CN104393171A - Nitrogen-doped nano-film material applied to quick high-stability phase transition storage and preparation method - Google Patents

Nitrogen-doped nano-film material applied to quick high-stability phase transition storage and preparation method Download PDF

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Publication number
CN104393171A
CN104393171A CN201410655783.7A CN201410655783A CN104393171A CN 104393171 A CN104393171 A CN 104393171A CN 201410655783 A CN201410655783 A CN 201410655783A CN 104393171 A CN104393171 A CN 104393171A
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China
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film material
sputtering
nitrogen
gas
phase transition
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CN201410655783.7A
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Inventor
袁丽
胡益丰
朱小芹
吴卫华
薛建忠
张建豪
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Jiangsu University of Technology
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Jiangsu University of Technology
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Abstract

The invention discloses a nitrogen-doped nano-film material applied to a quick high-stability phase transition storage. The nitrogen-doped nano-film material is characterized in that the chemical fomula is Sn15Sb85Nx, wherein x is the nitrogen flow rate based on the unit of sccm; the nitrogen-doped Sn15Sb85 is prepared by the room-temperature magnetron sputtering method; argon and nitrogen are charged at the same time during performing magnetron sputtering and depositing for the Sn15Sb85 film. The preparation method is characterized in that nitrogen-doped Sn15Sb85 nano phase transition thin materials with different N atom contents can be obtained by controlling the flow rate of Ar and N2; other preparation conditions cannot be ignored, which certainly influences the content and size of N atoms in the final nitrogen-doped Sn15Sb85 nano phase transition film material. The nitrogen-doped Sn15Sb85 nano film material can be applied to the phase transition storage and is high in crystallization temperature and crystallization resistance, and the heat stability of PCRAM can be greatly improved.

