CN108321294B - Thin film resistive random access memory with adjustable memory mechanism and preparation method thereof - Google Patents
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- H10N70/24—Multistable switching devices, e.g. memristors based on migration or redistribution of ionic species, e.g. anions, vacancies
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- H10N70/011—Manufacture or treatment of multistable switching devices
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- H10N70/8833—Binary metal oxides, e.g. TaOx
Abstract
The invention discloses a thin film resistive random access memory with an adjustable memory mechanism and a preparation method thereof. The preparation method takes high-purity metal copper as an evaporation source, realizes the preparation of the oxide film resistive random access memory through spontaneous oxidation in the evaporation process, and has simple and easy preparation process and excellent device performance.
Description
Technical Field
The invention belongs to the technical field of preparation of thin film resistive random access memories, and particularly relates to a thin film resistive random access memory with an adjustable storage mechanism and a preparation method thereof.
Background
Resistive Random Access Memory (RRAM) stores information by using the change of resistance of a semiconductor material in a high-low resistance state under the action of an external electric field. The resistive random access memory generally adopts a metal-semiconductor material-metal (MIM) capacitive structure, and has a good application prospect in the research field of next-generation nonvolatile memories due to simple structure, low power consumption, low manufacturing cost and high response speed. Currently, research has shown that a large number of semiconductor materials, such as binary transition metal oxides (ZrO)2，Adv.Mater.2010,22,411；TiO2，Nat Nanotechnol.2010,5,148；CuxO, appl. Phys. Lett.2015,107,113504, etc.), ion-conducting chalcogenides (Ag)2S，J.Mater.Chem.C 2013,1,3282；Cu2S，Appl.Phys.Lett.2007,91,073511；Cu2- xSe, appl.Phys.Lett.2013,103,193501, etc.), perovskite type composite oxides (SrZrO)3，IEEE Electron Device Lett.2008,29,1108；Sr2TiO4，Adv.mater.2010,22,411, etc.), organic semiconductor materials (Cu: TCNQ, appl.phys.lett.2003,83,1252, etc.), can be applied to the field of resistive random access memories, wherein copper oxide thin films have been widely studied since they are well compatible with standard copper interconnection processes in the existing microelectronic processes.
In order to obtain stable storage properties, a process for preparing a copper oxide thin film is very important. At present, researchers commonly employ CuxO ceramic target material, and Cu is realized on the substrate by a method of pulsed-State Electronics (2012, 73,11) or radio frequency magnetron sputtering (Appl. Phys. Lett.2009,95,012110)xDeposition of O film to avoid CuxThe decomposition of O is carried out under oxygen atmosphere during the deposition process; thin film deposition can also be achieved by liquid phase reactions using a sol-gel process (appl. phys. a 2011,104,1069). Because the ceramic target material is complicated in preparation process and has risks of easy cracking and the like, researchers have tried to perform Cu film oxidation to obtain CuxAnd (4) preparing an O film. The study of Hangzhou propylene, institute of microelectronics, China academy of sciences, adopted electroplating of a Cu film of 120nm, and then oxidizing the Cu film for 10-30 minutes in a reactive ion etching system under an oxygen atmosphere to partially convert the Cu film into a copper oxide film (appl. Phys. A2011,102,1015); professor Tseng radio frequency magnetron sputtering high-purity Cu target material, depositing a 300nm copper film, and then annealing in 400 ℃ oxygen atmosphere to form CuxO films (j.appl.phys.2010,108, 114110). In the oxidation process, the content of oxygen, the oxidation time and the like are important for influencing the components and the performance of the product film.
Since the copper oxide has a small standard free energy of formation (CuO of-66.91 kJ. mol. at 1000K)-1，Cu2O is-95.77 kJ. mol-1) Since spontaneous oxidation of Cu is unavoidable at higher temperatures, thermal evaporation of a high purity Cu source, spontaneous oxidation of Cu at lower vacuum chamber pressures and slower evaporation rates, promises to achieve Cu on substratesxAnd (4) depositing an O film.
