CN105742489A - Zr-doped Ge2Sb2Te5 thin-film material for phase change memory and preparation method of Zr-doped Ge2Sb2Te5 thin-film material - Google Patents
Zr-doped Ge2Sb2Te5 thin-film material for phase change memory and preparation method of Zr-doped Ge2Sb2Te5 thin-film material Download PDFInfo
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- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 8
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- H10N70/00—Solid-state devices having no potential barriers, and specially adapted for rectifying, amplifying, oscillating or switching
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Abstract
The invention discloses a Zr-doped Ge2Sb2Te5 thin-film material for a phase change memory and a preparation method of the Zr-doped Ge2Sb2Te5 thin-film material. The Zr-doped Ge2Sb2Te5 thin-film material is characterized in that a chemical structural formula is Zrx(Ge2Sb2Te5)(100-x), wherein x is smaller than to 20 and greater than to 0. The preparation method comprises the following specific steps: adopting a high-purity round block Zr element and Ge2Sb2Te5 as target materials, with high-purity argon as a working gas and a quartz plate or a silicon wafer as a substrate material, carrying out surface deposition by a magnetron sputtering apparatus and a double-target co-sputtering method; adjusting the DC sputtering power of the Zr element target to be 3-9W and the radio-frequency sputtering power of the Ge2Sb2Te5 target to be 60W; and carrying out co-sputtering at a room temperature for 15 minutes and then obtaining the Zr-doped Ge2Sb2Te5 thin-film material. The Zr-doped Ge2Sb2Te5 thin-film material has the advantages of relatively high crystallization temperature and data retentivity, relatively high crystallization speed, relatively high amorphous/crystalline resistance ratio and relatively good heat stability.
Description
Technical field
The present invention relates to phase-change storage material field, especially relate to a kind of Zr doping Ge for phase transition storage2Sb2Te5Thin-film material and preparation method thereof.
Background technology
Along with the fast development of computer technology, mobile communication and digital product, the demand of nonvolatile semiconductor memory is dramatically increased.At present the main flow in nonvolatile storage market is flash memory, but the some shortcomings that flash memory self exists, write time (> 10 μ s as longer) and relatively low cycle-index (~ 106) so that it is being difficult to meet future semiconductor memorizer and develop the highest erasable speed and the requirement of memory density, additionally, due to the basic demand of storage electric charge, floating boom can not be unconfined thinning, breaks through 45 nm manufacture of semiconductor and there is the biggest technical difficulty.PCRAM causes the concern of scientific circles and industry day by day, not only because it meets the various requirement of nonvolatile memory, also as its manufacturing process is relatively easy.PCRAM based on chalcogenide compound is by one of nonvolatile storage being extensively considered most prospect, the most commercially replace Flash and become nonvolatile storage of future generation, because PCRAM has, the performance of almost Perfect, such as micro be good, data retention is strong, low cost and with the feature such as CMOS technology compatibility is good.Additionally, PCRAM memory technology has anti-strong motion, radiation resistance, in field of aerospace, there is extremely important application prospect.
The combination property of PCRAM depends primarily on the phase-change characteristic of storage medium.In all of phase transformation chalcogenide compound, Ge2Sb2Te5(GST) it is to apply material the most frequently used in PCRAM.But, higher fusing point and relatively low crystalline resistance rate make GST higher RESET electric current and power consumption inevitably occur.Additionally in fields such as automotive electronics, data retention is had particular/special requirement: data can keep 10 years in the environment of 120 DEG C.Conventional GST material is because its crystallization temperature is low, and thermostability is the best, and the data of the PRAM memory element with GST material as storage medium are merely able to preserve 10 years at about 80 DEG C, and it is short, so GST can not meet this requirement that the data under high temperature preserve the life-span.For optimizing the performance of PCRAM, generally adulterate in GST other elements, improves phase-change material crystalline resistance rate, reduces RESET electric current and improves data retention, and after making doping, GST materials application is possibly realized in phase transition storage.
Summary of the invention
The technical problem to be solved is to provide a kind of Zr doping Ge for phase transition storage with higher crystallization temperature and data retention, faster crystallization rate, bigger amorphous state/crystalline resistance ratio and preferable heat stability2Sb2Te5Thin-film material and preparation method thereof, the method low cost, process controllability is strong, it is easy to large-scale production.
