CN108075039B - Nano composite ZnO-ZnSb phase change storage thin film material and preparation method thereof - Google Patents
Nano composite ZnO-ZnSb phase change storage thin film material and preparation method thereof Download PDFInfo
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- CN108075039B CN108075039B CN201711173404.0A CN201711173404A CN108075039B CN 108075039 B CN108075039 B CN 108075039B CN 201711173404 A CN201711173404 A CN 201711173404A CN 108075039 B CN108075039 B CN 108075039B
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Abstract
The invention discloses a nano composite ZnO-ZnSb phase change storage film material and a preparation method thereof, which are characterized in that the chemical structural formula of the material is (ZnSb)100‑x(ZnO)x，0<x<20, the preparation method comprises the following steps: the method comprises the steps of installing a ZnO ceramic target material on a magnetron direct current sputtering target, installing a ZnSb alloy target material on a magnetron radio frequency sputtering target, vacuumizing a sputtering chamber of a magnetron sputtering coating system, introducing high-purity argon until the air pressure in the sputtering chamber reaches 0.30Pa required by sputtering, fixing the sputtering power of the ZnSb radio frequency target to 35W, regulating the sputtering power of the ZnO direct current target to 3-21W, carrying out double-target co-sputtering coating at room temperature, and obtaining the phase change storage thin film material after the sputtering thickness reaches 180 nm.
Description
Technical Field
The invention relates to the technical field of phase change storage materials, in particular to a nano composite ZnO-ZnSb film material and a preparation method thereof.
Background
Chalcogenide thin film materials are widely used in electrical memories as well as optical data storage in DVDs. The chalcogenide thin film shows high infrared transmittance and high resistance in an amorphous state, similar to glass made of the chalcogenide thin film. However, under the action of the laser pulse or the electric pulse, the chalcogenide film after crystallization is caused to exhibit considerable light reflectance and conductivity. Chalcogenide thin films are most expected to be applied to next-generation nonvolatile memories (PCMs) as storage media because of their excellent properties of high speed, high density, low power consumption, long life span, and good scalability.
Located in GeTe-Sb2Te3Ge in ternary Structure2Sb2Te5(GST) is one of the most popular chalcogenide thin film materials in PCM as a storage medium, with excellent electrical and optical properties combined with good thermal stability of GeTe and Sb2Te3Fast speed of materialFast phase change capability. However, there are still a number of disadvantages, such as: the high melting point and the low crystallization resistance result in relatively high power consumption, and the problem of insufficient data retention capability in the aspect of automobile electronics also exists. To solve these problems, elements such as Al, Ag, Sn, Zn, In, W, O, and N are introduced into GST one after another In an attempt to improve the performance of the chalcogenide GST thin film. However, its crystallization mechanism based on nucleation results in a slow crystallization rate.
Recently, researchers have conducted crystallization studies on binary compounds containing little tellurium, such as GaSb, InSb, SiSb, and ZnSb, and found that the growth-mode-dominant crystallization mechanism exhibits a faster phase change rate. Especially ZnSb films, possess faster crystallization speed, higher crystallization resistance, higher crystallization temperature (above 250 ℃), higher data stability (ten years at above 200 ℃) and lower melting temperature (about 500 ℃) than other materials. However, the two-step crystallization behavior of the transition to the metastable ZnSb phase around about 250 ℃ and the stable ZnSb phase around about 350 ℃ will decrease the interface reliability between the PCM phase change layer and the electrode.
Disclosure of Invention
The invention aims to solve the technical problem of providing a nano composite ZnO-ZnSb phase change storage film material which has high crystallization temperature, high crystallization speed and high amorphous/crystalline resistance ratio and can realize the direct conversion from the amorphous state to the stable crystalline phase and a preparation method thereof.
The technical scheme adopted by the invention for solving the technical problems is as follows: a nano composite ZnO-ZnSb phase change storage film material is a composite of a dielectric material ZnO and a phase change material ZnSb, and has a chemical structural formula of (ZnSb)100-x(ZnO)xWherein 0 is<x<20。
The chemical structural formula of the phase change storage film material is (ZnSb)81.8(ZnO)18.2。
The phase change storage thin film material is obtained by co-sputtering ZnO ceramic target and ZnSb alloy target in a magnetron sputtering coating system through double targets.