Disclosure of Invention
On the basis of the prior art, the invention aims to construct a simple film resistive random access memory with an adjustable storage mechanism, which has important significance in the field of resistive random access memory development, and solves the technical problems that the composition of a film is adjusted through deposition conditions, and the storage mechanism of the memory is adjusted through the thickness of the film.
The invention solves the technical problem and adopts the following technical scheme:
the invention firstly discloses a thin film resistive random access memory with an adjustable memory mechanism, which is characterized in that: the method comprises the steps of taking a silicon-based substrate with an insulating layer covered on the upper surface as a base, and dispersing KCu on the insulating layer7S4A quasi-one-dimensional nanostructure; in the KCu7S4One end of the quasi-one-dimensional nanostructure is deposited with a first metal film electrode and the KCu7S4Forming ohmic contact by the quasi-one-dimensional nano structure; in the KCu7S4The other end of the quasi-one-dimensional nano structure is deposited with a copper oxide film; depositing a second metal film electrode in the same area above the copper oxide film;
the copper oxide film is evaporated by thermal evaporation with Cu particles with purity not lower than 99.99% as copper source, and the pressure in vacuum chamber is controlled to be 9 × 10 during evaporation-3～1×10-2Pa, evaporation rate of
So that the Cu is spontaneously oxidized in the evaporation process, thereby obtaining an oxide film of Cu-CuxAn O film;
the KCu7S4Quasi-one-dimensional nanostructure, the CuxThe O film and the second metal film electrode form a film resistive random access memory, and the following steps: when the Cu isxKCu when the thickness of the O film is 15-25nm7S4As the active metal electrode, CuxO to Cu+The device has the bipolar resistance change storage characteristic of a conductive wire mechanism; when the Cu isxWhen the thickness of the O film is 30-100nm, the thicker oxide layer is not easy to be subjected to soft breakdown, the trapping effect of the oxide layer plays a main role, and the device has the resistance change storage characteristic of an interface capture mechanism.
Further, the second metal thin film electrode is an Au electrode or a Pt electrode; the thickness of the second metal film electrode is 30-100 nm.
Further, the insulating layer is SiO2Insulating layer, insulating tape, Si3N4Insulating layer, HfO2Insulating layer or Al2O3An insulating layer having a resistivity of not less than 1 × 103Omega-cm, thickness of 100-500 nm.
Further, the KCu7S4The axial length of the quasi-one-dimensional nano structure is not less than 10 mu m, and the radial length is 100-1000 nm.
Further, the first metal thin film electrode is an Au electrode, a Ti/Au composite electrode, a Cr/Au composite electrode, a Ni/Au composite electrode or a Pt electrode; the thickness of the Au electrode and the Pt electrode is 30-100 nm; the Ti/Au composite electrode, the Cr/Au composite electrode and the Ni/Au composite electrode are respectively formed by depositing Au with the thickness of 30-100nm on Ti, Cr and Ni with the thickness of 3-10 nm.
Further, the minimum distance between the first metal thin-film electrode and the second metal thin-film electrode is 5-10 μm.
The invention also discloses a preparation method of the thin film resistive random access memory, which comprises the following steps:
(1) adopting a silicon wafer with an insulating layer covered on the upper surface as a substrate, and adding KCu7S4A quasi-one-dimensional nanostructure dispersed on the insulating layer;
(2) by one-time UV exposure lithography and thin film deposition technique in KCu7S4Depositing a first metal film electrode at one end of the quasi-one-dimensional nanostructure;
(3) by means of secondary ultraviolet exposure lithography and electron beam heating evaporation, Cu particles with purity not lower than 99.99% are used as copper source for evaporation, and the air pressure of the vacuum chamber is controlled to be 9 x 10 during evaporation-3～1×10-2Pa, evaporation rate of
So that Cu is spontaneously oxidized during evaporation and thus is in KCu7S4Another of the quasi-one-dimensional nanostructuresDepositing an oxide film of copper on the end;
(4) and depositing a second metal film electrode above the copper oxide film by using a film deposition technology, thereby completing the preparation of the film resistive random access memory.
