CN102534479A - Microcrystalline Si-SbxTe1-x composite phase change material and preparation method thereof - Google Patents
Microcrystalline Si-SbxTe1-x composite phase change material and preparation method thereof Download PDFInfo
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- CN102534479A CN102534479A CN2010105913906A CN201010591390A CN102534479A CN 102534479 A CN102534479 A CN 102534479A CN 2010105913906 A CN2010105913906 A CN 2010105913906A CN 201010591390 A CN201010591390 A CN 201010591390A CN 102534479 A CN102534479 A CN 102534479A
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Abstract
The invention discloses a microcrystalline Si-SbxTe1-x composite phase change material and a preparation method thereof. The composite phase change material is formed by composition of microcrystalline-state Si and a phase change material SbxTe1-x, wherein x is not less than 0.1 and not more than 0.9. The preparation method comprises the steps of forming an amorphous Si-SbxTe1-x material by PVD (physical vapor deposition), then annealing in a hydrogen atmosphere to form the microcrystalline Si-SbxTe1-x composite phase change material, and finally heating and dehydrogenating to complete the preparation of the material. In the microcrystalline Si-SbxTe1-x composite phase change material disclosed by the invention, the existence of the microcrystalline Si can effectively inhibit oxidation, so that mutual diffusion of the Si and the SbxTe1-x can be hindered, and the microcrystalline Si-SbxTe1-x composite phase change material is more stable. Simultaneously, the microcrystalline-state Si can change the current distribution in phase change so as to be conductive to reducing power consumption, prolonging service life and improving operation stability of a phase change memory.
Description
Technical field
The present invention relates to phase change material and preparation method, refer in particular to a kind of crystallite Si and Sb
xTe
1-xComposite phase-change material and preparation method, belong to the association area of semiconductor memory.
Background technology
Nonvolatile semiconductor memory has occupied consequence in infotech, its sales volume increases year by year, and it is applied in the consumer electronics ubiquitous especially, has vast market.At present, the most frequently used nonvolatile semiconductor memory is a flash memory, and the novel storer of other principles also continues to bring out.For example, phase transition storage, ferroelectric memory, RRAM (resistor random-access storage) etc., wherein, phase transition storage more is considered to non-volatile memory of future generation candidate the most likely.
The principle of phase transition storage is based on the transformation that the phase change material phase transformation causes resistance; Lean on the resistance of measuring resistance to come sense data; Than present most widely used GeSbTe series phase change material system, the novel phase-change material SiSb of information functional material laboratory PCRAM project team of Shanghai micro-system institute of Chinese Academy of Sciences independent research
xTe
1-xSystem has better thermostability and better data confining force, has been applied to the checking in early stage of through engineering approaches at present.
Yet experiment showed, SiSb
xTe
1-xThe phase change material of system is that amorphous Si is mutually compound with the SbTe crystalline at crystal form and since amorphous Si 500-600 degree centigrade still uncrystallizable, and exist many defectives to make SiSb among the non-crystalline state Si
xTe
1-xMaterial is unstable, thereby causes aspect its stability of raising and the erasable number of times very big improved space being arranged based on the phase change memory device of this material.
Summary of the invention
The technical problem that the present invention mainly solves is to provide a kind of crystallite Si and Sb
xTe
1-xComposite phase-change material and preparation method, to improve the stability of this phase change material.
In order to solve the problems of the technologies described above, the present invention adopts following technical scheme:
A kind of crystallite Si-Sb
xTe
1-xComposite phase-change material is by the Si and the phase change material Sb of crystallite attitude
xTe
1-xBe composited, wherein 0.1≤x≤0.9.
Preferably, the grain-size of the Si of said crystallite attitude is 3-20nm.
A kind of above-mentioned crystallite Si-Sb
xTe
1-xThe preparation method of composite phase-change material may further comprise the steps:
At first utilize PVD (physical vapor deposition) to form amorphous Si-Sb
xTe
1-xMaterial; Form crystallite Si-Sb through annealing in hydrogen atmosphere then
xTe
1-xComposite phase-change material; Heat dehydrogenation at last; 0.1≤x≤0.9 wherein.
Preferably, PVD forms amorphous Si-Sb
xTe
1-xAfter the material, earlier at this amorphous Si-Sb
xTe
1-xAnneal more than the Tc of material, make it form amorphous Si and Sb
xTe
1-xThe crystal phase-splitting, and then through annealing formation crystallite Si-Sb in hydrogen atmosphere
xTe
1-xComposite phase-change material.
Preferably, annealing forms crystallite Si-Sb in hydrogen atmosphere
xTe
1-xThe annealing temperature of composite phase-change material is 200-500 degree centigrade.
Preferably, annealing forms crystallite Si-Sb in hydrogen atmosphere
xTe
1-xThe annealing time of composite phase-change material is 10-30min.
Preferably, the heating dehydrogenation is to realize dehydrogenation at 300-600 degree centigrade of insulation 25-30min.
