CN107507914B - A kind of GeSb base nitrating nanometer thin-film material and preparation method thereof for phase transition storage - Google Patents
A kind of GeSb base nitrating nanometer thin-film material and preparation method thereof for phase transition storage Download PDFInfo
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- 239000010409 thin film Substances 0.000 title claims abstract description 43
- 230000000802 nitrating effect Effects 0.000 title claims abstract description 38
- 229910005872 GeSb Inorganic materials 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 238000003860 storage Methods 0.000 title claims abstract description 25
- 230000007704 transition Effects 0.000 title claims abstract description 25
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 68
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 34
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 14
- 239000000126 substance Substances 0.000 claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 238000004544 sputter deposition Methods 0.000 claims description 40
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 28
- 239000007789 gas Substances 0.000 claims description 18
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- 229910052786 argon Inorganic materials 0.000 claims description 14
- 239000002120 nanofilm Substances 0.000 claims description 11
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- 239000011248 coating agent Substances 0.000 claims description 8
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- 229910045601 alloy Inorganic materials 0.000 claims description 4
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- 238000001552 radio frequency sputter deposition Methods 0.000 claims description 4
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- 229910002058 ternary alloy Inorganic materials 0.000 description 2
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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 having no potential barriers, and specially adapted for rectifying, amplifying, oscillating or switching
- H10N70/801—Constructional details of multistable switching devices
- H10N70/881—Switching materials
- H10N70/883—Oxides or nitrides
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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 having no potential barriers, and specially adapted for rectifying, amplifying, oscillating or switching
- H10N70/011—Manufacture or treatment of multistable switching devices
- H10N70/021—Formation of switching materials, e.g. deposition of layers
- H10N70/026—Formation of switching materials, e.g. deposition of layers by physical vapor deposition, e.g. sputtering
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Abstract
The GeSb base nitrating nanometer thin-film material and preparation method thereof that the invention discloses a kind of for phase transition storage, the chemical composition general formula of material are (Ge10Sb90)xN1‑x, wherein x=0.68,0.63,0.60.Preparation method of the invention controls the content of nitrogen in GeSb base nitrating nanometer thin-film material by the nitrogen flow being passed through when control magnetron sputtering, and the content of nitrogen can be precisely controlled.
Description
The application is application No. is 201510067700.7, and the applying date is on 2 9th, 2015, and invention and created name is " to use
In the GeSb base nitrating nanometer thin-film material and preparation method thereof of phase transition storage " application for a patent for invention divisional application.
Technical field
The present invention relates to a kind of phase-change storage materials, and in particular to a kind of GeSb base nitrating nanometer for phase transition storage
Thin-film material and preparation method thereof.
Background technique
Phase transition storage (PCRAM) is a kind of novel nonvolatile memory, its crystalline state based on chalcogenide material
Conversion with amorphous state two-phase stores information.There is high resistance when phase-change material is in amorphous state, there is when crystalline state low electricity
Resistance realizes that the repetition between high-impedance state and low resistance state is converted using the Joule heat that electric pulse generates, achievees the purpose that information stores.
Phase transition storage has that low in energy consumption, reading speed is fast, stability is strong, storage density is high, compatible with traditional CMOS technology etc. excellent
Point, thus by the concern of more and more researchers (Kun Ren etc., Applied Physics Letter, 104
(173102), 2014).
At present research and the use of more phase-change material is Ge-Sb-Te ternary alloy three-partalloy, especially Ge2Sb2Te5, the material
It is to realize that data store using the difference of resistance before and after reversible transition.Although Ge2Sb2Te5In thermal stability, read or write speed
Have performance more outstanding, but there is also serious problems: the crystallization temperature of material is lower, and about 165 DEG C or so；Although
Based on Ge2Sb2Te5Memory data can be kept for 10 years at 110 DEG C, but memory is faced with data at high temperature and loses
The danger of mistake.In addition, the tellurium element low melting point low-steam pressure in material, is easy to generate volatilization in high temperature preparation process, to people
Body and environment have negative impact.If the Te in Ge-Sb-Te ternary alloy three-partalloy can be removed and become bianry alloy, while not shadow
The performance for even improving phase-change material is rung, is the technical problems to be solved by the invention.
