CN107093667A - A kind of Ge Cu Te nano phase changes thin-film materials and preparation method for high stability phase transition storage - Google Patents
A kind of Ge Cu Te nano phase changes thin-film materials and preparation method for high stability phase transition storage Download PDFInfo
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N70/00—Solid-state devices without a potential-jump barrier or surface barrier, and specially adapted for rectifying, amplifying, oscillating or switching
- H10N70/801—Constructional details of multistable switching devices
- H10N70/881—Switching materials
- H10N70/882—Compounds of sulfur, selenium or tellurium, e.g. chalcogenides
- H10N70/8828—Tellurides, e.g. GeSbTe
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N70/00—Solid-state devices without a potential-jump barrier or surface barrier, and specially adapted for rectifying, amplifying, oscillating or switching
- H10N70/011—Manufacture or treatment of multistable switching devices
- H10N70/021—Formation of the switching material, e.g. layer deposition
- H10N70/026—Formation of the switching material, e.g. layer deposition by physical vapor deposition, e.g. sputtering
Abstract
The present invention relates to a kind of material of microelectronics technology, and in particular to a kind of Ge Cu Te nano phase changes thin-film materials and preparation method for high stability phase transition storage, and the atomic percent composition of the Ge Cu Te nano phase change thin-film materials is GexCu100‑2xTex, the Ge Cu Te nano phase change thin-film materials are that the composite target material constituted with GeTe targets and circular pure Cu pieces is formed by the method deposition of high vacuum magnetron sputtering.Nano phase change thin-film material of the present invention has higher crystallization temperature, can greatly improve PCRAM amorphous heat endurance；With higher crystalline resistance, PCRAM power consumption can be reduced.
Description
Technical field
The present invention relates to a kind of material of microelectronics technology, and in particular to one kind is used for high stability phase transition storage
Ge-Cu-Te nano phase changes thin-film material and preparation method.
Background technology
Phase transition storage (PCRAM) is a kind of new nonvolatile memory, it using chalcogenide compound material crystalline state-
Occur different high low-resistance values between amorphous state during rapid phase transition to realize that information is stored.When different electric pulses applies
The repetition reversible transformation between high-impedance state and low resistance state can be realized, the purpose of information storage is reached.Compared to making extensively now
Flash storage, PCRAM has storage density is high, low in energy consumption, reading speed is fast, compatible with traditional CMOS technology etc.
Advantage, thus paid close attention to by increasing researcher.
The performance of phase-change material directly affects PCRAM indices.Ge2Sb2Te5It is current application most wide, most study
Phase-change storage material.In recent years, in order to realize more high stability, the purpose of faster phase velocity, increasing Novel photo
Become storage material to be increasingly developed out.Kingdom is auspicious etc. to have developed Zr-Sb-Se phase-change materials, and the thin-film material has nanosecond
Magnitude high-speed phase change, with stronger high high-temp stability and crystalline resistance, obvious resistance difference between larger amorphous state and crystalline state
Different and preferable Reversible Cycle phase transformation ability.(CN201410473416.5, kingdom is auspicious etc., the Zn-Sb- for phase transition storage
Se phase transiting storing thin-film materials).
Putero, Magali etc. have developed the GaSb phase-change materials of Ge doping, have more compared to GaSb, Ge-GaSb
Good amorphous state heat endurance and smaller amorphous-crystalline density change (the 108th phase Applied Physics in 2016
Letters, Ge-doped GaSb thin films with zero mass density change upon
crystallization for applications in phase change memories).In addition, Si-Sb-Se, Ti-
The phase-change materials such as Sb-Te, W-Sb-Te are also studied, with preferable storage performance.