Further, the deposition mode of the first metal film electrode in the step (2) is electron beam evaporation, and the air pressure of the vacuum chamber during evaporation is not higher than 6 x 10-3Pa, evaporation rate of
The deposition mode of the second metal film electrode in the step (4) is electron beam evaporation, and the air pressure of a vacuum chamber is not higher than 6 multiplied by 10 during evaporation-3Pa, evaporation rate of
Compared with the prior art, the invention has the beneficial effects that:
1. the invention adopts electron beam heating evaporation high-purity Cu source, realizes the preparation of the oxide film memory by spontaneous oxidation in the evaporation process, and has simpler raw materials and preparation process and good controllability compared with the method of evaporating and sputtering ceramic target materials or oxidizing metal films in oxygen atmosphere.
2. The invention constructs the nanometer film resistive random access memory based on the quasi-one-dimensional nanometer structure, and provides a new idea for constructing the nanometer scale memory.
3. According to the invention, the regulation and control of different storage mechanisms of the resistive random access memory are realized through thickness regulation, and the method has a certain guiding significance in the aspects of researches such as the improvement of the performance and the stability of the oxide thin film memory.
4. The bipolar resistive random access memory prepared by the invention has the starting voltage of 0.58V, the erasing voltage of-0.21V and the switching ratio of more than 102Cu-based structures with better performance than similar structuresxO thin film resistive random access memory such as: kwon et al Ag/CuO/TiN structure constructed by RF magnetron sputtering method with the starting voltage of 0.96V, the erasing voltage of-1.5V and the on-off ratio of 102(j.mater.chem.c 2015,3, 9540); and S.Y.Wang, etcConstructed Ti/CuxThe O/Pt structure has the starting voltage of 0.8V, the erasing voltage of-0.5V and the on-off ratio of 102(J.appl.Phys.2010,108, 114110). The resistive random access memory is simple in preparation method and lower in power consumption.
Drawings
Fig. 1 is a schematic device structure diagram of a thin film resistive random access memory with an adjustable memory mechanism, wherein: 1 is a silicon-based substrate, 2 is an insulating layer, and 3 is KCu7S4The quasi-one-dimensional nanostructure is characterized in that 4 is a first metal film electrode, 5 is a copper oxide film, and 6 is a second metal film electrode.
FIG. 2 is an enlarged schematic view of a memory cell interface.
FIG. 3 is an XRD pattern of a copper oxide thin film in example 1 of the present invention.
FIG. 4 is an XPS spectrum of a copper oxide thin film in example 1 of the present invention, wherein a is an XPS spectrum of Cu2p and b is Cu2p3/2And (5) performing peak separation fitting on the map.
FIG. 5 shows the pressure of the vacuum chamber being 2X 10-3Pa, deposition rate of
XRD pattern of product film obtained by electron beam evaporation of high purity Cu source.
Fig. 6 is a typical current-voltage characteristic curve of the resistive random access memory prepared in embodiment 1 of the present invention before activation.
Fig. 7 is an activation process of the resistive random access memory prepared in embodiment 1 of the present invention.
Fig. 8 is a typical current-voltage characteristic curve of the resistive random access memory prepared in example 1 of the present invention after activation.
Fig. 9 shows the repeatability of the bipolar memory device after the resistive random access memory prepared in embodiment 1 of the present invention is activated.
Fig. 10 is a graph showing the high and low resistance retention times read at 0.25V for the bipolar memory device prepared in example 1 of the present invention.
Fig. 11 is a typical current-voltage characteristic curve of the resistive random access memory prepared in embodiment 2 of the present invention before activation.
