CN107768518A - 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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- 239000000758 substrate Substances 0.000 claims description 18
- 239000013077 target material Substances 0.000 claims description 17
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 15
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- 238000000576 coating method Methods 0.000 claims description 3
- 238000001552 radio frequency sputter deposition Methods 0.000 claims description 2
- 239000012782 phase change material Substances 0.000 abstract description 12
- 238000005265 energy consumption Methods 0.000 abstract description 3
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- 229910005872 GeSb Inorganic materials 0.000 description 8
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Abstract
The invention belongs to microelectronic phase-change material 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 layers of the latter alternate cycle are deposited on the Ge of previous alternate cycle10Sb90Layer top.The present invention is using the Al/Ge for phase transition storage10Sb90Class superlattices phase change film material, it is a kind of novel phase-change material, not only heat endurance is good, while retains the advantages of its speed is fast, low in energy consumption again.
Description
Technical field
The invention belongs to microelectronic phase-change material and preparation method thereof, is used for phase transition storage more particularly to one kind
Al/Ge10Sb90Class superlattices phase change film material and preparation method.
Background technology
Memory occupies critical role in semi-conductor market, only DRAM (dynamnicRandamAccessMemory) and
Two kinds of FLASH just occupies the 15% of whole market, with the progressively popularization of portable electric appts, the market of nonvolatile memory
Also increasing, FLASH accounts for the main flow of nonvolatile memory, about 90% at present.But with the progress of semiconductor technology, FLAH is met
Increasing technical bottleneck is seen, storing the floating boom of electric charge first can not subtract as the development of integrated circuit technology is unconfined
Thin, some other shortcoming of FLASH technologies also limits his application in addition.
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 apply to phase
What the conception of change storage medium was set up, be a kind of cheap, stable performance memory device.Phase transition storage can be done
In silicon wafer substrate, its critical material is recordable phase-change thin film, heating electrode material, heat-insulating material and extraction electrode material
Study hotspot also just around its device technology deploy:The physical mechanism research of device, includes how to reduce device material etc..Phase transformation
The general principle of memory is to be acted on using electric impulse signal on device cell, make phase-change material amorphous state and polycrystalline state it
Between reversible transition occurs, low-resistance during high resistant and polycrystalline state during by differentiating amorphous state, it is possible to achieve write-in, the erasing of information
And read operation.
Phase transition storage is because with high speed reading, high erasable number, non-volatile, component size is small, low in energy consumption, anti-
The advantages that strong motion and radioresistance, thought most possibly to substitute current flash memories to form by International Semiconductor Industry Association
For future memory main product and at first as the device of commercial product.
Reading and writing, the wiping operation of phase transition storage are exactly to apply different in width and the voltage or electricity of height on device cell
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
It is high to after more than fusion temperature, then by quick cooling so as to realizing phase-change material polycrystalline state to amorphous conversion, i.e. one state
To the conversion of " 0 " state;Write operation (SET), it 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, so as to realize amorphous state to polycrystalline state
Conversion, i.e. " 0 " state to one state conversion;Read operation, it is very weak when adding a state to phase-change material not have an impact
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, its physical characteristic has vital effect.In order to simultaneously real
Existing high stability, the cycle life of length and ultrafast reading speed, phase-change material must simultaneously have larger amorphous state/crystalline state
Good stability, preferable chemical stability and relatively low fusing point and thermal conductivity under resistance ratio, amorphous state.
There are three kinds of methods currently with regulation and control of the GeSb material to phase transformation GeSb alloy phase change performances:One is change GeSb
Atom composition realize phase transition performance change (YifengGu etc., Applied Physics A, 2009,99:205-209);Its
Second, 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 real not over conductive metal films such as Al
The research of existing superlattices regulation and control.
GeSb series storage materials occupy critical role in phase-change material, but its heat endurance can not meet large number of rows
The needs of industry, its development is govern always.Therefore, seek a kind of good GeSb storage materials of heat endurance as information technology to enter
The road of the certainty of step.
The content of the invention
It is an object of the invention to overcome prior art take GeSb series storage materials heat endurance it is undesirable the defects of,
A kind of Al/Ge for phase transition storage is provided10Sb90Class superlattices phase change film material and preparation method.
The 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
Into by Al layers and Ge10Sb90Layer is used as an alternate cycle, and the Al layers of the latter alternate cycle are deposited on previous alternate cycle
Ge10Sb90Layer top.