The present invention solves the technical scheme that above-mentioned technical problem used: a kind of Zr for phase transition storage adulterates Ge2Sb2Te5Thin-film material, its chemical structural formula is Zrx(Ge2Sb2Te5)100-x, wherein 0 < x < 20.
The crystallization temperature of described phase change film material is 150-300 DEG C.
The amorphous resistance of described phase change film material is 106~108Ω, crystalline resistance 103~104Ω。
The chemical structural formula of described thin-film material is Zr12(Ge2Sb2Te5)88.The data retention of this phase change film material can preserve 10 years at 120.9 DEG C.
The above-mentioned Zr doping Ge for phase transition storage2Sb2Te5The preparation method of thin-film material, uses high-purity nahlock shape Zr simple substance and Ge2Sb2Te5As target, using magnetic control sputtering device, use double target co-sputtering method, using high-purity argon gas as working gas, using piezoid or silicon chip is that backing material carries out surface deposition, specifically comprises the following steps that
(1) by Ge2Sb2Te5Nahlock shape glass target and the Zr simple substance target back side, completely laminating one piece are identical with glass target diameter, and thickness is the copper sheet of 1mm, prepare magnetron sputtering plating target；Zr simple substance target is arranged in magnetic control DC sputtering target, by Ge2Sb2Te5Target is arranged in magnetron RF sputtering system target；
(2) piezoid or silicon chip substrate material are put in deionized water, ultrasonic cleaning 20 minutes, it is then placed in ultrasonic cleaning 20 minutes in dehydrated alcohol, dries up with high pure nitrogen after taking-up, put into sputtering chamber；
(3) magnetron sputtering chamber is carried out evacuation, until vacuum reaches 2 × 10 in sputtering chamber-4During Pa, being passed through high-purity argon gas to indoor, argon flow amount is 50ml/min, until sputtering chamber internal gas pressure reaches to sputter required build-up of luminance air pressure 0.3Pa；
(4) open radio-frequency power supply, after aura is stable, the d.c. sputtering power of Zr simple substance target is adjusted to 3 ~ 9W, Ge2Sb2Te5The radio-frequency sputtering power of target is adjusted to 60W, carries out sputter coating at room temperature, after cosputtering 15min, obtains the Zr doping Ge for phase transition storage2Sb2Te5Thin-film material.
Described Zr target and described Ge2Sb2Te5The purity of target is 99.99%.
The Zr doping Ge of the deposited that step (4) step is obtained2Sb2Te5Thin-film material is put in quick anneal oven, under high-purity argon gas atmosphere is protected, is brought rapidly up annealing at 200 ~ 350 DEG C, i.e. obtains the doping GST phase transiting storing thin-film material of the Zr after heat treatment.
Compared with prior art, it is an advantage of the current invention that: a kind of Zr doping GST thin-film material for phase transition storage of the present invention and preparation method thereof, its chemical formula structure is Zrx(Ge2Sb2Te5)100-x, wherein 0 < x < 20, the crystallization temperature of this thin film is 165 ~ 200 DEG C, and it is 84.4 ~ 120.9 DEG C that data preserve the maximum temperature of 10 years；Test result shows, along with the increase of Zr doping content, the crystalline resistance of sample is also increasing, and advantageously reduces the power consumption of PRAM.It is strong that the present invention has process controllability, production cost is low, reproducible, the Zr doping GST thin-film material prepared not only has that component deviation is little, adhesive strength is high, the advantage of film quality even compact, and there is higher crystallization temperature, faster crystallization rate, bigger amorphous state/crystalline resistance ratio and preferably heat stability, may be used for industrially scalable and prepare large-area phase-change thin film, thus meet the application demand of following phase-change storage material.
Accompanying drawing explanation
Fig. 1 is the Zr of different componentx(GST)100-xFilm rectangular resistance varies with temperature relation curve；
Fig. 2 is the Zr of different componentx(GST)100-xThe data retention result of calculation figure of thin film；
Fig. 3 is component Zr9(GST)91Film sample anneal at different temperatures after X ray diffracting spectrum；
Fig. 4 is the Zr of different componentx(GST)100-xThin film anneal at 250 DEG C after X ray diffracting spectrum；
Fig. 5 is the Zr of different componentx(GST)100-xThin film anneal at 300 DEG C after X ray diffracting spectrum；
Fig. 6 is the Zr of different componentx(GST)100-xThin film anneal at 350 DEG C after X ray diffracting spectrum.