The phase change material ZnSb in the phase change storage film material is uniformly dispersed in the dielectric material ZnO in the form of nano-scale particles.
A preparation method of a nano composite ZnO-ZnSb phase change storage film material is obtained by adopting a double-target co-sputtering method, and comprises the following specific steps: in a magnetron sputtering coating system, a quartz plate or a silicon oxide wafer is used as a substrate, a ZnO ceramic target material is arranged on a magnetron direct current sputtering target, a ZnSb alloy target material is arranged on a magnetron radio frequency sputtering target, and a sputtering chamber of the magnetron sputtering coating system is vacuumized until the indoor vacuum degree reaches 5.6 multiplied by 10-4Pa, introducing high-purity argon with the volume flow of 50.0ml/min into the sputtering chamber until the air pressure in the sputtering chamber reaches the glow starting air pressure of 0.30Pa required by sputtering, fixing the sputtering power of a ZnSb radio-frequency target to 35W, regulating the sputtering power of a ZnO direct-current target to 3-21W, carrying out double-target co-sputtering coating at room temperature until the sputtering thickness reaches 180nm to obtain the deposited nano composite ZnO-ZnSb phase change storage film material with the chemical structural formula of (ZnSb)100-x(ZnO)xWherein 0 is<x<20。
The chemical structural formula of the phase change storage film material is (ZnSb)81.8(ZnO)18.2。
Compared with the prior art, the invention has the advantages that: the invention relates to a preparation method of a nano composite ZnO-ZnSb phase change storage film material, which is characterized in that a dielectric material ZnO and a phase change material ZnSb are compounded under the nanoscale to form a uniformly distributed nano composite phase change storage material, and a nano composite structure is constructed by introducing the dielectric material to inhibit the performance of a metastable phase improved material. The chemical structural formula is (ZnSb)100-x(ZnO)xWherein 0 is<x<20. The film material has higher crystallization temperature, larger amorphous state/crystalline state resistance ratio and higher crystallization speed; along with the increase of the doping concentration of ZnO oxide, the amorphous resistance, the amorphous/crystalline resistance ratio, the crystallization temperature and the thermal stability are gradually increased, and the transformation process from the amorphous state to the metastable phase is gradually inhibited, so that the amorphous/crystalline resistance ratio is directly transformed into the stable phase, the one-step crystallization behavior is realized, and the reliability of the interface between the PCM phase change layer and the electrode is improved; the crystallization temperature of the nano composite ZnO-ZnSb film material (c)T c) Is composed of274-305 ℃ and the amorphous/crystalline resistance ratio is 1.21 multiplied by 105~9.18×105(ii) a Preferably, component (ZnSb)81.8(ZnO)18.2Crystallization temperature of (C: (C))T c) 305 ℃ and an amorphous/crystalline resistance ratio of 9.18X 105The ten year data held a maximum temperature of 229.2 ℃.
Drawings
FIG. 1 shows the different components (ZnSb)100-x(ZnO)xThe square resistance of the film changes with the temperature;
FIG. 2 shows the different components (ZnSb)100-x(ZnO)xThe storage time of the amorphous film at different temperatures and a maximum temperature graph of ten-year data retention capacity fitted by the storage time;
FIG. 3 is (ZnSb)100-x(ZnO)xX-ray diffraction pattern of a thin film sample at an annealing temperature of 250 ℃;
FIG. 4 shows (ZnSb)100-x(ZnO)xX-ray diffraction patterns of thin film samples at 300 ℃ annealing temperature;
FIG. 5 shows (ZnSb)100-x(ZnO)xX-ray diffraction pattern of a thin film sample at an annealing temperature of 350 ℃;
FIG. 6 shows (ZnSb)100-x(ZnO)xX-ray diffraction pattern of thin film samples at 430 ℃ annealing temperature.
Detailed Description
The invention is described in further detail below with reference to the accompanying examples.
