clean Ge10Sb90Alloy target material surface；Ge10Sb90After alloy target material surface cleaning, Ge is closed10Sb90Apply on alloy target position
Radio-frequency power supply, space base support is rotated into Al target position, opens the radio-frequency power supply on Al target position, sets sputtering time 100s, is started
Al target material surface is sputtered, Al target material surface is cleaned, after Al target material surface cleans, is applied on closing Al target position straight
Galvanic electricity source, by SiO to be sputtered2/ Si (100) substrate rotates to Al alloy target position.
B, start the Al layer of first alternate cycle of sputtering: opening the radio-frequency power supply on Al target, set Al layers of sputterings speed
Rate is 3s/nm, sputters sputtering time 16s, the Al layer of 8nm thickness is obtained after sputtering；After the completion of Al layers of sputtering, Al is closed
The radio-frequency power supply applied on target.
C, the substrate for having sputtered Al layers is rotated into Ge10Sb90Target position opens Ge10Sb90Radio-frequency power supply on target position,
Set Ge10Sb90Layer sputter rate is 2s/nm, and sputtering time 12s obtains the Ge of 4nm thickness after sputtering10Sb90Layer.
D, repeat the above steps b and c, and number of repetition is 4 times, obtains Al layers of-Ge10Sb90Layer-Al
Layer-Ge10Sb90Al (8nm) Ge of the repetition alternating deposit of layer ...10Sb90(4nm)]5Multi-layer compound film.
Embodiment 2
The Al/Ge of the present embodiment10Sb90Class superlattices phase change film material membrane structure is [Al (9nm) Ge10Sb90
(3nm)]5, i.e., each layer Al layers with a thickness of 9nm, each layer of Ge10Sb90Layer with a thickness of 3nm, Al layers and Ge10Sb90The friendship of layer
It is 5 for periodicity, [Al (9nm) Ge10Sb90(3nm)]5Superlattices phase change film material with a thickness of 60nm.
Remaining is same as Example 1 for preparation method, the difference is that: in the preparation of 2. magnetron sputtering, set Ar gas
Flow is 30SCCM, and by argon sputter air pressure adjustment to 0.25Pa, sets the sputtering power of radio-frequency power supply as 28W.In step
3. Al layers of sputter rate is 4s/nm in b, sputtering time is 18s；The Ge in the step 3. c10Sb90Layer sputter rate be
3s/nm, sputtering time are 9s.
Embodiment 3
The Al/Ge of the present embodiment10Sb90Class superlattices phase change film material membrane structure is [Al (10nm) Ge10Sb90
(2nm)]5, i.e., each layer Al layers with a thickness of 10nm, each layer of Ge10Sb90Layer with a thickness of 2nm, Al layers and Ge10Sb90Layer
Alternate cycle number is 5, [Al (10nm) Ge10Sb90(2nm)]5Superlattices phase change film material with a thickness of 60nm.
Remaining is same as Example 1 for preparation method, the difference is that: in the preparation of 2. magnetron sputtering, set Ar gas
Flow is 35SCCM, and by argon sputter air pressure adjustment to 0.25Pa, sets the sputtering power of radio-frequency power supply as 30W.
Al layers of sputter rate is 5s/nm in the step 3. b, and sputtering time is 20s；In the step 3. c
Ge10Sb90Layer sputter rate is 4s/nm, and sputtering time is 6s.
Embodiment 4
The Al/Ge of the present embodiment10Sb90Class superlattices phase change film material membrane structure is [Al (12nm) Ge10Sb90
(2nm)]4, i.e., each layer Al layers with a thickness of 12nm, each layer of Ge10Sb90Layer with a thickness of 2nm, Al layers and Ge10Sb90Layer
Alternate cycle number is 4, [Al (12nm) Ge10Sb90(2nm)]4Superlattices phase change film material with a thickness of 60nm.
Remaining is same as Example 1 for preparation method, the difference is that: in the preparation of 2. magnetron sputtering, set Ar gas
Flow is 28SCCM, and by argon sputter air pressure adjustment to 0.35Pa, sets the sputtering power of radio-frequency power supply as 35W.Described
3. Al layers of sputter rate is 3s/nm to step in b, and sputtering time is 24s；The Ge in the step 3. c10Sb90Layer sputter rate
For 4/nm, sputtering time is 6s.
Embodiment 5
The Al/Ge of the present embodiment10Sb90Class superlattices phase change film material membrane structure is [Al (14nm) Ge10Sb90
(2nm)]4, i.e., each layer Al layers with a thickness of 14nm, each layer of Ge10Sb90Layer with a thickness of 2nm, Al layers and Ge10Sb90Layer
Alternate cycle number is 4, [Al (14nm) Ge10Sb90(2nm)]4Superlattices phase change film material with a thickness of 60nm.