Summary of the invention
That technical problem to be solved by the invention is to provide a kind of stability is high, operates low in energy consumption deposit for phase transformation simultaneously
GeSb base nitrating nanometer thin-film material of reservoir and preparation method thereof.
The technical solution for realizing the object of the invention is a kind of GeSb base nitrating nanometer thin-film material for phase transition storage,
Chemical composition general formula is (Ge10Sb90)xN1-x, wherein x=0.50~0.90.
Preferably, x=0.55~0.80.It is further preferred that x=0.80,0.68,0.63,0.60,0.55.
The preparation method of the above-mentioned GeSb base nitrating nanometer thin-film material for phase transition storage, comprising the following steps:
1. it is stand-by to be cleaned drying by the preparation of substrate for substrate.
2. the preparation of magnetron sputtering, in magnetron sputtering coating system, 1. substrate to be sputtered that step is cleaned is placed
On base, by Ge10Sb90Alloy target material is mounted in magnetron RF sputtering system target, and by the sputtering chamber of magnetron sputtering coating system
Room is vacuumized.
3. (Ge10Sb90)xN1-xThe preparation of nano film material is passed through high-purity argon gas and high pure nitrogen conduct to sputtering chamber
The total flow of sputter gas, high-purity argon gas and high pure nitrogen is 30sccm, and sputtering pressure is 0.15Pa~0.35Pa；It cleans first
Ge10Sb90Target material surface, to Ge10Sb90After target material surface cleans, Ge is closed10Sb90The radio-frequency power supply applied on target, will
SiO to be sputtered2/ Si(100) substrate rotates to Ge10Sb90Target position is then turned on Ge10Sb90Target position radio-frequency power supply starts to sputter
Obtain (Ge10Sb90)xN1-xNano film material.
2. target is mounted in magnetron RF sputtering system target by above-mentioned steps after, by the sputtering chamber of magnetron sputtering coating system
Vacuumize until vacuum degree reaches 1 × 10 in chamber-4 Pa。
Above-mentioned steps 3. in high pure nitrogen flow be 1sccm~9sccm.
Preferably, the flow of high pure nitrogen is 1sccm, the GeSb base nitrating nanometer obtained for phase transition storage
The chemical formula of thin-film material is (Ge10Sb90)0.80N0.20；Or the flow of high pure nitrogen is 2sccm, it is obtained to be deposited for phase transformation
The chemical formula of the GeSb base nitrating nanometer thin-film material of reservoir is (Ge10Sb90)0.68N0.32；Or the flow of high pure nitrogen is
4sccm, the chemical formula of the GeSb base nitrating nanometer thin-film material obtained for phase transition storage are (Ge10Sb90)0.63N0.37；
Or the flow of high pure nitrogen is 7sccm, the chemistry of the GeSb base nitrating nanometer thin-film material obtained for phase transition storage
Formula is (Ge10Sb90)0.60N0.40；Or the flow of high pure nitrogen is 9sccm, the GeSb base obtained for phase transition storage is mixed
The chemical formula of nitrogen nano film material is (Ge10Sb90)0.55N045。
Further, 3. step prepares (Ge10Sb90)xN1-xWhen nano film material, the sputtering power of radio-frequency power supply is set
For 25W~35W.Open Ge10Sb90Target position radio-frequency power supply starts sputtering and obtains (Ge10Sb90)xN1-xWhen nano film material, splash
Firing rate rate is 2 s/nm, i.e. the every thickness for increasing 1nm of film needs to sputter 2s.
The present invention has the effect of positive:
(1) with traditional Ge2Sb2Te5Phase change film material is compared, GeSb base nitrating nanometer thin-film material tool of the invention
There is faster crystallization rate, the storage speed of PCRAM can be greatly improved；In addition GeSb base nitrating nanometer thin-film material have compared with
High crystallization temperature and activation energy, so as to greatly improve the stability of PCRAM.
(2) GeSb base nitrating nanometer thin-film material of the invention has higher amorphous state and crystalline resistance, can be effective
It reduces PCRAM and operates power consumption.
(3) preparation method of the invention controls GeSb Ji Candanna by the nitrogen flow being passed through when control magnetron sputtering
The content of nitrogen in rice thin-film material, the content of nitrogen can be precisely controlled.