Detailed description of the invention
Below in conjunction with accompanying drawing embodiment, the present invention is described in further detail.
One, specific embodiment
A kind of Zr doping Ge for phase transition storage2Sb2Te5Thin-film material, its chemical structural formula is Zrx(Ge2Sb2Te5)100-x, wherein 0 < x < 20, the crystallization temperature of this thin-film material is 150-300 DEG C, and amorphous resistance is 106~108Ω, crystalline resistance 103~104Ω.Its preparation method is as follows: use high-purity nahlock shape Zr simple substance and Ge2Sb2Te5As target, using magnetic control sputtering device, use double target co-sputtering method, using high-purity argon gas as working gas, using piezoid or silicon chip is that backing material carries out surface deposition, specifically comprises the following steps that
(1) by Ge2Sb2Te5Nahlock shape glass target and the Zr simple substance target back side, completely laminating one piece are identical with glass target diameter, and thickness is the copper sheet of 1mm, prepare magnetron sputtering plating target；Zr simple substance target is arranged in magnetic control DC sputtering target, by Ge2Sb2Te5Target is arranged in magnetron RF sputtering system target；
(2) piezoid or silicon chip substrate material are put in deionized water, ultrasonic cleaning 20 minutes, it is then placed in ultrasonic cleaning 20 minutes in dehydrated alcohol, dries up with high pure nitrogen after taking-up, put into sputtering chamber；
(3) magnetron sputtering chamber is carried out evacuation, until vacuum reaches 2 × 10 in sputtering chamber-4During Pa, being passed through high-purity argon gas to indoor, argon flow amount is 50ml/min, until sputtering chamber internal gas pressure reaches to sputter required build-up of luminance air pressure 0.3Pa；
(4) open radio-frequency power supply, after aura is stable, the d.c. sputtering power of Zr simple substance target is adjusted to 3 ~ 9W, Ge2Sb2Te5The radio-frequency sputtering power of target is adjusted to 60W, carries out sputter coating at room temperature, after cosputtering 15min, obtains the Zr doping Ge for phase transition storage2Sb2Te5Thin-film material.
The Zr doping Ge of deposited obtained above2Sb2Te5Thin-film material is put in quick anneal oven, under high-purity argon gas atmosphere is protected, is brought rapidly up annealing at 200 ~ 350 DEG C, i.e. obtains the doping GST phase transiting storing thin-film material of the Zr after heat treatment.
The JGP-450 magnetron sputtering deposition system that above-mentioned magnetic control sputtering device used is manufactured by Shenyang Scientific Instrument Research & Mfg. Center Co., Ltd., C.A.S.The sputtering target material used is purity 99.99%, size Φ 50 × 3mm.At nahlock shape Ge2Sb2Te5The copper sheet that diameter thick for 1mm is identical is pasted, to solve glass target heat dissipation problem in sputter procedure with the Zr simple substance back side.
Embodiment 1
A kind of Zr doping Ge for phase transition storage2Sb2Te5Thin-film material, its preparation method is as follows:
(1) Ge is used2Sb2Te5With Zr simple substance double target co-sputtering plated film: Zr simple substance target is arranged in magnetic control DC sputtering target, by Ge2Sb2Te5Target is arranged in magnetron RF sputtering system target；Sputtering chamber is carried out evacuation process, when in sputtering chamber, vacuum reaches 2 × 10-4During Pa, being filled with high-purity argon gas to indoor, argon flow amount is 50.0ml/min, until reaching in chamber to sputter required build-up of luminance air pressure 0.3Pa；Opening radio-frequency power supply, after aura is stable, the d.c. sputtering target power output at regulation Zr simple substance place is 3W, Ge2Sb2Te5Target place magnetron RF sputtering system power is 60W, after power stability, opens substrate rotating disk rotation and autorotation speed is set as 5rpm, opening the baffle plate below substrate, obtains the Zr doping GST thin film of deposited after sputtering 15 minutes；
(2) the phase change memory film sample of deposited step (1) obtained is put in quick anneal oven, under the protection of high pure nitrogen atmosphere, is brought rapidly up at 200 ~ 350 DEG C annealing, and obtains the doping Ge of the Zr after heat treatment2Sb2Te5Thin-film material.The effect being passed through high pure nitrogen during annealing is for avoiding thin film at high temperature to aoxidize.