The Al/Ge10Sb90The membrane structure of class superlattices phase change film material formula [Al (a)/Ge10Sb90(b)]xTable
Show, wherein a be individual layer Al layers thickness, 1nm≤a≤50nm;B is individual 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, Ge and Sb atomic ratio 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:
①SiO2The preparation of/Si (100) substrate, it is stand-by that substrate is cleaned into drying;
2. the preparation of magnetron sputtering, by step, 1. clean substrate to be sputtered is placed on base, by Al alloys and
Ge10Sb90It is separately mounted to as sputtering target material in magnetron RF sputtering system target, and by the sputtering chamber of magnetron sputtering coating system
Vacuumized, sputter gas is used as using high-purity argon gas;
3. magnetron sputtering prepares [Al (a)/Ge10Sb90(b)]xMulti-layer compound film;
A, Ge is cleaned first10Sb90Alloy target material and Al target material surfaces;
B, after target material surface cleaning, by SiO to be sputtered2/ Si (100) substrate rotates to Al alloy target position, opens
Target baffle plate starts to sputter Al layers, after the completion of the sputtering of Al layers, closes Al alloy target position target baffle plates;
C, the substrate for having sputtered Al layers is rotated into Ge10Sb90Target position, open Ge10Sb90Baffle plate on target position, sputtering
Ge is obtained after end10Sb90Layer;
D, repeat the above steps b and c, and number of repetition is x-1 times, and sputtering end obtains being used for high-speed low-power-consumption phase change memory
The Ga of device40Sb60/ Sb class superlattices phase change film materials.
Further, the step 2. middle high-purity argon gas percent by volume >=99.999%, Ar throughput for 25~
35SCCM, argon sputter air pressure are 0.15Pa~0.35Pa.
The sputter rate of Al layers is 3~5s/nm, the Ge in the step 3. c in the step 3. b10Sb90Layer sputtering
Speed is 2~4s/nm.
Beneficial effects of the present invention:(1) present invention is using the Al/Ge for phase transition storage10Sb90Class superlattices phase transformation
Thin-film material, it is a kind of novel phase-change material, not only heat endurance is good, while retains the advantages of its speed is fast, low in energy consumption again;
(2) at that same temperature, resistance variations speed is bigger, then crystallization is fast, and crystalline rate is faster, the operating time of high resistant to low-resistance
Shorten, so as to improve the service speed of device.(3) in the presence 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 high low resistance before and after reversible transition.Due to Al addition, improve
Al/Ge10Sb90The data retention of class superlattices phase change film material, enhance the stability of device.
Brief description of the drawings
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 of phase change film material and time changing curve figure, illustration is phase
The Arrhenius curve answered;
Fig. 3 is [Al (8nm) Ge of the embodiment of the present invention 110Sb90(4nm)]5The resistance of phase change film material is bent with time change
Line chart, illustration are corresponding Arrhenius curve;
Fig. 4 is [Al (9nm) Ge of the embodiment of the present invention 210Sb90(3nm)]5The resistance of phase change film material is bent with time change
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 map, illustration are corresponding Arrhenius curve.
Embodiment
With reference to specific embodiment, the present invention is further illustrated.
The Al/Ge for phase transition storage of the present invention10Sb90Class superlattices phase change film material is multilayer complex films knot
Structure, thickness are 48~72nm;By by Al layers and Ge10Sb90Layer alternating deposit be combined, i.e., in the film, according to Al layers-
Ge10Sb90Layer-Al layers-Ge10Sb90The order of layer ... repeats to be alternately arranged.
By one layer of Al layer and one layer of Ge10Sb90Layer is used as an alternate cycle, and the Al layers of the latter alternate cycle are deposited on
The Ge of previous alternate cycle10Sb90Layer top.Ge10Sb90Contain two kinds of elements of Ge and Sb in layer, Ge and Sb atomic ratio are 1:
9。
Al/Ge10Sb90The membrane structure of class superlattices phase change film material formula [Al (a)/Ge10Sb90(b)]xRepresent, its
Middle a be individual layer Al layers thickness, 1nm≤a≤50nm;B is individual 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., the thickness of each layer Al layer is 8nm, each layer of Ge10Sb90The thickness of layer is 4nm, Al layers and Ge10Sb90The friendship of layer
It is 5 for periodicity, [Al (8nm) Ge10Sb90(4nm)]5The thickness of superlattices phase change film material is 60nm.