Detailed description of the invention
Fig. 1 is the EDS energy spectrum diagram of GeSb base nitrating nanometer thin-film material made from embodiment 1；
Fig. 2 is the nano phase change thin-film material of each embodiment and the Ge of comparative example 110Sb90The electricity in situ of phase change film material
The relation curve with temperature is hindered, the Temperature of abscissa is temperature in Fig. 1, and the Resistance of ordinate is resistance；
Fig. 3 is the nano phase change thin-film material of each embodiment and the Ge of comparative example 110Sb90When the failure of phase change film material
Between corresponding relationship curve with inverse temperature, the Failure-time of ordinate is the out-of-service time in Fig. 2.
Specific embodiment
(embodiment 1)
The chemical composition general formula of the GeSb base nitrating nanometer thin-film material for phase transition storage of the present embodiment is
(Ge10Sb90)xN1-x, wherein x=0.80 in x=0.50~0.90(the present embodiment).
GeSb base nitrating nanometer thin-film material is made using magnetron sputtering method；High pure nitrogen and high-purity argon are passed through when preparation
The total gas flow rate of gas, nitrogen and argon gas is 30sccm, and sputtering pressure is 0.15 Pa~0.35Pa, and specific preparation method includes
Following steps:
1. the preparation of substrate.Choose the SiO having a size of 5mm × 5mm2/ Si(100) substrate, it first will in supersonic cleaning machine
Substrate is washed complete taking-up and is rinsed with deionized water ultrasonic cleaning 3~5 minutes in acetone (purity is 99% or more)；Then in ultrasound
Substrate is cleaned by ultrasonic 3~5 minutes in ethyl alcohol (purity is 99% or more) in cleaning machine, complete taking-up is washed and is rinsed with deionized water,
High-purity N is used after rinsing well2Dry up surface and the back side；Substrate after drying, which is sent into baking oven, dries steam, the substrate after drying
For use, wherein oven temperature 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 Ge10Sb90Alloy (atomic percent 99.999%) is mounted on magnetic control radio frequency (RF) sputtering as target
In target, and the sputtering chamber of magnetron sputtering coating system vacuumize until vacuum degree reaches 1 × 10 in chamber-4 Pa。
3. (Ge10Sb90)xN1-xThe preparation of nano film material.
High-purity argon gas and high pure nitrogen are passed through as sputter gas to sputtering chamber, argon gas percent by volume in high-purity argon gas
Reach 99.999%；Nitrogen percent by volume reaches 99.999% in high pure nitrogen.Ar throughput is set as 29sccm, N2Flow is
Obtained film (is denoted as GSN1) by 1sccm, and sputtering pressure is adjusted in 0.15Pa~0.35Pa(the present embodiment and is
0.3Pa)；The sputtering power of radio-frequency power supply is set to be 30W in 25W~35W(the present embodiment).
Space base support is rotated into Ge10Sb90Target position opens Ge10Sb90The radio-frequency power supply applied on target, according to splashing for setting
Time 100s is penetrated, is started to Ge10Sb90Target is sputtered to clean Ge10Sb90Target material surface.
To Ge10Sb90After target material surface cleans, Ge is closed10Sb90The radio-frequency power supply applied on target, will be to be sputtered
SiO2/ Si(100) substrate rotates to Ge10Sb90Target position is then turned on Ge10Sb90Target position radio-frequency power supply starts sputtering and obtains
(Ge10Sb90)xN1-xNano film material, sputter rate are that the every thickness for increasing 1nm of 2 s/nm(, that is, film needs to sputter 2s),
Sputtering time is 100s.
(the Ge that the present embodiment sputtering obtains10Sb90)xN1-xNano film material with a thickness of 50nm.The thickness of thin-film material
It is controlled by sputtering time, sputtering time is longer, and the thickness of film is thicker.
Through field emission scanning electron microscope energy disperse spectroscopy EDS(model: Hitachi S-4700) quantitative analysis, the present embodiment it is thin
Chemical constitution formula (the Ge of membrane material10Sb90)xN1-xMiddle x=0.80.EDS energy spectrum diagram is shown in Fig. 1.
(embodiment 2)
Chemical constitution formula (the Ge of the GeSb base nitrating nanometer thin-film material for phase transition storage of the present embodiment10Sb90)xN1-xIn, x=0.68.
Remaining is same as Example 1 for preparation method, the difference is that: step 3. to sputtering chamber be passed through high-purity argon gas and
When high pure nitrogen, Ar throughput is set as 28sccm, N2Flow is 2sccm.