Fig. 12 is an activation process of the resistive random access memory prepared in embodiment 2 of the present invention.
Fig. 13 is a typical current-voltage characteristic curve of a device prepared in example 3 of the present invention.
Detailed Description
The following embodiments of the present invention will be described in detail with reference to the accompanying drawings, which are provided for implementing the technical solution of the present invention, and provide detailed embodiments and specific procedures, but the scope of the present invention is not limited to the following embodiments.
Example 1
Referring to fig. 1, the thin film resistive random access memory of the present invention uses a silicon-based substrate 1 as a base, and 300nm silicon dioxide is grown at all positions of the upper surface of the silicon-based substrate 1 by thermal oxidation to form an insulating layer 2; KCu is dispersed on the upper surface of the insulating layer 27S4A quasi-one-dimensional nanostructure 3; in KCu7S4One end of the quasi-one-dimensional nano structure 3 is deposited with a first metal film electrode 4 and KCu7S4The quasi-one-dimensional nano structure 3 forms ohmic contact; in KCu7S4The other end of the quasi-one-dimensional nano structure 3 is deposited with a copper oxide film 5 and a second metal film electrode 6.
Specifically, the method comprises the following steps: KCu used in this example7S4KCu synthesized by quasi-one-dimensional nano structure through solution method7S4A nanowire; the first metal thin film and the second metal thin film electrodes are Au electrodes having a thickness of 50nm, and the copper oxide thin film has a thickness of 16 nm.
Specifically, KCu7S4The preparation method of the quasi-one-dimensional nano structure comprises the following steps:
3.88g NaOH and 5.11g KOH were added to 30mL deionized water, dissolved by magnetic stirring and allowed to cool to room temperature, then 0.51g CuCl was added2·2H2O, 300. mu.L of ethylenediamine, 2.88g of Na2S·9H2O and 3mL of hydrazine hydrate, fully stirring, putting the mixture into a constant-temperature drying box at 80 ℃ for reacting for 50 minutes, taking out a flocculent product at the upper layer, centrifugally cleaning the flocculent product until the pH value of the supernatant reaches neutral, and then cleaning the flocculent product for 2 to 3 times by using alcohol to obtain a product KCu7S4Quasi-one-dimensional nano-junctionAnd (5) forming. Then the mixture is placed in a constant-temperature drying oven at 60 ℃ to be dried for 4 hours, and the obtained powder is ready for use.
Specifically, the preparation method of the copper oxide film is as follows:
using electron beam evaporation coating equipment, taking Cu particles with the purity of 99.99 percent as a Cu source, and controlling the air pressure of a vacuum cavity to be 9.8 multiplied by 10-3Pa, and controlling the deposition rate to
The thickness of the deposited film was monitored in real time using a film thickness meter, and the thickness of the deposited film was controlled to 16 nm.
The XRD pattern of the copper oxide film obtained in this example is shown in FIG. 3, from which it can be seen that the copper oxide film is mainly composed of monoclinic CuO (JCPDS card No. 48-1548) and cubic Cu2O (JCPDS card No. 77-0199).
An XPS spectrum of the copper oxide film obtained in this example is shown in FIG. 4. As can be seen from FIG. 4a, the XPS spectrum of Cu2p has two significant satellite peaks, indicating that the product film has significant oxidation, and the peak fitting results of FIG. 4b confirm that Cu2p3/2The peak can be divided into two peaks, the peak values are 932.2eV and 933.8eV respectively, and the oxide film is mainly composed of Cu2O and CuO.
FIG. 5 shows a vacuum chamber with a pressure of 2X 10-3Pa, deposition rate of
The XRD pattern of the product film obtained by electron beam evaporation shows that the main component of the product is cubic crystal simple substance Cu (JCPDS card No. 04-0836), and the regulation and control of the components of the product film can be realized by regulating the deposition condition.