The content of the invention
The purpose of the present invention is to overcome phase-change material heat endurance is not good, operation converted power consumption is higher in the prior art to lack
There is provided a kind of Ge-Cu-Te nano phase changes thin-film material and its preparation method and application for point.The present invention is using Ge-Cu-Te as phase transformation
Material, not only has the advantages that preferable heat endurance, data holding ability are higher, and fast with small power consumption, phase velocity
A series of advantages.Ge-Cu-Te is compared with Ge2Sb2Te5(being abbreviated as GST) has more preferable heat endurance, is preferable phase change memory
Material, with preferable market application foreground.
The present invention is to adopt the following technical scheme that to realize above-mentioned purpose：
A kind of Ge-Cu-Te nano phase change thin-film materials for high stability phase transition storage, it is described Ge-Cu-Te nanometers
The atomic percent composition of phase change film material is GexCu100-2xTex, the Ge-Cu-Te nano phase changes thin-film material be with
The composite target material that GeTe targets and circular pure Cu pieces are constituted is formed by the method deposition of high vacuum magnetron sputtering；The GeTe targets are straight
Footpath is 50.8mm, and the diameter for overlaying the circular pure Cu pieces above GeTe targets is respectively 20mm, 30mm and 40mm；(the Ge-
The atomic percent composition of Cu-Te nano phase change thin-film materials is GexCu100-2xTexIt is to be determined by EDS energy disperse spectroscopies, that is, represents Ge
Atomic percent be x%, the atomic percent that Cu atomic percent is (100-2x) %, Te is x%.
Circular pure Cu pieces are overlayed at GeTe pinwheels in the composite target material.
The Ge-Cu-Te nano phase change thin-film material thickness for high stability phase transition storage is preferably 50nm, can
To be regulated and controled by the high vacuum magnetron sputtering time.
Can be by adjusting the composite target material Ge that GeTe sputtering target materials and circular pure Cu pieces are constituted in the present inventionxCu100-2xTex
The circular area ratios of middle circular pure Cu pieces adjusts composite target material GexCu100-2xTexMiddle X size, such as in fixed GeTe targets
In the case of a diameter of 50.8mm, a diameter of 20mm, 30mm, 40mm of the circular pure Cu pieces stacked, the Ge preparedxCu100- 2xTexThe atomic percent composition of material is respectively Ge35Cu30Te35、Ge30Cu40Te30、Ge25Cu50Te25。
Ge prepared by the present inventionxCu100-2xTexNano phase change thin-film material shows the phase transformation of obvious amorphous-crystalline
Process, and GexCu100-2xTexThe crystallization temperature of nano phase change thin-film material is higher than GeTe, crystalline resistance also greater than GeTe,
Therefore the energy consumed during RESET is less.
According to another aspect of the present invention, the invention provides a kind of Ge-Cu- for high stability phase transition storage
The preparation method of Te nano phase change thin-film materials, specifically includes following steps：
1) cleaning substrate Si O2/ Si (100) substrate cleaning surface, the back side, remove dust granule, organic and inorganic impurity；
2) the composite target material Ge that GeTe sputtering target materials and circular pure Cu pieces are constituted is installedxCu100-2xTex；Setting sputtering work(
Rate, setting sputtering Ar throughputs and sputtering pressure；Ge of the present inventionxCu100-2xTexMiddle 100-2x represents Cu in GeTe targets and circle
The pure Cu pieces of shape constitute the atomic percent in composite target material；
3) Ge is prepared using room temperature magnetically controlled sputter methodxCu100-2xTexNano phase change thin-film material.
The preparation method of Ge-Cu-Te nano phase change thin-film materials of the present invention for phase transition storage, step 1)
Clean substrate Si O2/ Si (100) substrate, cleaning surface, the back side, removes dust granule, organic and inorganic impurity, specific steps
For：
A) substrate Si O2/ Si (100) substrate is strong in acetone soln to be cleaned by ultrasonic 10 minutes, deionized water rinsing；
B) it is strong in ethanol solution to be cleaned by ultrasonic 10 minutes, deionized water rinsing, high-purity N2Dry up surface and the back side；
C) in 200 DEG C of drying in oven steam, about 30 minutes.