The Zr doping Ge that above-described embodiment 1 prepares2Sb2Te5Film composition is recorded by X-ray energy spectrum analytic process (EDS), and film thickness is recorded by step instrument, and test result is: film composition is Zr4(GST)96, film thickness is 210nm.
Embodiment 2
With embodiment 1, its distinctive points is, the d.c. sputtering target power output at regulation Zr simple substance place is 5W, Ge2Sb2Te5Target place magnetron RF sputtering system power is 60W.
The Zr doping Ge that above-described embodiment 1 prepares2Sb2Te5Film composition is recorded by X-ray energy spectrum analytic process (EDS), and film thickness is recorded by step instrument, and test result is: film composition is Zr6(GST)94, film thickness is 235nm.
Embodiment 3
With embodiment 1, its distinctive points is, the d.c. sputtering target power output at regulation Zr simple substance place is 7W, Ge2Sb2Te5Target place magnetron RF sputtering system power is 60W.
The Zr doping Ge that above-described embodiment 1 prepares2Sb2Te5Film composition is recorded by X-ray energy spectrum analytic process (EDS), and film thickness is recorded by step instrument, and test result is: film composition is Zr9(GST)91, film thickness is 260nm.
Embodiment 4
With embodiment 1, its distinctive points is, the d.c. sputtering target power output at regulation Zr simple substance place is 9W, Ge2Sb2Te5Target place magnetron RF sputtering system power is 60W.
The Zr doping Ge that above-described embodiment 1 prepares2Sb2Te5Film composition is recorded by X-ray energy spectrum analytic process (EDS), and film thickness is recorded by step instrument, and test result is: film composition is Zr12(GST)88, film thickness is 290nm.
Two, interpretation
Zr prepared by above-described embodimentx(GST)100-xThin film carries out performance test, Fig. 1 and Fig. 2 is In-situ resistance the performance test results.Fig. 1 is that the thin film of different component is at 10 DEG C/Min heating rate lower block resistance and the relation of temperature.Owing to the resistance of thin film drastically declines at crystallization temperature (Tc) place, from figure 1 it appears that component is Zr4(GST)96Thin film there is twice crystalline polamer, along with the increase of Zr content, twice crystalline polamer is suppressed, the crystallization temperature of material is the most significantly raised, the heat stability of material is improved, and then can improve the data retention of phase transition storage, and this is confirmed the most in fig. 2.As shown in Figure 2, along with the increase of Zr content, material 10 annual data retentivity also improves constantly.
Fig. 3 is component Zr9(GST)91Film sample anneal at different temperatures after X-ray diffractogram.As seen from the figure, the X-ray diffractogram after 150 DEG C of annealing presents wide big envelope, crystallize peak does not occurs, a point Zr is described9(GST)91Film sample is amorphous state at such a temperature；When temperature is higher than 200 DEG C, occur in that obvious crystallize peak, this show the recrystallization temperature of film sample of this component between 150 DEG C to 200 DEG C, this result is consistent with Fig. 1.
Fig. 4, Fig. 5 and Fig. 6 are the Zr of different componentx(GST)100-xThe thin film X ray diffracting spectrum respectively at 250 DEG C, after annealing at 300 DEG C and 350 DEG C.The phase transformation from amorphous state to polycrystalline state of the thin film of embodiment 1 preparation is the crystallization process of two steps, first changes to metastable state face-centred cubic structure (fcc) from amorphous state, then continues to change to the close pile structure of six side (hex) from fcc.It will be seen from figure 6 that anneal at a temperature of 350 DEG C after 3min, Zrx(GST)100-xEach component of thin film has crystal to separate out.And along with the increase of Zr content, the intensity at crystallize peak has and significantly weakens, the doping of this explanation Zr inhibits the crystallize of GST, thus improves Zrx(GST)100-xThe crystallization temperature of thin film so that the heat stability of material is substantially improved.
Described above not limitation of the present invention, the present invention is also not limited to the example above.Those skilled in the art, in the essential scope of the present invention, the change made, retrofit, add or replace, and also should belong to protection scope of the present invention, and protection scope of the present invention is as the criterion with claims.
Claims (7)
1. the Zr doping Ge for phase transition storage2Sb2Te5Thin-film material, it is characterised in that: its chemical structural formula is Zrx(Ge2Sb2Te5)100-x, wherein 0 < x < 20.
Zr doping Ge for phase transition storage the most according to claim 12Sb2Te5Thin-film material, it is characterised in that: the crystallization temperature of described phase change film material is 150-300 DEG C.