A nanometer composite ZnO-ZnSb phase change storage film material is a ZnO oxide and ZnSb alloy composite with a chemical structural formula of (ZnSb)100-x(ZnO)xWherein 0 is<x<20, the specific preparation process comprises the following steps: in a magnetron sputtering coating system, a quartz plate or a silicon oxide wafer is used as a substrate, a ZnO ceramic target material is arranged on a magnetron direct current sputtering target, a ZnSb alloy target material is arranged on a magnetron radio frequency sputtering target, and a sputtering chamber of the magnetron sputtering coating system is vacuumized until the indoor vacuum degree reaches 5.6 multiplied by 10-4Pa, then introducing high-purity argon with the volume flow of 50.0ml/min into the sputtering chamberAnd (3) until the air pressure in the sputtering chamber reaches the starting air pressure of 0.30Pa required by sputtering, fixing the sputtering power of the ZnSb radio frequency target to 35W, regulating the sputtering power of the ZnO direct current target to 3-21W, carrying out double-target co-sputtering coating at room temperature, and obtaining the deposited nano composite ZnO-ZnSb phase change storage film material after the sputtering thickness reaches 180 nm.
Example one
In a magnetron sputtering coating system, a quartz plate or a silicon oxide wafer is used as a substrate, a ZnO ceramic target material is arranged on a magnetron direct current sputtering target, a ZnSb alloy target material is arranged on a magnetron radio frequency sputtering target, and a sputtering chamber of the magnetron sputtering coating system is vacuumized until the indoor vacuum degree reaches 5.6 multiplied by 10-4Pa, then introducing high-purity argon with the volume flow of 50.0ml/min into the sputtering chamber until the air pressure in the sputtering chamber reaches the glow starting air pressure of 0.30Pa required by sputtering, then controlling the sputtering power of the ZnO ceramic target to be 3W and the sputtering power of the ZnSb alloy target to be 35W, carrying out double-target co-sputtering coating at room temperature, and obtaining the nano composite (ZnSb) in a deposition state after the sputtering thickness is 180nm100-x(ZnO)xAnd (3) phase change storage thin film material. Wherein x =5.3, i.e. chemical structural formula is (ZnSb)94.7(ZnO)5.3。
The in-situ resistance test of the prepared film material is performed, the test result is shown in fig. 1 and fig. 2, and it can be seen from fig. 1 and fig. 2 that the performance indexes of the film prepared in this example are as follows: crystallization temperatureT c283 ℃, ten-year holding capacity maximum temperature of 213.4 ℃, and amorphous/crystalline resistance ratio of 1.21 x 105。
Example two
The difference from the first embodiment is that: in the sputtering process, the sputtering power of the ZnO ceramic target is controlled to be 8W, the sputtering power of the ZnSb alloy target is controlled to be 35W, double-target co-sputtering coating is carried out at room temperature, and after the sputtering thickness is 180nm, the nano composite (ZnSb) in a deposition state is obtained100-x(ZnO)xAnd (3) phase change storage thin film material. Wherein x =9.5, namely the chemical structural formula is (ZnSb)90.5(ZnO)9.5。
The prepared film material is subjected to in-situ resistance test, and the test results are shown in figure 1 and figure2, it can be seen from fig. 1 and 2 that the performance indexes of the film prepared in this example are as follows: crystallization temperatureT c287 ℃ and a ten-year retention maximum temperature of 216.7 ℃, and the amorphous/crystalline resistance ratio is 2.20X 105。
EXAMPLE III
The difference from the first embodiment is that: in the sputtering process, the sputtering power of the ZnO ceramic target is controlled to be 12W, the sputtering power of the ZnSb alloy target is controlled to be 35W, double-target co-sputtering coating is carried out at room temperature, and after the sputtering thickness is 180nm, the nano composite (ZnSb) in a deposition state is obtained100-x(ZnO)xAnd (3) phase change storage thin film material. Wherein x =12.3, i.e. chemical structural formula is (ZnSb)87.7(ZnO)12.3。
The in-situ resistance test of the prepared film material is performed, the test result is shown in fig. 1 and fig. 2, and it can be seen from fig. 1 and fig. 2 that the performance indexes of the film prepared in this example are as follows: crystallization temperatureT c294 deg.C, ten-year holding power maximum temperature of 220.5 deg.C, and amorphous/crystalline resistance ratio of 7.29 × 105。
Example four