The preparation method of Ge-Cu-Te nano phase change thin-film materials of the present invention for phase transition storage, step 2)
Install the composite target material Ge that GeTe sputtering target materials and circular pure Cu pieces are constitutedxCu100-2xTex；Set sputtering power, setting sputtering
Ar throughputs and sputtering pressure, it is concretely comprised the following steps：
A) GeTe sputtering target materials are installed, the center that circular pure Cu pieces are overlayed to a diameter of 50.8mm GeTe targets is constituted
Composite target material, and base vacuum is evacuated to 1 × 10-4Pa；It is preferred that the sputtering target material GeTe atomic percent purity reach
99.999%, the atomic percent purity of the Cu pieces preferably reaches 99.999%；
B) setting sputtering power 30W；
C) use high-purity Ar gas as sputter gas (Ar air volume percent purities reach 99.999%), set Ar air-flows
Measure as 40sccm, and sputtering pressure is adjusted to 0.4Pa.
The preparation method of Ge-Cu-Te nano phase change thin-film materials of the present invention for phase transition storage, step 3)
Middle use room temperature magnetically controlled sputter method prepares GexCu100-2xTexNano phase change thin-film material, specifically includes following steps：
A) space base support is rotated into GexCu100-2xTexComposition target target position, opens the radio-frequency power supply on target, according to splashing for setting
The time is penetrated for 200s (pre-sputtering time), is started to GexCu100-2xTexComposite target material surface is sputtered, cleaning target position surface；
b)GexCu100-2xTexAfter the completion of composition target surface cleaning, Ge is closedxCu100-2xTexApplied on composition target target position
Radio-frequency power supply, by step 1) in clean after SiO2/ Si (100) substrate is mounted in magnetic control sputtering device in sample disc and revolved
Go to GexCu100-2xTexTarget position, opens GexCu100-2xTexWhen the radio-frequency power supply on composition target target position, sputtering according to setting
Between, start to sputter Ge-Cu-Te films；
The Ge-Cu-Te nano phase changes thin-film material of the present invention can be applied to phase transition storage, with traditional phase-change thin film
Material is compared and had the following advantages that：
First, Ge-Cu-Te nano phase changes thin-film material has higher crystallization temperature, can greatly improve the non-of PCRAM
Brilliant heat endurance；Ge25Cu50Te25The crystalline resistance of material has brought up to 4657 Ω by GeTe 315 Ω, contributes to reduction
The power consumption of RESET processes；Crystallization temperature brings up to 254 DEG C by 185 DEG C, and heat endurance is greatly improved；
Secondly, Ge-Cu-Te nano phase changes thin-film material has higher crystalline resistance, so as to reduce PCRAM work(
Consumption；Ge25Cu50Te25Resistance-voltage tester Dependence Results that PCRAM devices are made with GeTe phase change film materials show,
Ge25Cu50Te25RESET voltage be 2.27V, and GeTe RESET voltage be 3.6V, Ge25Cu50Te25With lower work(
Consumption；Ge25Cu50Te25Reversible transition can be realized under 8ns voltage pulse, illustrate that it has faster phase velocity.
Brief description of the drawings
Fig. 1 is Ge of the inventionxCu100-2xTexAnd for the In-situ resistance of the GeTe nano phase change thin-film materials compared
With the relation curve of temperature.
Fig. 2 is Ge of the inventionxCu100-2xTexAnd for the out-of-service time of the GeTe nano phase change thin-film materials compared
With inverse temperature relation curve.
Fig. 3 is the Ge based on the present invention25Cu50Te25And for the PCRAM devices of the GeTe nano phase change thin-film materials compared
Part resistance~voltage curve.
Embodiment
To make the object, technical solutions and advantages of the present invention of greater clarity, with reference to embodiment, to this
Invention is further described.It should be understood that these descriptions are merely illustrative, and it is not intended to limit the scope of the present invention.