Zr doping Ge for phase transition storage the most according to claim 12Sb2Te5Thin-film material, it is characterised in that: the amorphous resistance of described phase change film material is 106~108Ω, crystalline resistance 103~104Ω。
Zr doping Ge for phase transition storage the most according to claim 12Sb2Te5Thin-film material, it is characterised in that: the chemical structural formula of described thin-film material is Zr12(Ge2Sb2Te5)88。
5. one kind according to according to any one of claim 1-4 for phase transition storage Zr adulterate Ge2Sb2Te5The preparation method of thin-film material, it is characterised in that: use high-purity nahlock shape Zr simple substance and Ge2Sb2Te5As target, using magnetic control sputtering device, use double target co-sputtering method, using high-purity argon gas as working gas, using piezoid or silicon chip is that backing material carries out surface deposition, specifically comprises the following steps that
(1) by Ge2Sb2Te5Nahlock shape glass target and the Zr simple substance target back side, completely laminating one piece are identical with glass target diameter, and thickness is the copper sheet of 1mm, prepare magnetron sputtering plating target；Zr simple substance target is arranged in magnetic control DC sputtering target, by Ge2Sb2Te5Target is arranged in magnetron RF sputtering system target；
(2) piezoid or silicon chip substrate material are put in deionized water, ultrasonic cleaning 20 minutes, it is then placed in ultrasonic cleaning 20 minutes in dehydrated alcohol, dries up with high pure nitrogen after taking-up, put into sputtering chamber；
(3) magnetron sputtering chamber is carried out evacuation, until vacuum reaches 2 × 10 in sputtering chamber-4During Pa, being passed through high-purity argon gas to indoor, argon flow amount is 50ml/min, until sputtering chamber internal gas pressure reaches to sputter required build-up of luminance air pressure 0.3Pa；
(4) open radio-frequency power supply, after aura is stable, the d.c. sputtering power of Zr simple substance target is adjusted to 3 ~ 9W, Ge2Sb2Te5The radio-frequency sputtering power of target is adjusted to 60W, carries out sputter coating at room temperature, after cosputtering 15min, obtains the Zr doping Ge for phase transition storage2Sb2Te5Thin-film material.
Zr doping GST thin-film material for phase transition storage the most according to claim 5 and preparation method thereof, it is characterised in that: described Zr target and described Ge2Sb2Te5The purity of target is 99.99%.
Zr doping GST thin-film material for phase transition storage the most according to claim 5 and preparation method thereof, it is characterised in that: the Zr doping Ge of the deposited that step (4) step is obtained2Sb2Te5Thin-film material is put in quick anneal oven, under high-purity argon gas atmosphere is protected, is brought rapidly up annealing at 200 ~ 350 DEG C, i.e. obtains the doping GST phase transiting storing thin-film material of the Zr after heat treatment.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106374043A (en) * | 2016-09-26 | 2017-02-01 | 江苏理工学院 | Si-Sb-Se nano phase-change thin film material and preparation method and application thereof |
| CN106960907A (en) * | 2017-02-28 | 2017-07-18 | 宁波大学 | A kind of rare earth Er doping Ge2Sb2Te5Phase transiting storing thin-film material and preparation method thereof |
| CN110176536A (en) * | 2019-04-18 | 2019-08-27 | 宁波大学 | A kind of vanadium dioxide-Sb thin-film material and preparation method thereof having both high speed and high data retention |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106374043A (en) * | 2016-09-26 | 2017-02-01 | 江苏理工学院 | Si-Sb-Se nano phase-change thin film material and preparation method and application thereof |
| CN106960907A (en) * | 2017-02-28 | 2017-07-18 | 宁波大学 | A kind of rare earth Er doping Ge2Sb2Te5Phase transiting storing thin-film material and preparation method thereof |
| CN106960907B (en) * | 2017-02-28 | 2019-03-15 | 宁波大学 | A kind of rare earth Er doping Ge2Sb2Te5Phase transiting storing thin-film material and preparation method thereof |
| CN110176536A (en) * | 2019-04-18 | 2019-08-27 | 宁波大学 | A kind of vanadium dioxide-Sb thin-film material and preparation method thereof having both high speed and high data retention |
| CN110176536B (en) * | 2019-04-18 | 2023-04-18 | 宁波大学 | Vanadium dioxide-Sb thin film material and preparation method thereof |
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| CN105742489B (en) | 2018-06-29 |
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