Description

A kind of nitrating nanometer thin-film material for quick high stability phase transition storage and preparation method thereof
Technical field
The present invention relates to the storage medium of microelectronics technology, be specifically related to a kind of nitrating Sn for quick low-power consumption high stability 15sb 85nano phase change thin-film material and preparation method thereof.
Background technology
Phase transition storage (PCRAM) is that when utilizing material to change back and forth from crystalline state to amorphous state, resistance also converts thereupon between high resistant and low-resistance, and two resistance states represent " 0 " and " 1 " respectively, thus the object that the information that realizes stores.It has non-volatile, have extended cycle life, reading speed is fast, good stability, high-density city, low in energy consumption and can the advantages such as function is strong be embedded, be thus considered to the memory technology of future generation having application prospect most.
There are some researches show, with traditional Ge 2sb 2te 5phase-change material is compared, and SnSb class alloy has phase velocity faster, higher crystallization temperature and better stability (Feng Rao etc., Applied PhysicsLetters, 95,032105,2009).By mixing appropriate atom N or O atom can reduce crystallite dimension in phase-change material, increase number of grain boundaries, thus increase crystalline resistance, improve crystallization temperature, finally improve the thermal stability of material.Material thermal stability (Xia etc., ChinesePhys.Lett.30,037401,2013) is improve, Sb after SnTe nitrating 2after Te nitrating, thermal stability improves greatly, and energy consumption is than Ge 2sb 2te 5low 10 times (Min Zhu etc., Journal of Alloys and Compounds, 509,10105 – 10109,2011).
Summary of the invention
The object of the invention is to overcome Sn 15sb 85the shortcoming that alloy thermal stability is not high, provides one can improve phase-change material stability, reduces the nitrating Sn of its operation power consumption simultaneously 15sb 85nano phase change thin-film material and preparation method thereof.
To achieve these goals, the present invention by the following technical solutions: a kind of nitrating nanometer thin-film material for quick high stability phase transition storage, its chemical general formula is Sn 15sb 85nx, is abbreviated as SnSbNx, and wherein x is nitrogen flow value, and its unit is sccm.
Described x is 1,2,3 or 4.
For a preparation method for the nitrating nanometer thin-film material of quick high stability phase transition storage, described nitrating Sn 15sb 85adopt the preparation of room temperature magnetically controlled sputter method, by radio frequency sputtering deposition Sn 15sb 85pass into argon gas and nitrogen in the process of film simultaneously, specifically comprise the following steps:
(1) SiO is cleaned 2/ Si (100) substrate;
(2) sputtering target material is installed; Setting sputtering power, setting sputtering Ar gas and N 2the gas flow of gas and sputtering pressure;
(3) room temperature magnetically controlled sputter method is adopted to prepare SnSbNx nano phase change thin-film material:
A) empty sample base is rotated to Sn 15sb 85target position, opens Sn 15sb 85radio-frequency power supply on target, opens target baffle plate build-up of luminance under build-up of luminance air pressure 0.25Pa;
B), after build-up of luminance, close target baffle plate, substrate to be sputtered is rotated to Sn 15sb 85target position, changes Ar gas and N 2the flow proportional of gas, slowly regulates sputtering pressure to be 4 × 10 -1pa, opens Sn 15sb 85target baffle plate on target position, according to the sputtering time 100s of setting, starts sputtering for Sn SbNx film; Described nitrating Sn is obtained after sputtering 15sb 85nano phase change thin-film material.
Described Ar gas and N 2the gas flow ratio of gas is: (26 ~ 29): (1 ~ 4).
Described Ar gas and N 2the purity of gas is greater than percent by volume 99.999%.
Described Sn 15sb 85the purity of target is at atomic percent more than 99.999%, and background vacuum is not more than 6 × 10 -4pa.
Described Sn 15sb 85target all adopts radio-frequency power supply, and sputtering power is 30W, and sputtering pressure is 4 × 10 - 1pa.
Pure Sn 15sb 85the crystallization temperature of alloy is about 150 DEG C, and crystalline active energy is 2.8696eV, and crystalline resistance is on the low side, and its thin-film material data keep the temperature of 10 years to only have 88 DEG C.With pure Sn 15sb 85alloy phase ratio, nitrating alloy of the present invention preferably resolves Sn 15sb 85the shortcoming and defect of material.By mixing nitrogen-atoms, make Sn 15sb 85crystallization temperature be significantly improved, data holding ability is strengthened, and thus improves its stability.Simultaneously by the raising of crystalline resistance, make its RESET lower power consumption.In a word, by nitrating, make Sn 15sb 85alloy becomes the phase-change material of a kind of high speed, high stability, low-power consumption, thus has good market application foreground.
Preparation method of the present invention is by control Ar and N 2gas flow and obtain the nitrating Sn with different N atom content 15sb 85nano phase change thin-film material, other conditions in preparation process are also very important, to the final nitrating Sn obtained 15sb 85the content size of the atom N in nano phase change thin-film material also plays certain influence.
Nitrating Sn of the present invention 15sb 85nano film material can be applied to phase transition storage, and tool has the following advantages compared with traditional phase change film material: first, and SnSbNx nano phase change thin-film material has crystallization rate faster, greatly can improve the storage speed of PCRAM; Secondly, SnSbNx nano phase change thin-film material has higher crystallization temperature and activation energy, thus can greatly improve the stability of PCRAM; Again, the Sn of non-nitrating is compared 15sb 85thin-film material, Sn 15sb 85nx nano phase change thin-film material has higher amorphous state and crystalline resistance, thus effectively can reduce PCRAM operation power consumption.
Accompanying drawing explanation
Fig. 1 is Sn of the present invention 15sb 85nx (x=1,2,3,4) nano phase change thin-film material and the Sn for contrasting 15sb 85the In-situ resistance of thin film phase change material and the relation curve of temperature.