(embodiment 3)
The chemical composition general formula of the GeSb base nitrating nanometer thin-film material for phase transition storage of the present embodiment is
(Ge10Sb90)xN1-x, wherein x=0.63.
Remaining is same as Example 1 for preparation method, the difference is that: step 3. to sputtering chamber be passed through high-purity argon gas and
When high pure nitrogen, Ar throughput is set as 26sccm, N2Flow is 4sccm.
(embodiment 4)
The chemical composition general formula of the GeSb base nitrating nanometer thin-film material for phase transition storage of the present embodiment is
(Ge10Sb90)xN1-x, wherein x=0.60.
Remaining is same as Example 1 for preparation method, the difference is that: step 3. to sputtering chamber be passed through high-purity argon gas and
When high pure nitrogen, Ar throughput is set as 23sccm, N2Flow is 7sccm.
(embodiment 5)
The chemical composition general formula of the GeSb base nitrating nanometer thin-film material for phase transition storage of the present embodiment is
(Ge10Sb90)xN1-x, wherein x=0.55.
Remaining is same as Example 1 for preparation method, the difference is that: step 3. to sputtering chamber be passed through high-purity argon gas and
When high pure nitrogen, Ar throughput is set as 21sccm, N2Flow is 9sccm.
(comparative example 1)
That prepared by this comparative example is the Ge of non-nitrating10Sb90Phase change film material, preparation method remaining with 1 phase of embodiment
Together, the difference is that:
Step 3. in, adjust the high-purity argon gas being passed through to sputtering chamber flow be 30sccm, sputtering pressure 0.3Pa.
Ge10Sb90After target material surface cleans, Ge is closed10Sb90The radio-frequency power supply applied on target, by substrate to be sputtered
Rotate to Ge10Sb90Target position opens Ge10Sb90Target position radio-frequency power supply obtains Ge after sputtering 100s10Sb90Phase change film material is thin
Film thickness is 50nm.
(experimental example 1)
In order to understand the performance of the GeSb base nitrating nanometer thin-film material for phase transition storage of the invention, according to implementation
The film thickness GeSb base nitrating nanometer film different for the itrogen content of getter with nitrogen doped of 50nm is made to the preparation method of embodiment 5 in example 1 respectively
Material tests thin-film material made from thin-film material made from embodiment 1 to embodiment 5 and comparative example 1, obtains each phase
Pair of the out-of-service time and inverse temperature of the In-situ resistance of thinning membrane material and the relation curve of temperature and each phase change film material
Answer relation curve.
The In-situ resistance of each phase change film material and the relation curve of temperature are shown in Fig. 2, when the failure of each phase change film material
Between with the corresponding relationship curve of inverse temperature see Fig. 3.In figure 2 and figure 3, GSN0 is the thin-film material of the non-nitrating of comparative example 1；
GSN1 is GeSb base nitrating nanometer film prepared by embodiment 1, and the flow for the high pure nitrogen that sputtering chamber is passed through when sputtering is
1sccm；GSN2 is GeSb base nitrating nanometer film prepared by embodiment 2, the stream for the high pure nitrogen that sputtering chamber is passed through when sputtering
Amount is 2sccm；GSN4 is GeSb base nitrating nanometer film prepared by embodiment 3, the high pure nitrogen that sputtering chamber is passed through when sputtering
Flow be 4sccm；GSN7 is GeSb base nitrating nanometer film prepared by embodiment 4, and sputtering chamber is passed through high-purity when sputtering
The flow of nitrogen is 7sccm；GSN9 is GeSb base nitrating nanometer film prepared by embodiment 5, and sputtering chamber is passed through when sputtering
The flow of high pure nitrogen is 9sccm.
The In-situ resistance of each phase change film material and the relation test method of temperature are as follows: external by a heating platform
One 6517 megameter of Keithley has built the test system of an in situ measurement resistance v. temperature and resistivity-time relationship
System.The temperature of heating platform is adjusted by 94 type temperature control system of Linkam scientific instrument Co., Ltd, Britain TP,
Cooling is controlled by LNP94/2 type cooling system using liquid nitrogen, and temperature rate ranges up to 90
DEG C/min, temperature control is very accurate.Heating rate employed in this test process is 20 DEG C/min.In heating and cooling
Cheng Zhong, the fixed voltage being added on film probe is 2.5V, the electric current varied with temperature is measured using megameter, then be converted into phase
The resistance answered.