Embodiment 1
The atomic percent composition of the Ge-Cu-Te nano phase change thin-film materials prepared in the present embodiment is Ge35Cu30Te35。
Preparation process is：
1. clean SiO2/ Si (100) substrate, cleaning surface, the back side, removes dust granule, organic and inorganic impurity；
A) it is strong in acetone soln to be cleaned by ultrasonic 10 minutes, deionized water rinsing；
B) it is strong in ethanol solution to be cleaned by ultrasonic 10 minutes, deionized water rinsing, high-purity N2Dry up surface and the back side；
C) in 200 DEG C of drying in oven steam, about 30 minutes.
2. Ge is prepared using RF sputtering method35Cu30Te35Prepare before film, that is, install GeTe sputtering target materials and circle
The composite target material Ge that pure Cu pieces are constitutedxCu100-2xTex；Set sputtering power, setting sputtering Ar throughputs and sputtering pressure；：
A) GeTe sputtering target materials are installed, the center that a diameter of 20mm circular pure Cu pieces are overlayed into GeTe targets constitutes multiple
Close target GexCu100-2xTex.The purity of GeTe and Cu pieces reaches 99.999% (atomic percent), and base vacuum is evacuated to
1×10-4Pa；
B) setting sputtering power 30W；
C) use high-purity Ar gas as sputter gas (Ar air volume percent purities reach 99.999%), set Ar air-flows
Measure as 40sccm, and sputtering pressure is adjusted to 0.4Pa.
3. Ge is prepared using magnetically controlled sputter method35Cu30Te35Nano phase change thin-film material：
A) space base support is rotated into GexCu100-2xTexCompound target position, opens GexCu100-2xTexApplied on composition target
Radio-frequency power supply, according to the sputtering time set as 200s (pre-sputtering time), starts to GexCu100-2xTexComposition target surface is carried out
Sputtering, cleans GexCu100-2xTexComposition target target material surface；
b)GexCu100-2xTexAfter the completion of composition target surface cleaning, Ge is closedxCu100-2xTexWhat is applied on composition target penetrates
Frequency power, by the SiO after being cleaned in step 12/ Si (100) substrate is in the sample disc of magnetic control sputtering device and rotates to
GexCu100-2xTex composition target target position, opens GexCu100-2xTexComposition target target position radio-frequency power supply, according to the sputtering time set as
175s (film thickness × sputter rate), starts to sputter Ge35Cu30Te35Film.
The Ge finally obtained35Cu30Te35Film thickness is 50nm, and film thickness is controlled by sputtering time,
Ge35Cu30Te35Sputter rate be 3.5s/nm.
Embodiment 2
The atomic percent composition of film manufactured in the present embodiment is Ge30Cu40Te30、Ge25Cu50Te25, it is specific to prepare
Process is similar to Example 1, and different places is that the diameter of Cu targets is different, prepares Ge30Cu40Te30Shi Caiyong Cu target diameters
For 30mm, Ge is prepared25Cu50Te25The Shi Caiyong a diameter of 40mm of Cu targets.
Comparative example 1
Individual layer GeTe phase change film materials, thickness 50nm are prepared in this example.
Preparation process is：
1. clean SiO2/ Si (100) substrate, cleaning surface, the back side, removes dust granule, organic and inorganic impurity；
A) it is strong in acetone soln to be cleaned by ultrasonic 10 minutes, deionized water rinsing；
B) it is strong in ethanol solution to be cleaned by ultrasonic 10 minutes, deionized water rinsing, high-purity N2Dry up surface and the back side；
C) in 200 DEG C of drying in oven steam, about 30 minutes.
Prepare 2. being prepared using RF sputtering method before GeTe films：
A) GeTe sputtering target materials are installed, the purity of target reaches 99.999% (atomic percent), and by base vacuum
It is evacuated to 1 × 10-4Pa；
B) setting sputtering power 30W；
C) use high-purity Ar gas as sputter gas (percent by volume reaches 99.999%), set Ar throughputs as
40sccm, and sputtering pressure is adjusted to 0.4Pa.