[Al (8nm) Ge of the present embodiment10Sb90(4nm)]5Superlattices phase change film material is made using magnetron sputtering method,
Specific preparation method, comprises the following steps:
1. the preparation of substrate.
Choose the SiO that size is 5mm × 5mm2/ Si (100) substrate is first (pure in acetone by substrate in supersonic cleaning machine
Spend for more than 99%) in be cleaned by ultrasonic 3~5 minutes, wash complete taking-up deionized water rinsing;Then by base in supersonic cleaning machine
Piece is cleaned by ultrasonic 3~5 minutes in ethanol (purity is more than 99%), complete taking-up deionized water rinsing is washed, 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 arranged to 120 DEG C, drying time 20 minutes.
2. the preparation of magnetron sputtering.
In magnetron sputtering coating system (JGP-450 types), 1. SiO to be sputtered that step is prepared2/ Si (100) base
Piece is placed on base, by Ge10Sb909) and Al (atomic percents alloy (purity 99.999%, atomic percent Ge: Sb=1:
Than content 99.999%) it is separately mounted to as sputtering target material in magnetic control radio frequency (RF) sputtering target, and by magnetron sputtering membrane system
The sputtering chamber of system vacuumize until vacuum reaches 1 × 10 in chamber-4Pa。
Using high-purity argon gas (percent by volume reaches 99.999%) as sputter gas, set Ar throughputs 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 surfaces.Space base support is rotated into Ge10Sb90Target position, open
Ge10Sb90Dc source on target position, sputtering time 100s is set, is started 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 surfaces are sputtered, clean Al target material surfaces, after Al target material surfaces clean, are applied on closing Al target position straight
Power supply is flowed, by SiO to be sputtered2/ Si (100) substrate rotates to Al alloy target position.
B, the Al layers of first alternate cycle of sputtering are started:Open the radio-frequency power supply on Al targets, setting Al layer sputtering speed
Rate is 3s/nm, sputters sputtering time 16s, and sputtering obtains the Al layers of 8nm thickness after terminating;After the completion of the sputtering of Al layers, Al targets are closed
The radio-frequency power supply applied on material.
C, the substrate for having sputtered Al layers is rotated into Ge10Sb90Target position, open Ge10Sb90Radio-frequency power supply on target position,
Set Ge10Sb90Layer sputter rate is 2s/nm, sputtering time 12s, and sputtering obtains the Ge of 4nm thickness after terminating10Sb90Layer.
D, repeat the above steps b and c, and number of repetition is 4 times, obtains Al layers-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., the thickness of each layer Al layer is 9nm, each layer of Ge10Sb90The thickness of layer is 3nm, Al layers and Ge10Sb90The friendship of layer
It is 5 for periodicity, [Al (9nm) Ge10Sb90(3nm)]5The thickness of superlattices phase change film material is 60nm.
Remaining is same as Example 1 for preparation method, and difference is:In the preparation of 2. magnetron sputtering, Ar gas is set
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. the sputter rate of Al layers 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., the thickness of each layer Al layer is 10nm, each layer of Ge10Sb90The thickness of layer is 2nm, Al layers and Ge10Sb90Layer
Alternate cycle number is 5, [Al (10nm) Ge10Sb90(2nm)]5The thickness of superlattices phase change film material is 60nm.
Remaining is same as Example 1 for preparation method, and difference is:In the preparation of 2. magnetron sputtering, Ar gas is set
Flow is 35SCCM, and by argon sputter air pressure adjustment to 0.25Pa, sets the sputtering power of radio-frequency power supply as 30W.
The sputter rate of Al layers 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., the thickness of each layer Al layer is 12nm, each layer of Ge10Sb90The thickness of layer is 2nm, Al layers and Ge10Sb90Layer
Alternate cycle number is 4, [Al (12nm) Ge10Sb90(2nm)]4The thickness of superlattices phase change film material is 60nm.
Remaining is same as Example 1 for preparation method, and difference is:In the preparation of 2. magnetron sputtering, Ar gas is set
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. the sputter rate of Al layers 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., the thickness of each layer Al layer is 14nm, each layer of Ge10Sb90The thickness of layer is 2nm, Al layers and Ge10Sb90Layer
Alternate cycle number is 4, [Al (14nm) Ge10Sb90(2nm)]4The thickness of superlattices phase change film material is 60nm.