See Fig. 2, at low temperature, all thin-film materials are in high-resistance amorphous state.With the continuous raising of temperature, film
The resistance of material slowly reduces, and when reaching its phase transition temperature, the resistance of thin-film material is reduced rapidly, and reaches basic after a certain value
It keeps the resistance constant, shows that thin-film material has occurred by the transformation of amorphous state to crystalline state.The crystallization temperature of film is by non-nitrating
When 192 DEG C increase 280 DEG C of GSN9, illustrate that the thermal stability of phase change film material of the invention is higher.Meanwhile this hair
205 Ω when the crystalline resistance of bright phase change film material is by non-nitrating increase the 8.1 × 10 of GSN93Ω is expanded to original
40 times come, so as to which the power consumption of RESET process is effectively reduced.
The out-of-service time of each phase change film material and the corresponding relationship test method of inverse temperature are as follows: different constant
The resistance of phase change film material is measured under annealing temperature with the change curve of annealing time, when the resistance of thin-film material is reduced to original
Come be worth 50% when, we i.e. think that resistance is no longer valid.By the work reciprocal of out-of-service time and corresponding temperature under different temperatures
Figure, and curve is extended to 10 years (about 315360000s), obtain corresponding temperature.According to unified judgment criteria in the industry it
One, temperature corresponding when being kept data 10 years using phase-change material is judged to the data holding ability of material.
See Fig. 3, the Ge of the non-nitrating of comparative example 110Sb90The temperature that data are kept for 10 years is only had 90 DEG C by phase change film material,
And GSN of the inventionx ( x=4,7,9) temperature that data are kept for 10 years is improved by phase-change thin film, wherein GSN9
The temperature that data are kept for 10 years has been increased to 196 DEG C by nano film material.Traditional Ge2Sb2Te5Thin-film material protects data
The temperature held 10 years is 85 DEG C.GeSb base nitrating nanometer thin-film material for phase transition storage of the invention has than tradition
Ge2Sb2Te5The more excellent data holding ability of thin-film material.
Claims (3)
1. a kind of GeSb base nitrating nanometer thin-film material for phase transition storage, it is characterised in that: chemical composition general formula is
(Ge10Sb90)xN1-x, wherein x=0.68.
2. a kind of preparation method for the GeSb base nitrating nanometer thin-film material of phase transition storage as described in claim 1,
Characterized by the following steps:
1. it is stand-by to be cleaned drying by the preparation of substrate for substrate；
2. 1. substrate to be sputtered that step is cleaned is placed on base in magnetron sputtering coating system by the preparation of magnetron sputtering
In support, by Ge10Sb90Alloy target material is mounted in magnetron RF sputtering system target, and by the sputtering chamber of magnetron sputtering coating system into
Row vacuumizes；
3. (Ge10Sb90)xN1-xThe preparation of nano film material is passed through high-purity argon gas and high pure nitrogen as sputtering to sputtering chamber
The total flow of gas, high-purity argon gas and high pure nitrogen is 30sccm, and wherein the flow of high pure nitrogen is 2sccm, and sputtering pressure is
0.15Pa~0.35Pa；
Ge is cleaned first10Sb90Target material surface, to Ge10Sb90After target material surface cleans, Ge is closed10Sb90Applied on target
Radio-frequency power supply, by SiO to be sputtered2/ Si(100) substrate rotates to Ge10Sb90Target position is then turned on Ge10Sb90Target position radio frequency
Power supply starts sputtering and obtains (Ge10Sb90)xN1-xNano film material.
3. the preparation method of the GeSb base nitrating nanometer thin-film material according to claim 2 for phase transition storage,
Be characterized in that: 2. target is mounted in magnetron RF sputtering system target by step after, by the sputtering chamber of magnetron sputtering coating system into
Row vacuumizes until vacuum degree reaches 1 × 10 in chamber-4 Pa。
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| CN106206942B (en) * | 2016-07-30 | 2018-09-18 | 江苏理工学院 | Rare earth Er doped and modified GeSb nano film and preparation method thereof |
| CN106601908A (en) * | 2016-12-16 | 2017-04-26 | 同济大学 | Antimony-germanium multilayer nano-composite phase-change material and preparation and application thereof |
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