The difference from the first embodiment is that: in the sputtering process, the sputtering power of the ZnO ceramic target is controlled to be 16W, the sputtering power of the ZnSb alloy target is controlled to be 35W, double-target co-sputtering coating is carried out at room temperature, and after the sputtering thickness is 180nm, the nano composite (ZnSb) in a deposition state is obtained100-x(ZnO)xAnd (3) phase change storage thin film material. Wherein x =15.1, namely the chemical structural formula is (ZnSb)84.9(ZnO)15.1。
The in-situ resistance test of the prepared film material is performed, the test result is shown in fig. 1 and fig. 2, and it can be seen from fig. 1 and fig. 2 that the performance indexes of the film prepared in this example are as follows: crystallization temperatureT c299 deg.C, ten-year holding capacity maximum temperature of 224.5 deg.C, and amorphous/crystalline resistance ratio of 8.55 × 105。
EXAMPLE five
The difference from the first embodiment is that: in the sputtering process, the sputtering power of the ZnO ceramic target is controlled to be 21W, and the sputtering power of the ZnSb alloy targetThe rate is 35W, the film is co-sputtered by double targets at room temperature, and the sputtering thickness is 180nm, so as to obtain the nano composite (ZnSb) in a deposition state100-x(ZnO)xAnd (3) phase change storage thin film material. Wherein x =18.2, i.e. chemical formula (ZnSb)81.8(ZnO)18.2。
The in-situ resistance test of the prepared film material is performed, the test result is shown in fig. 1 and fig. 2, and it can be seen from fig. 1 and fig. 2 that the performance indexes of the film prepared in this example are as follows: crystallization temperatureT c305 ℃ and a ten-year retention capacity maximum temperature of 229.2 ℃, and the amorphous/crystalline resistance ratio of 9.18 multiplied by 105。
Comparative test
The difference from the first embodiment is that: and in the sputtering process, controlling the sputtering power of the ZnO ceramic target to be 0W and the sputtering power of the ZnSb alloy target to be 35W, carrying out double-target co-sputtering coating at room temperature, and obtaining the deposited ZnSb phase change storage film after the sputtering thickness is 180 nm.
The in-situ resistance test of the prepared film material is performed, the test results are shown in fig. 1 and fig. 2, and the performance indexes of the ZnSb film prepared in this example can be obtained from fig. 1 and fig. 2 as follows: crystallization temperatureT cAt 274 deg.C, a ten-year holding capacity maximum temperature of 201.7 deg.C, and an amorphous/crystalline resistance ratio of 5.74X 104。
The different examples described above were compared and the results analyzed as follows:
the sputtering power, the ZnO and ZnSb contents and the related parameters of the targets of the different embodiments are shown in Table 1.
TABLE 1 nanocomposite ZnO-ZnSb phase change film Material compositions prepared under different conditions
FIG. 1 shows the resistance of ZnSb film and ZnO-ZnSb composite film as a function of temperature measured at a temperature rise rate of 10K/min. The graph shows that the trend of the decrease of the sheet resistance with the increase of the temperature after the introduction of ZnO is shifted to a high temperature section, indicating that the crystallization temperature of the film is increased.The crystallization temperatures of samples 1, 2, 3, 4, and 5 were 283, 287, 294, 299, and 305 ℃, respectively, which were all higher than the crystallization temperature of ZnSb (-274 ℃). In addition, samples 1 and 2 had slight secondary phase transition with respect to ZnSb, and this phenomenon was completely disappeared in samples 3, 4 and 5, indicating that the secondary phase transition phenomenon of ZnSb occurring at about 350 ℃ was gradually suppressed with the increase of ZnO concentration, resulting in the improvement of the reliability of the interface between the PCM phase change layer and the electrode. In addition, the amorphous resistance of the ZnO-ZnSb composite film is obviously improved, so that the ratio of the amorphous state to the crystalline state is kept at 105Above, 10 higher than ZnSb4The film has a higher on/off ratio.
FIG. 2 is a graph of amorphous state thermal stability relationship between a ZnSb film and a ZnO-ZnSb composite film obtained by an in-situ resistance measurement method, and ten-year data storage maximum temperatures of the ZnO-ZnSb composite film are calculated by fitting and are 213.4, 216.7, 220.5, 224.5 and 229.2 ℃, which are all higher than 201.7 ℃ of ZnSb. It can be seen that the amorphous thermal stability of the ZnSb film after ZnO recombination is further improved.