Fig. 2 is Sn of the present invention 15sb 85nx (x=1,2,3,4) nano phase change thin-film material and the Sn for contrasting 15sb 85the corresponding relation curve of thin film phase change material out-of-service time and inverse temperature.
Embodiment
Below by way of specific instantiation, embodiments of the present invention are described, those skilled in the art the content disclosed by this specification can understand other advantages of the present invention and effect easily.The present invention can also be implemented or be applied by embodiments different in addition, and the every details in this specification also can based on different viewpoints and application, carries out various modification or change not deviating under spirit of the present invention.
Embodiment 1
The nitrating Sn prepared in the present embodiment 15sb 85nano phase change Thin Films is specially
Sn 15Sb 85N 1。
Preparation process is:
1. clean SiO 2/ Si (100) substrate, clean surface, the back side, remove dust granule, organic and inorganic impurity;
A) strong ultrasonic cleaning 10 minutes in ethanolic solution;
B) alcohol residue liquid is dried up with the warm shelves of hair-dryer, about 30 minutes.
2. adopt RF sputtering method to prepare Sn 15sb 85n 1prepare before film:
A) Sn is installed 15sb 85sputtering target material, the purity of target reaches 99.999% (atomic percent), and base vacuum is evacuated to 5 × 10 -4pa;
B) sputtering power 30W is set;
C) high-purity Ar and high-purity N is used 2as sputter gas (percent by volume all reaches 99.999%), setting Ar throughput is 29sccm, N 2flow is 1sccm, and by build-up of luminance air pressure adjustment to 0.25Pa.
3. adopt magnetically controlled sputter method to prepare Sn 15sb 85n 1nano phase change thin-film material:
A) empty sample carrier is rotated to Sn 15sb 85target position, opens Sn 15sb 85the radio-frequency power supply that target applies, opens target baffle plate and carries out build-up of luminance, and to Sn 15sb 85target sputters, clean Sn 15sb 85target material surface;
B) Sn 15sb 85after target material surface has cleaned, close target baffle plate, slowly sputtering pressure is adjusted to 4 × 10 - 1pa, rotates to Sn by substrate to be sputtered 15sb 85target position, opens target baffle plate, according to the sputtering time 100s of setting, starts to sputter nitrating Sn 15sb 85film.
Embodiment 2
Prepare the SnSbNx nano phase change thin-film material of the present embodiment, its concrete structure is respectively Sn 15sb 85n 2, Sn 15sb 85n 3and Sn 15sb 85n 4, preparation method is identical with example 1, and described in receive Sn 15sb 85n 2, Sn 15sb 85n 3and Sn 15sb 85n 4the sputtering time of nano phase change thin-film material is all 100s.Just prepare Sn 15sb 85n 2the Ar throughput of nano phase change thin-film material setting is 28sccm, N 2flow is 2sccm, and the method for manufacturing thin film of other structures by that analogy.
Comparative example Sn 15sb 85film
Individual layer Sn is prepared in this comparative example 15sb 85phase change film material, sputtering time is also 100s.
Preparation process is identical with example 1 with method, just prepares Sn 15sb 85the Ar throughput of nano phase change thin-film material setting is 30sccm, N 2for 0sccm.
By the Sn of above-described embodiment 1 and 2 15sb 85n 1, Sn 15sb 85n 2, Sn 15sb 85n 3and Sn 15sb 85n 4with the Sn in comparative example 15sb 85phase change film material is tested, and obtains the In-situ resistance of each phase change film material and relation curve Fig. 1 of temperature; By the Sn of above-described embodiment 1 and 2 15sb 85n 1, Sn 15sb 85n 2, Sn 15sb 85n 3and Sn 15sb 85n 4with the Sn in comparative example 15sb 85phase change film material is tested, and obtains the out-of-service time of each phase change film material and the corresponding relation curve chart 2 of inverse temperature.
The testing result of Fig. 1, Fig. 2 is as follows:
Fig. 1 is Sn of the present invention 15sb 85nx nano phase change thin-film material and the Sn for contrasting 15sb 85the In-situ resistance of thin-film material and the relation curve of temperature, the heating rate in test process is 10 DEG C/min.At low temperatures, all films are in high-resistance amorphous state.Along with the continuous rising of temperature, film resistor slowly reduces, and when reaching its phase transition temperature, film resistor reduces rapidly, and after arriving a certain resistance value, basic this value that keeps is constant, shows that film there occurs by the transformation of amorphous state to crystalline state.Test result shows, along with the increase of itrogen content of getter with nitrogen doped, crystallization temperature and the crystalline resistance of film all constantly increase thereupon, and the crystallization temperature of material increases Sn by 150 during non-nitrating DEG C 15sb 85n 4247 DEG C, show that the thermal stability of phase change film material is enhanced; The crystalline resistance of film increases Sn by 225 Ω during non-nitrating 15sb 85n 42.5 × 10 3Ω, expands 10 times, thus effectively reduces the power consumption of RESET process.
Fig. 2 is Sn of the present invention 15sb 85nx (x=1,2,3,4) nano phase change thin-film material and the Sn for contrasting 15sb 85the out-of-service time of thin-film material and the corresponding relation curve of inverse temperature.According to one of unified judgment criteria in the industry, temperature corresponding when utilizing phase-change material data to be kept 10 years is to pass judgment on the data holding ability of material.Can find out, the Sn of non-nitrating 15sb 85data keep the temperature of 10 years to only have 88 DEG C by phase change film material, and Sn of the present invention 15sb 85data keep the temperature of 10 years to be all improved by Nx (x=1,2,3,4) phase-change thin film, wherein Sn 15sb 85n 3data keep the temperature of 10 years to bring up to 173 DEG C by nano film material.Traditional Ge 2sb 2te 5the temperature that data keep 10 years by thin-film material is 85 DEG C.That is, Sn of the present invention 15sb 85n 1, Sn 15sb 85n 2, Sn 15sb 85n 3and Sn 15sb 85n 4have than traditional Ge 2sb 2te 5the data holding ability that thin-film material is more excellent.
Above-described embodiment is exemplary illustration principle of the present invention and effect thereof only, but not for limiting the present invention.Any person skilled in the art scholar all without prejudice under spirit of the present invention and category, can modify above-described embodiment or changes.Therefore, such as have in art usually know the knowledgeable do not depart from complete under disclosed spirit and technological thought all equivalence modify or change, must be contained by claim of the present invention.