Wherein, the Sb that relates to
xTe
1-xThe series phase change material comprises the material of the various ingredients with phase-change characteristic, like Sb
2Te
3Deng.Lower temperature has been adopted in annealing in nitrogen atmosphere; Because the existence of H makes non-crystalline state Si form crystallite and not cause phase change material component segregation or performance change at high temperature in this temperature in the atmosphere, and after the heating dehydrogenation, can not influence the phase transformation performance of phase change material.
Beneficial effect of the present invention is:
With the amorphous Si-Sb after the phase-splitting
xTe
1-xMaterial is annealed in nitrogen atmosphere, can realize that amorphous Si is to the transformation of crystallite at a lower temperature, and this temperature is lower than Sb
xTe
1-xThe fusing point of compound can not have influence on the phase-change characteristic of material.The novel crystallite Si and the Sb that prepare in this way
xTe
1-xThe compound phase change material has better thermostability, and wherein crystallite Si grain-size is about 3-20nm, and defective is lacked than non-crystalline state, and effectively inhibited oxidation hinders Si and Sb
xTe
1-xThe phase mutual diffusion, have more stable properties.The Si of crystallite attitude has changed the distribution of electric current in the phase transformation simultaneously, helps reducing power consumption, improves the life-span, improves phase velocity, improves the operational stability of phase transition storage.Therefore be a kind of good NEW TYPE OF COMPOSITE phase change material.
Description of drawings
Fig. 1 is the XRD figure after embodiment one anneals in nitrogen atmosphere, is used to prove the formation of crystallite Si.
Fig. 2 is that embodiment two is with crystallite Si-Sb
xTe
1-xComposite phase-change material is applied in the device performance test pattern in the phase transition storage.
Embodiment
Through specific embodiment, further illustrate substantive distinguishing features of the present invention and obvious improvement, but the present invention only is confined to described embodiment by no means below.
Embodiment one
Present embodiment is through preparation crystallite Si-Sb
2Te
3Composite phase-change material, and it is tested further specify technical scheme of the present invention.Concrete preparation method is following:
(1) utilizes the PVD equipment Si that on sheet glass, grows
2Sb
2Te
3Material.For example can adopt methods such as magnetron sputtering, obtain the thin-film material of stoichiometric(al) through modulation process parameter (sputtering power, operating air pressure etc.), the technology that wherein adopts PVD technology growing film is for those skilled in the art's convention, so do not give unnecessary details at this.Present embodiment preferred growth Si
2Sb
2Te
3Material, however the present invention is not limited only to this, can also be the Si-Sb of other proportionings of growth
xTe
1-xMaterial, 0.1≤x≤0.9.Si-Sb in the PVD deposited
xTe
1-xIn the material, Si exists with the form of amorphous.
(2) with this Si
2Sb
2Te
3Material places N
2With 300 degrees centigrade of annealing 3 minutes, make its formation comprise non-crystalline state Si and crystalline state Sb in the atmosphere
2Te
3The compound phase of two kinds of phase-splittings.Wherein form the annealing temperature and the annealing time of phase-splitting, can adjust based on actual conditions.
(3) with the Si after the phase-splitting
2Sb
2Te
3Phase change material places hydrogen atmosphere to anneal, and makes amorphous Si wherein change crystallite Si into, thereby forms crystallite Si-Sb
2Te
3Composite phase-change material.The annealing temperature of this step is preferably 200-500 degree centigrade, and annealing time is preferably 10-30min, can do suitable adjustment to annealing temperature and annealing time according to the difference of real material proportioning, thereby selects optimum processing parameter.Present embodiment is to Si
2Sb
2Te
3Material was preferably annealed 15 minutes down at 350 degrees centigrade.
(4) annealing forms crystallite Si-Sb in hydrogen atmosphere
2Te
3After the composite phase-change material, also need heat dehydrogenation and handle it.Through the formed crystallite Si-Sb of heating steps (3)
2Te
3Composite phase-change material makes it at 300-600 degree centigrade of insulation 25-30min, realizes dehydrogenation.The Heating temperature of dehydrogenation and time also are to regulate according to the difference of real material, are preferably in the present embodiment at 400 degrees centigrade of insulation 30min.Promptly obtain the composite phase-change material film of good heat stability after the dehydrogenation
To above-mentioned crystallite Si-Sb
2Te
3The composite phase-change material sample carries out the XRD test.Test result is as shown in Figure 1, visible through in hydrogen atmosphere, annealing, the Si in this sample changes crystallite into by non-crystalline state, has occurred the characteristic peak in (111), (220), (311) crystal orientation in the XRD figure, and the grain-size of crystallite Si is 3-20nm.