FIG. 3, FIG. 4, FIG. 5 and FIG. 6 are XRD diffraction patterns of different film components after annealing at 250 deg.C, 300 deg.C, 350 deg.C and 430 deg.C for 10min, respectively. It can be seen that the thin film is in an amorphous state even when annealed at a high temperature of 250 c for ten minutes, which sufficiently demonstrates the high thermal stability of the thin film. The metastable phase diffraction peak corresponding to ZnSb did not appear for the control, samples 1 and 2 until the annealing temperature increased to 300 deg.C, but the diffraction peak for sample 2 was very weak. Whereas samples 3, 4 and 5 did not show metastable devitrification peaks. With further increases in the annealing temperature to 350 and 430 degrees, all films exhibited devitrification peaks corresponding to stabilized ZnSb. The XRD diffraction spectrum proves that the result obtained by in-situ resistance test analysis shows that the film compounded with ZnO oxide in ZnSb not only improves the thermal stability of the amorphous film, but also inhibits the secondary phase change phenomenon of ZnSb at 350 ℃.
In conclusion, the nano-composite ZnO-ZnSb phase change storage film material prepared by the invention inhibits the secondary phase change of ZnSb, has high stability and high crystallization speed, also has higher amorphous/crystalline resistance and improves the comprehensive performance of the phase change material.
The above description is not intended to limit the present invention, and the present invention is not limited to the above examples. Those skilled in the art will appreciate that various modifications, additions and substitutions are possible, without departing from the scope and spirit of the invention as disclosed in the accompanying claims.
Claims (4)
1. A nanometer composite ZnO-ZnSb phase change storage film material is characterized in that: the chemical structural formula of the phase change storage film material is (ZnSb)100-x(ZnO)xWherein, the atomic percentage of ZnO is between 5.3 and X and 18.2 percent, and the atomic percentage of the whole ZnSb is between 81.8 and 100-X and 94.7 percent.
2. The nano-composite ZnO-ZnSb phase-change storage thin film material according to claim 1, wherein: the phase change storage thin film material is obtained by co-sputtering ZnO ceramic target and ZnSb alloy target in a magnetron sputtering coating system through double targets.
3. The nano-composite ZnO-ZnSb phase-change storage thin film material according to claim 1, wherein: the phase change material ZnSb in the phase change storage film material is uniformly dispersed in the dielectric material ZnO in the form of nano-scale particles.
4. The preparation method of the nano-composite ZnO-ZnSb phase change storage thin film material according to claim 1, which is characterized by comprising the following steps: in a magnetron sputtering coating system, a quartz plate or a silicon oxide wafer is used as a substrate, a ZnO ceramic target material is arranged on a magnetron direct current sputtering target, a ZnSb alloy target material is arranged on a magnetron radio frequency sputtering target, and a sputtering chamber of the magnetron sputtering coating system is vacuumized until the indoor vacuum degree reaches 5.6 multiplied by 10-4Pa, introducing high-purity argon with the volume flow of 50.0ml/min into the sputtering chamber until the air pressure in the sputtering chamber reaches the glow starting air pressure of 0.30Pa required by sputtering, fixing the sputtering power of the ZnSb alloy target to 35W, regulating the sputtering power of the ZnO ceramic target to 3-21W,co-sputtering the film with two targets at room temperature to obtain the deposited nano composite ZnO-ZnSb phase change storage film material with the chemical structural formula of (ZnSb) and the sputtering thickness of 180nm100-x(ZnO)xWherein, the atomic percentage of ZnO is between 5.3 and X and 18.2 percent, and the atomic percentage of the whole ZnSb is between 81.8 and 100-X and 94.7 percent.
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| CN109285944B (en) * | 2018-08-09 | 2022-08-19 | 江苏理工学院 | Superlattice-like phase-change thin film material with rapid transformation performance |
| CN109273596B (en) * | 2018-08-09 | 2022-08-19 | 江苏理工学院 | Multilayer phase change film material with high thermal stability and low power consumption performance |
| CN109860388B (en) * | 2019-01-09 | 2022-12-23 | 江苏理工学院 | Multilayer phase change film, preparation method and application |
| CN110983270B (en) * | 2019-12-03 | 2021-12-03 | 天津大学 | Oxide-metal composite nano glass material |
| CN112786782B (en) * | 2021-01-11 | 2022-09-20 | 宁波大学 | Sb-Si for phase change memory 3 N 4 Thin film material and preparation method thereof |
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