Claims (7)

1. for a preparation method for the nitrating nanometer thin-film material of quick high stability phase transition storage, it is characterized in that: described nitrating Sn 15sb 85adopt the preparation of room temperature magnetically controlled sputter method, by radio frequency sputtering deposition Sn 15sb 85pass into argon gas and nitrogen in the process of film simultaneously, specifically comprise the following steps:
(1) SiO is cleaned 2/ Si (100) substrate;
(2) sputtering target material is installed; Setting sputtering power, setting sputtering Ar gas and N 2the gas flow of gas and sputtering pressure;
(3) room temperature magnetically controlled sputter method is adopted to prepare SnSbNx nano phase change thin-film material:
A) empty sample base is rotated to Sn 15sb 85target position, opens Sn 15sb 85radio-frequency power supply on target, opens target baffle plate build-up of luminance under build-up of luminance air pressure 0.25Pa;
B), after build-up of luminance, close target baffle plate, substrate to be sputtered is rotated to Sn 15sb 85target position, changes Ar gas and N 2the flow proportional of gas, slowly regulates sputtering pressure to be 4 × 10 -1pa, opens Sn 15sb 85target baffle plate on target position, according to the sputtering time 100s of setting, starts sputtering for Sn SbNx film; Described nitrating Sn is obtained after sputtering 15sb 85nano phase change thin-film material.
2. the preparation method of the nitrating nanometer thin-film material for quick high stability phase transition storage according to claim 1, is characterized in that: described Ar gas and N 2the gas flow ratio of gas is: (26 ~ 29): (1 ~ 4).
3. the preparation method of the nitrating nanometer thin-film material for quick high stability phase transition storage according to claim 2, is characterized in that: described Ar gas and N 2the purity of gas is greater than percent by volume 99.999%.
4. the preparation method of the nitrating nanometer thin-film material for quick high stability phase transition storage according to claim 1, is characterized in that: described Sn 15sb 85the purity of target is at atomic percent more than 99.999%, and background vacuum is not more than 6 × 10 -4pa.
5. the preparation method of the nitrating nanometer thin-film material for quick high stability phase transition storage according to claim 4, is characterized in that: described Sn 15sb 85target all adopts radio-frequency power supply, and sputtering power is 30W, and sputtering pressure is 4 × 10 -1pa.
6. the nitrating nanometer thin-film material that according to any one of claim 1 to 5 prepared by method, is characterized in that: its chemical general formula is Sn 15sb 85nx, wherein x is nitrogen flow value, and its unit is sccm.
7. nitrating nanometer thin-film material according to claim 6, is characterized in that: described x is 1,2,3 or 4.
CN201410655783.7A 2014-11-17 2014-11-17 Nitrogen-doped nano-film material applied to quick high-stability phase transition storage and preparation method Pending CN104393171A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
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CN105006519A (en) * 2015-07-14 2015-10-28 同济大学 High-speed low-power-consumption Sn18Sb82-SnSe2 nanometer composite multilayer film, preparation method and application thereof
CN105514271A (en) * 2015-12-31 2016-04-20 江苏理工学院 Erbium-doped Sn15Sb85-based phase change thin film material used for phase change memory and thin film preparation method
CN108365090A (en) * 2018-01-05 2018-08-03 江苏理工学院 A kind of SnSb nano phase change thin-film materials and preparation method thereof for mixing oxygen
CN109817807A (en) * 2018-12-26 2019-05-28 江苏理工学院 One type superlattices ZnSb/SiO2Nano phase change thin-film material and preparation method thereof
CN110010761A (en) * 2019-03-14 2019-07-12 江苏理工学院 A kind of Mg-Sn-Sb thin-film material and preparation method thereof for phase transition storage