3. GeTe nano phase change thin-film materials are prepared using magnetically controlled sputter method：
A) space base support is rotated into GeTe target position, opens the radio-frequency power supply applied on GeTe targets, the sputtering according to setting
Time 200s (pre-sputtering time), starts to sputter GeTe targets, cleans GeTe target material surfaces；
B) after the completion of the cleaning of GeTe target material surfaces, the radio-frequency power supply applied on GeTe targets is closed, substrate to be sputtered is revolved
GeTe target position is gone to, GeTe target position radio-frequency power supplies are opened, according to the sputtering time 125s (film thickness × sputter rate) of setting,
Start to sputter GeTe films.
By above-described embodiment 1 and 2 and the Ge of comparative example 135Cu30Te35、Ge30Cu40Te30、Ge25Cu50Te25With GeTe phase transformations
Thin-film material is tested, and obtains the In-situ resistance of each phase change film material and relation curve Fig. 1 of temperature；By above-described embodiment
The 1 and 2 and Ge of comparative example 135Cu30Te35、Ge30Cu40Te30、Ge25Cu50Te25With GeTe phase change film materials at different temperatures
Isothermal Crystallization experiment is carried out, the out-of-service time of each material and the corresponding relation of inverse temperature is obtained；By above-described embodiment 2 and contrast
The Ge of example 125Cu50Te25PCRAM devices are made with GeTe phase change film materials, its resistance~voltage curve Fig. 3 is tested.Fig. 1-figure
3 testing result is as follows：
Fig. 1 is Ge of the invention35Cu30Te35、Ge30Cu40Te30、Ge25Cu50Te25With the GeTe nano phase changes of comparative example 1
Heating rate in the In-situ resistance of thin-film material and the relation curve of temperature, test process is 30 DEG C/min.At low temperature, institute
There is film to be in high-resistance amorphous state.With the continuous rise of temperature, film resistor is slowly reduced, when reaching its phase transition temperature
When, film resistor is reduced rapidly, is dropped to after a certain value and is kept the resistance constant substantially, shows that film there occurs by amorphous state to crystalline substance
The transformation of state.Test result shows that GeTe crystallization temperature is 185 DEG C, Ge35Cu30Te35、Ge30Cu40Te30、Ge25Cu50Te25
The crystallization temperature of film is respectively 234 DEG C, 245 DEG C, 254 DEG C.Show the phase-change material of the present invention compared with GeTe phase-change thin film materials
The heat endurance of material is enhanced.Meanwhile, Ge of the invention30Cu40Te30、Ge25Cu50Te25The crystalline resistance of material
4657 Ω are brought up to by GeTe 315 Ω, this can aid in the power consumption of reduction RESET processes.
Fig. 2 is Ge of the invention35Cu30Te35、Ge30Cu40Te30、Ge25Cu50Te25With the GeTe out-of-service times of comparative example 1
With the corresponding relation of inverse temperature.As a result show, the temperature that GeTe materials can keep data 10 years is 78 DEG C, and of the invention
Ge35Cu30Te35、Ge30Cu40Te30、Ge25Cu50Te2510 years keeping temperatures be respectively 103 DEG C, 126 DEG C and 159 DEG C, namely
The phase-change material of the present invention has more preferable data reliability.
Fig. 3 is the Ge based on the present invention25Cu50Te25Resistance-voltage of PCRAM devices is made with GeTe phase change film materials
Test curve.As a result show, Ge of the invention25Cu50Te25RESET voltage be 2.27V, and GeTe RESET voltage is
3.6V, it can be seen that Ge of the invention25Cu50Te25With lower power consumption.In addition, the Ge of the present invention25Cu50Te25Can be
Reversible transition is realized under 8ns voltage pulse, illustrates that it has faster phase velocity.