Remaining is same as Example 1 for preparation method, and difference is:In the preparation of 2. magnetron sputtering, Ar gas is set
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. the sputter rate of Al layers 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 individual 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 during sputtering, sputtering obtains the individual layer Ge of 60nm thickness after terminating10Sb90It is mutually thinning
Membrane material.
In order to understand the Al/Ge of the present 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 obtains the original of each phase change film material
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 of phase change film material and time changing curve figure, illustration is phase
The Arrhenius curve answered;
Fig. 3 is [Al (8nm) Ge of the embodiment of the present invention 110Sb90(4nm)]5The resistance of phase change film material is bent with time change
Line chart, illustration are corresponding Arrhenius curve;
Fig. 4 is [Al (9nm) Ge of the embodiment of the present invention 210Sb90(3nm)]5The resistance of phase change film material is bent with time change
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 map, illustration are corresponding Arrhenius curve.
The above is only the section Example of the present invention, any formal limitation not done to the present invention, it is every according to
Any simple modification made according to the technical spirit of the present invention to above-described embodiment, equivalent variations and modification, belong to the present invention
In the range of technical scheme.
Claims (7)
- A kind of 1. 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 layers of the latter alternate cycle are deposited on previous alternate cycle Ge10Sb90Layer top.The Al/Ge10Sb90The membrane structure of class superlattices phase change film material formula [Al (a)/Ge10Sb90(b)]xRepresent, its Middle a be individual layer Al layers thickness, 1nm≤a≤50nm;B is individual layer Ge10Sb90The thickness of layer, 1nm≤b≤50nm;X is Al layers And Ge10Sb90The alternate cycle number of layer, x is positive integer.
- 2. the Al/Ge according to claim 1 for phase transition storage10Sb90Class superlattices phase change film material, its feature It is:The Ge10Sb90Contain two kinds of elements of Ge and Sb in layer, Ge and Sb atomic ratio are 1: 9.
- 3. the Al/Ge according to claim 1 for phase transition storage10Sb90Class superlattices phase change film material, its feature It is:The 6nm≤(a+b) * x≤80nm.
- 4. the Al/Ge according to claim 1 for phase transition storage10Sb90Class superlattices phase change film material, its feature It is:The 30nm≤(a+b) * x≤70nm.
- A kind of 5. Al/Ge for phase transition storage as described according to any one of Claims 1 to 410Sb90Class superlattices phase transformation The preparation method of thin-film material, it is characterised in that comprise the following steps:①SiO2The preparation of/Si (100) substrate, it is stand-by that substrate is cleaned into drying;2. the preparation of magnetron sputtering, 1. substrate to be sputtered that step is cleaned is placed on base, by Al alloys and Ge10Sb90 It is separately mounted to as sputtering target material in magnetron RF sputtering system target, and the sputtering chamber of magnetron sputtering coating system take out very Sky, sputter gas is used as using high-purity argon gas;3. magnetron sputtering prepares [Al (a)/Ge10Sb90(b)]xMulti-layer compound film:A, Ge is cleaned first10Sb90Alloy target material and Al target material surfaces;B, after target material surface cleaning, by SiO to be sputtered2/ Si (100) substrate rotates to Al alloy target position, opens target baffle plate Start to sputter Al layers, after the completion of the sputtering of Al layers, close Al alloy target position target baffle plates;C, the substrate for having sputtered Al layers is rotated into Ge10Sb90Target position, open Ge10Sb90Baffle plate 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)]xClass superlattices phase change film material.
- 6. the Al/Ge according to claim 5 in phase transition storage10Sb90The preparation side of class superlattices phase change film material Method, it is characterised in that:The step 2. middle high-purity argon gas percent by volume >=99.999%, Ar throughput for 25~ 35SCCM, argon sputter air pressure are 0.15Pa~0.35Pa.
- 7. the Al/Ge according to claim 5 in phase transition storage10Sb90The preparation side of class superlattices phase change film material Method, it is characterised in that:The sputter rate of Al layers is 3~5s/nm, the Ge in the step 3. c in the step 3. b10Sb90 Layer sputter rate is 2~4s/nm.
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