A typical current-voltage characteristic curve of the thin film resistive random access memory obtained in this example before activation is shown in fig. 6. When the current limiting value is 100 muA and the voltage scanning mode is-1V → 0V → 1V, a significant electric hysteresis phenomenon occurs in the forward scanning voltage range of the device, the device reaches a low-resistance state at 0.65V and recovers to a high-resistance state at 0.4V, and the electric hysteresis phenomenon is formed by capturing electrons during forward scanning of the oxide layer and releasing the electrons when the voltage is reduced.
The activation process of the thin film resistive random access memory obtained in this embodiment is as shown in fig. 7, the current limiting value is set to be 1000 μ a, and the voltage scanning mode is-1V → 0V → -1V, and it can be seen from the figure that the electrical hysteresis phenomenon of the device is significantly changed, and the hysteresis curve in the forward voltage region is converted into the bipolar hysteresis curve.
A typical current-voltage characteristic curve of the thin film resistive random access memory obtained in this embodiment after activation is shown in fig. 8. When the current limiting value is 100 muA, the voltage scanning mode is-1V → 0V → 1V → 0V → -1V, the device has remarkable bipolar resistance switching characteristics, the turn-on voltage is 0.58V, the erase voltage is-0.21V, and the switching ratio is more than 102。
The repeatability of the storage characteristics of the thin film resistive random access memory obtained in the embodiment after being activated is shown in fig. 9. It can be seen from the figure that the current-voltage characteristic curve is substantially consistent during 20 voltage cycle scans, indicating that the device has good repeatability.
The high and low resistance retention time read by the thin film resistive random access memory obtained in the embodiment at 0.25V is shown in FIG. 10. As can be seen from the figure, the high and low resistance states can be kept above 450s without obvious attenuation, which indicates that the device has good stability.
Example 2
The thin film resistance change memory of this example and the manufacturing method thereof are the same as example 1 except that the thickness of the copper oxide thin film is 32 nm.
A typical current-voltage characteristic curve of the thin film resistive random access memory obtained in this example before activation is shown in fig. 11. When the current limiting value is 100 μ a and the voltage scanning mode is-1V → 0V → -1V, the memory characteristics of the device are similar to those of the memory before activation in embodiment 1, a forward electrical hysteresis phenomenon formed by electrons trapped and released by the oxide layer is exhibited, the device reaches a low resistance state at 0.81V and returns to a high resistance state at 0.41V.
The activation process of the thin film resistive random access memory obtained in this embodiment is shown in fig. 12. When the current limiting value is 1000 muA, the electrical hysteresis phenomenon of the device has no obvious change, which indicates that the device can not be subjected to soft breakdown and can not present the bipolar resistance switching behavior.
Example 3
The device of this example was fabricated in the same manner as in example 1, except that the thickness of the copper oxide layer was 4 nm.
A typical current-voltage characteristic curve of the device obtained in this example is shown in fig. 13. As can be seen from the graph, the current-voltage characteristics exhibited a good linear relationship when the thickness of the copper oxide layer was 4nm, indicating that this thinner oxide layer did not respond to KCu due to easier breakdown7S4The electrical contact with Au is affected. This also demonstrates the controllability of the thickness of the films of the invention on the device performance.