Although embodiments of the present invention are described in detail, it should be understood that, without departing from the present invention's
In the case of spirit and scope, embodiments of the present invention can be made with various changes, replace and change.
Claims (7)
1. a kind of Ge-Cu-Te nano phase change thin-film materials for high stability phase transition storage, the Ge-Cu-Te nanometers of phase
The atomic percent composition of thinning membrane material is GexCu100-2xTex, the Ge-Cu-Te nano phase changes thin-film material is with GeTe
The composite target material that target and circular pure Cu pieces are constituted is formed by the method deposition of high vacuum magnetron sputtering.
2. the Ge-Cu-Te nano phase change thin-film materials according to claim 1 for high stability phase transition storage, its
It is characterised by：The thickness of the Ge-Cu-Te nano phase change thin-film materials for high stability phase transition storage is 50nm.
3. the Ge-Cu-Te nano phase change thin-film materials according to claim 1 for high stability phase transition storage, its
It is characterised by：The atomic percent composition of the Ge-Cu-Te nano phase changes thin-film material is Ge35Cu30Te35、Ge30Cu40Te30
Or Ge25Cu50Te25。
4. a kind of system of the Ge-Cu-Te nano phase change thin-film materials for high stability phase transition storage described in claim 1
Preparation Method, comprises the following steps：
1) cleaning substrate Si O2/ Si (100) substrate, cleaning surface, the back side, removes dust granule, organic and inorganic impurity；
2) the composite target material Ge that GeTe sputtering target materials and circular pure Cu pieces are constituted is installedxCu100-2xTex；Sputtering power is set, if
Surely Ar throughputs and sputtering pressure are sputtered；
3) Ge is prepared using room temperature magnetically controlled sputter methodxCu100-2xTexNano phase change thin-film material.
5. preparation method according to claim 4, it is characterised in that：The step 1) cleaning substrate Si O2/ Si (100) base
Piece, cleaning surface, the back side, removes dust granule, organic and inorganic impurity, concretely comprises the following steps：
A) substrate Si O2/ Si (100) substrate is strong in acetone soln to be cleaned by ultrasonic 10 minutes, deionized water rinsing；
B) it is strong in ethanol solution to be cleaned by ultrasonic 10 minutes, deionized water rinsing, high-purity N2Dry up surface and the back side；
C) in 200 DEG C of drying in oven steam.
6. preparation method according to claim 4, it is characterised in that：Step 2) described install GeTe sputtering target materials and circle
The composite target material Ge that the pure Cu pieces of shape are constitutedxCu100-2xTex；Set sputtering power, setting sputtering Ar throughputs and sputtering pressure, tool
Body step is：
A) GeTe sputtering target materials are installed, the center composition that circular pure Cu pieces are overlayed to a diameter of 50.8mm GeTe targets is compound
Target, and base vacuum is evacuated to 1 × 10-4Pa；
B) setting sputtering power 30W；
C) high-purity Ar gas is used as sputter gas, sets Ar throughputs as 40sccm, and sputtering pressure is adjusted to 0.4Pa.
7. preparation method according to claim 4, it is characterised in that：Step 3) the use room temperature magnetically controlled sputter method system
Standby GexCu100-2xTexNano phase change thin-film material, is concretely comprised the following steps：
A) space base support is rotated into GexCu100-2xTexComposition target target position, opens the radio-frequency power supply on target, starts to GexCu100- 2xTexComposite target material surface is sputtered, cleaning target position surface；
b)GexCu100-2xTexAfter the completion of composition target surface cleaning, Ge is closedxCu100-2xTexThe radio frequency applied on composition target target position
Power supply, by step 1) in clean after SiO2/ Si (100) substrate is mounted in magnetic control sputtering device in sample disc and rotated to
GexCu100-2xTexComposition target target position, opens GexCu100-2xTexWhen the radio-frequency power supply on composition target target position, sputtering according to setting
Between, start sputtered film.
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Application publication date: 20170825 |