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US20090251944A1 (en) * 2008-04-07 2009-10-08 Macronix International Co., Ltd. Memory cell having improved mechanical stability
CN102800807A (en) * 2012-08-23 2012-11-28 同济大学 Oxygen-doped nanometre thin-film material for low-power-consumption and high-reliability phase change memory as well as preparation and application of thin-film material
CN103887430A (en) * 2014-03-28 2014-06-25 江苏理工学院 Nitrating modified phase-change thin-film materials and preparing method thereof

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US7491573B1 (en) * 2008-03-13 2009-02-17 International Business Machines Corporation Phase change materials for applications that require fast switching and high endurance
US20090251944A1 (en) * 2008-04-07 2009-10-08 Macronix International Co., Ltd. Memory cell having improved mechanical stability
CN102800807A (en) * 2012-08-23 2012-11-28 同济大学 Oxygen-doped nanometre thin-film material for low-power-consumption and high-reliability phase change memory as well as preparation and application of thin-film material
CN103887430A (en) * 2014-03-28 2014-06-25 江苏理工学院 Nitrating modified phase-change thin-film materials and preparing method thereof

Cited By (8)

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Publication number Priority date Publication date Assignee Title
CN105006519A (en) * 2015-07-14 2015-10-28 同济大学 High-speed low-power-consumption Sn18Sb82-SnSe2 nanometer composite multilayer film, preparation method and application thereof
CN105006519B (en) * 2015-07-14 2018-05-08 同济大学 The tin antimony of high-speed low-power-consumption-tin selenium nano composite multiple layer film and preparation and application
CN105514271A (en) * 2015-12-31 2016-04-20 江苏理工学院 Erbium-doped Sn15Sb85-based phase change thin film material used for phase change memory and thin film preparation method
CN105514271B (en) * 2015-12-31 2018-06-08 江苏理工学院 For the Er ions Sn of phase transition storage15Sb85Base phase change film material and method for manufacturing thin film
CN108365090A (en) * 2018-01-05 2018-08-03 江苏理工学院 A kind of SnSb nano phase change thin-film materials and preparation method thereof for mixing oxygen
CN109817807A (en) * 2018-12-26 2019-05-28 江苏理工学院 One type superlattices ZnSb/SiO2Nano phase change thin-film material and preparation method thereof
CN110010761A (en) * 2019-03-14 2019-07-12 江苏理工学院 A kind of Mg-Sn-Sb thin-film material and preparation method thereof for phase transition storage
CN110010761B (en) * 2019-03-14 2023-04-18 江苏理工学院 Mg-Sn-Sb thin film material for phase change memory and preparation method thereof

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