Remaining is same as Example 1 for preparation method, the difference is that: in the preparation of 2. magnetron sputtering, set Ar gas
Flow is 32SCCM, and by argon sputter air pressure adjustment to 0.22Pa, sets the sputtering power of radio-frequency power supply as 32W.Described
3. Al layers of sputter rate is 5s/nm to step in b, and sputtering time is 28s；The Ge in the step 3. c10Sb90Layer sputter rate
For 3/nm, sputtering time is 6s.
Comparative example
This example prepares the Ge of single layer10Sb90Phase change film material is with as a comparison, thickness 60nm.According to the side of embodiment 1
Method, Ge10Sb90Sputter rate is 2s/nm, and 145s when sputtering obtains the single layer Ge of 60nm thickness after sputtering10Sb90Phase transformation
Thin-film material.
In order to understand Al/Ge of the invention10Sb90The performance of class superlattices phase change film material, to embodiment 1 to implementation
Ge made from thin-film material made from example 5 and comparative example10Sb90Thin-film material is tested, and the original of each phase change film material is obtained
The graph of relation of position resistance and temperature.
Fig. 1 is Al/Ge of the embodiment of the present invention 1 to embodiment 510Sb90Class superlattices phase change film material and comparative example
The In-situ resistance of phase change film material and the graph of relation of temperature；
Fig. 2 is the Ge of comparative example of the present invention10Sb90The resistance and time changing curve figure of phase change film material, illustration is phase
The Arrhenius curve answered；
Fig. 3 is [Al (8nm) Ge of the embodiment of the present invention 110Sb90(4nm)]5The resistance and time change of phase change film material are bent
Line chart, illustration are corresponding Arrhenius curve；
Fig. 4 is [Al (9nm) Ge of the embodiment of the present invention 210Sb90(3nm)]5The resistance and time change of phase change film material are bent
Line chart, illustration are corresponding Arrhenius curve；
Fig. 5 is [Al (10nm) Ge of the embodiment of the present invention 310Sb90(2nm)]5The resistance and time change of phase change film material
Curve graph, illustration are corresponding Arrhenius curve.
The above is only section Examples of the invention, not do limitation in any form to the present invention, it is all according to
According to any simple modification that technical spirit of the invention makees above-described embodiment, equivalent variations and modification belong to the present invention
In technical proposal scope.
Claims (4)
1. a kind of Al/Ge for phase transition storage10Sb90Class superlattices phase change film material, it is characterised in that: the Al/
Ge10Sb90Class superlattices phase change film material is MULTILAYER COMPOSITE membrane structure, by Al layers and Ge10Sb90Layer alternating deposit is combined,
By Al layers and Ge10Sb90Layer is used as an alternate cycle, and the Al layer of the latter alternate cycle is deposited on previous alternate cycle
Ge10Sb90Layer top；
The Al/Ge10Sb90The membrane structure of class superlattices phase change film material general formula [Al (a)/Ge10Sb90(b)] x is indicated,
The thickness that middle a is single layer Al layers, a=10nm；B is single layer Ge10Sb90The thickness of layer, b=2nm；X is Al layers and Ge10Sb90Layer
Alternate cycle number, x 5；Its thickness of the multilayer complex films meets (a+b) × x=60nm.
2. a kind of Al/Ge for being used for phase transition storage as defined in claim 110Sb90Class superlattices phase change film material
Preparation method, which comprises the following steps:
①SiO2It is stand-by to be cleaned drying by the preparation of/Si (100) substrate for substrate；
2. 1. substrate to be sputtered that step is cleaned is placed on base, by Al alloy and Ge by the preparation of magnetron sputtering10Sb90
It is separately mounted in magnetron RF sputtering system target as sputtering target material, and the sputtering chamber of magnetron sputtering coating system take out very
Sky uses high-purity argon gas as sputter gas；
3. magnetron sputtering prepares [Al (a)/Ge10Sb90(b)] x multi-layer compound film:
A, Ge is cleaned first10Sb90Alloy target material and Al target material surface；
B, after target material surface cleaning, by SiO to be sputtered2/ Si (100) substrate rotates to Al alloy target position, opens target baffle
Start Al layers of sputtering and closes Al alloy target position target baffle after the completion of Al layers of sputtering；
C, the substrate for having sputtered Al layers is rotated into Ge10Sb90Target position opens Ge10Sb90Baffle on target position, sputtering terminate
After obtain Ge10Sb90Layer；
D, repeat the above steps b and c, and number of repetition is x-1 times, and sputtering terminates to obtain for high-speed low-power-consumption phase change memory
[Al(a)/Ge10Sb90(b)] x class superlattices phase change film material.
3. the Al/Ge according to claim 2 for phase transition storage10Sb90The preparation of class superlattices phase change film material
Method, it is characterised in that: the step 2. in high-purity argon gas percent by volume >=99.999%, Ar throughput be 25~
35SCCM, argon sputter air pressure are 0.15Pa~0.35Pa.
4. the Al/Ge according to claim 2 for phase transition storage10Sb90The preparation of class superlattices phase change film material
Method, it is characterised in that: Al layers of sputter rate is 3~5s/nm in the step 3. b, in the step 3. c
Ge10Sb90Layer sputter rate is 2~4s/nm.
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