In sum, with the amorphous Si-Sb after the phase-splitting
xTe
1-xMaterial is annealed in nitrogen atmosphere, can realize that amorphous Si is to the transformation of crystallite at a lower temperature, and this temperature (200-500 degree centigrade) is lower than Sb
xTe
1-xThe fusing point of compound can not have influence on the phase-change characteristic of material.Crystallite Si compares with amorphous Si, and defective is few, and effectively inhibited oxidation hinders Si and Sb
xTe
1-xThe phase mutual diffusion, have more stable properties.
Embodiment two
Crystallite Si-Sb with preparation among the embodiment one
2Te
3Composite phase-change material is applied in the phase transition storage, further analyzes its performance.
(a) utilize PVD equipment with Si
2Sb
2Te
3Material is grown in preparation to be had in the flow substrate of electrode;
(b) repeat to implement step (2)-(4) in, form crystallite Si-Sb
2Te
3Composite phase-change material;
(c) subsequent step of flow is accomplished in continuation, comprises growth TiN, etching, and growth Al, complete phase-changing memory unit is produced in corrosion etc.;
(d) to the phase-changing memory unit of accomplishing write, wiping, read operation, study storage characteristics and the fatigue characteristic of this material etc.
Fig. 2 is a test result, and is visible with crystallite Si-Sb
2Te
3Composite phase-change material is applied in the phase transition storage, and the Si of crystallite attitude has changed the distribution of electric current in the phase transformation, helps reducing power consumption, improves the life-span, improves phase velocity, improves the operational stability of phase transition storage.
Here description of the invention and application is illustrative, is not to want with scope restriction of the present invention in the above-described embodiments.Here the distortion of the embodiment that is disclosed and change are possible, and the replacement of embodiment is known with the various parts of equivalence for those those of ordinary skill in the art.Those skilled in the art are noted that under the situation that does not break away from spirit of the present invention or essential characteristic, and the present invention can be with other forms, structure, layout, ratio, and realize with other substrates, material and parts.Under the situation that does not break away from the scope of the invention and spirit, can carry out other distortion and change here to the embodiment that is disclosed.
Claims (7)
1. crystallite Si-Sb
xTe
1-xComposite phase-change material is characterized in that: by the Si and the phase change material Sb of crystallite attitude
xTe
1-xBe composited, wherein 0.1≤x≤0.9.
2. according to the said a kind of crystallite Si-Sb of claim 1
xTe
1-xComposite phase-change material is characterized in that: the grain-size of the Si of said crystallite attitude is 3-20nm.
3. crystallite Si-Sb
xTe
1-xThe preparation method of composite phase-change material is characterized in that, may further comprise the steps: at first utilize PVD to form amorphous Si-Sb
xTe
1-xMaterial; Form crystallite Si-Sb through annealing in hydrogen atmosphere then
xTe
1-xComposite phase-change material; Heat dehydrogenation at last; 0.1≤x≤0.9 wherein.
4. according to the said a kind of crystallite Si-Sb of claim 3
xTe
1-xThe preparation method of composite phase-change material is characterized in that: PVD forms amorphous Si-Sb
xTe
1-xAfter the material, earlier at this amorphous Si-Sb
xTe
1-xAnneal more than the Tc of material, make it form amorphous Si and Sb
xTe
1-xThe crystal phase-splitting, and then through annealing formation crystallite Si-Sb in hydrogen atmosphere
xTe
1-xComposite phase-change material.
5. according to the said a kind of crystallite Si-Sb of claim 3
xTe
1-xThe preparation method of composite phase-change material is characterized in that: annealing forms crystallite Si-Sb in hydrogen atmosphere
xTe
1-xThe annealing temperature of composite phase-change material is 200-500 degree centigrade.
6. according to the said a kind of crystallite Si-Sb of claim 3
xTe
1-xThe preparation method of composite phase-change material is characterized in that: annealing forms crystallite Si-Sb in hydrogen atmosphere
xTe
1-xThe annealing time of composite phase-change material is 10-30min.
7. according to the said a kind of crystallite Si-Sb of claim 3
xTe
1-xThe preparation method of composite phase-change material is characterized in that: the heating dehydrogenation is for realizing dehydrogenation at 300-600 degree centigrade of insulation 25-30min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102157685A (en) * | 2011-01-30 | 2011-08-17 | 中国科学院上海微系统与信息技术研究所 | Phase-change storage material and manufacture method thereof |
| CN102386327A (en) * | 2011-11-23 | 2012-03-21 | 中国科学院上海微系统与信息技术研究所 | Preparation method of phase-change material |
| CN113201944A (en) * | 2021-03-26 | 2021-08-03 | 苏州经贸职业技术学院 | Intelligent material and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102157685A (en) * | 2011-01-30 | 2011-08-17 | 中国科学院上海微系统与信息技术研究所 | Phase-change storage material and manufacture method thereof |
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| CN102386327A (en) * | 2011-11-23 | 2012-03-21 | 中国科学院上海微系统与信息技术研究所 | Preparation method of phase-change material |
| CN113201944A (en) * | 2021-03-26 | 2021-08-03 | 苏州经贸职业技术学院 | Intelligent material and preparation method thereof |
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