The present invention is not limited to the above exemplary embodiments, and any modifications, equivalent replacements, and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A thin film resistive random access memory with an adjustable memory mechanism is characterized in that: the silicon-based substrate (1) with the surface covered with the insulating layer (2) is taken as a base, and KCu is dispersed on the insulating layer (2)7S4A quasi-one-dimensional nanostructure (3); in the KCu7S4One end of the quasi-one-dimensional nano structure (3) is deposited with a first metal film electrode (4) and the KCu7S4The quasi-one-dimensional nano structure (3) forms ohmic contact; in the KCu7S4The other end of the quasi-one-dimensional nano structure (3) is deposited with a copper oxide film (5); a second metal film electrode (6) is deposited in the same area above the copper oxide film (5);
the copper oxide film is evaporated by thermal evaporation with Cu particles with purity not lower than 99.99% as copper source, and the pressure in vacuum chamber is controlled to be 9 × 10 during evaporation-3～1×10-2Pa, evaporation rate of
So that the Cu is spontaneously oxidized in the evaporation process, thereby obtaining an oxide film of Cu-CuxAn O film;
the KCu7S4Quasi-one-dimensional nanostructure, the CuxThe O film and the second metal film electrode form a film resistive random access memory, and the following steps: when the Cu isxKCu when the thickness of the O film is 15-25nm7S4As the active metal electrode, CuxO to Cu+The device has the bipolar resistance change storage characteristic of a conductive wire mechanism; when the Cu isxWhen the thickness of the O film is 30-100nm, the thicker oxide layer is not easy to be subjected to soft breakdown, the trapping effect of the oxide layer plays a main role, and the device has the resistance change storage characteristic of an interface capture mechanism.
2. The thin film resistive-switching memory according to claim 1, wherein: the second metal film electrode (6) is an Au electrode or a Pt electrode; the thickness of the second metal film electrode is 30-100 nm.
3. The thin film resistive-switching memory according to claim 1, wherein: the insulating layer (2) is SiO2Insulating layer, insulating tape, Si3N4Insulating layer, HfO2Insulating layer or Al2O3An insulating layer having a resistivity of not less than 1 × 103Omega-cm, thickness of 100-500 nm.
4. The thin film resistive-switching memory according to claim 1, wherein: the KCu7S4The axial length of the quasi-one-dimensional nano structure is not less than 10 mu m, and the radial length is 100-1000 nm.
5. The thin film resistive-switching memory according to claim 1, wherein: the first metal film electrode (4) is an Au electrode, a Ti/Au composite electrode, a Cr/Au composite electrode, a Ni/Au composite electrode or a Pt electrode;
the thickness of the Au electrode and the Pt electrode is 30-100 nm;
the Ti/Au composite electrode, the Cr/Au composite electrode and the Ni/Au composite electrode are respectively formed by depositing Au with the thickness of 30-100nm on Ti, Cr and Ni with the thickness of 3-10 nm.
6. The thin film resistive-switching memory according to claim 1, wherein: the minimum distance between the first metal thin-film electrode (4) and the second metal thin-film electrode (6) is 5-10 μm.
7. A preparation method of the thin film resistive random access memory according to any one of claims 1 to 6, characterized by comprising the following steps:
(1) adopting a silicon wafer with an insulating layer covered on the upper surface as a substrate, and adding KCu7S4A quasi-one-dimensional nanostructure dispersed on the insulating layer;
(2) by one-time UV exposure lithography and thin film deposition technique in KCu7S4Depositing a first metal film electrode at one end of the quasi-one-dimensional nanostructure;
(3) by means of secondary ultraviolet exposure lithography and electron beam heating evaporation, Cu particles with purity not lower than 99.99% are used as copper source for evaporation, and the air pressure of the vacuum chamber is controlled to be 9 x 10 during evaporation-3～1×10-2Pa, evaporation rate of
So that Cu is spontaneously oxidized during evaporation and thus is in KCu7S4Depositing a copper oxide film on the other end of the quasi-one-dimensional nanostructure;
(4) and depositing a second metal film electrode above the copper oxide film by using a film deposition technology, thereby completing the preparation of the film resistive random access memory.
8. The method of claim 7, wherein: the deposition mode of the first metal film electrode in the step (2) is electron beam evaporation, and the air pressure of a vacuum chamber is not higher than 6 multiplied by 10 during evaporation-3Pa, evaporation rate of
The deposition mode of the second metal film electrode in the step (4) is electron beam evaporation, and the air pressure of a vacuum chamber is not higher than 6 multiplied by 10 during evaporation-3Pa, evaporation rate of
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