CN110010762B - Nonvolatile dual-mode resistive random access memory and preparation method thereof - Google Patents
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Abstract
The invention belongs to the field of resistive random access memory devices, and relates to a dual-mode resistive random access memory device prepared by using interface engineering and a preparation method thereof. The memory device comprises a lower electrode with a nano structure on the surface, a middle functional layer with nano holes on the surface and an upper electrode. Specifically, conducting reduced graphene oxide (rGO) with nano-wrinkled surfaces is adopted as a lower electrode; the middle functional layer is a middle active layer which is formed by coating organic polymer materials on the surface of the lower electrode in a rotating way under certain humidity to form surface holes; metal aluminum (Al) is evaporated as an upper electrode. And finally preparing the nonvolatile dual-mode resistive random access memory. The device has the characteristics of simple structure, excellent performance, diversified functions and the like, and has simple preparation process, low cost and wide application prospect in the field of intelligent storage.
Description
Technical Field
The invention relates to the technical field of semiconductor memories, in particular to a nonvolatile dual-mode resistive random access memory and a preparation method thereof.
Background
With the explosive growth of data, mass information appears in our lives, and meanwhile, the storage of the mass information also becomes a great challenge for the development of storage technology, so that the memory development trend under the background of 'big data' is formed by searching larger storage capacity, more diversified storage, faster reading and writing speed, more convenient use, lower cost and higher environmental protection performance. Currently, applications that utilize organic electronic devices to replace silicon-based electronics have achieved good results. For example, an organic light emitting device is realized by using an organic light emitting material. Importantly, organic resistive random access memories implement Flash-type (Flash) memories by employing filamentary conductance, charge transfer and conformational transition mechanisms, for Dynamic Random Access Memories (DRAMs) by charge trapping and detrapping mechanisms, and for write-once-read-many (WORM) -type storage by carbon filament and redox effects.
Resistive Random Access Memory (RRAM) is a powerful competitor of the next-generation non-volatile memory because of its simple material and structure, small unit area, low manufacturing cost, compatibility with the conventional CMOS process, strong scalability, fast read/write speed, low operation power consumption, and so on.
To date, a range of electroactive polymers, including polymer-based nanocomposites, conjugated polymers, insulating polymers, and metal complexes, have been used to construct resistive memory devices, with metal oxides, metals, graphene, and conductive polymers being the most widely used electrodes. Among them, most resistive memory diodes focus on the implementation of a single function in a single cell, such as a Flash mode, a DRAM mode, and a WORM mode. However, implementing two storage modes or more functions based on a single storage element is challenging.
The traditional memory is mainly focused on a single memory function device, and along with the coming of the 'late molal' era, the traditional single function memory can not meet the use requirements of people more and more, so that the design and preparation of the multifunctional memory become a problem which needs to be solved urgently in the current semiconductor scientific development.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention aims to provide a design idea and a preparation method of a dual-mode resistive random access memory.
In order to achieve the purpose, the invention adopts the following technical scheme:
a nonvolatile dual-mode resistive random access memory adopts conductive reduced graphene oxide (rGO) with nano-wrinkled surfaces as a lower electrode and evaporated metal aluminum (Al) as an upper electrode, and an intermediate functional layer is an intermediate active layer which is formed by coating an organic polymer material on the surface of the lower electrode in a spinning mode under certain humidity to form surface holes.
Organic polymer material of the intermediate functional layer the organic polymer material of the intermediate functional layer is 3-hexyl substituted polythiophene or polymethyl methacrylate.
A nonvolatile dual-mode resistive random access memory is prepared by the following method, which comprises the following specific steps:
1) cleaning treatment of a silicon/silicon dioxide (Si/SiO2) substrate;
2) preparing a reduced graphene oxide lower electrode with a nano-fold structure on the surface by adopting a spin coating method;
3) preparing an intermediate functional layer with nano holes on the surface by adopting a respiratory map method;
4) and preparing an upper electrode.
The nonvolatile dual-mode resistive random access memory prepared by the steps is tested by using a semiconductor tester.
Further technical scheme, in the step 1), Si/SiO2The substrate is treated by respectively adopting deionized water, ethanol, isopropanol and deionized water to carry out ultrasonic treatment for 10min-30min, blowing the substrate by using nitrogen, and finally putting the substrate into an oxygen plasma cleaning machine with the power of 80w and the time of 5min so as to enhance the hydrophilicity of the surface of the substrate.
According to the further technical scheme, the preparation of the lower electrode in the step 2) is that a Graphene Oxide (GO) solution is spin-coated on a substrate, then the substrate is placed in a tubular furnace, argon-hydrogen mixed gas is introduced into the tubular furnace, and high-temperature thermal reduction is carried out to obtain rGO, wherein the reduction temperature is 1000 ℃ and the time is 120 min.
In a further technical scheme, the preparation of the graphene oxide solution is synthesized by an improved Hummers method: 1g of graphite powder and 0.5g of sodium nitrate and 23mL of sulfuric acid (98 wt%) were added to a 500mL flask under an ice-water bath, followed by slow addition of 3g of potassium permanganate and stirring was maintained until a homogeneous solution formed. The solution was kept at 35 ℃ and stirred for 8 hours to avoid overheating and explosion. Then 46mL of deionized water at 40 ℃ was added, the flask was transferred to an oil bath and slowly heated to 95 ℃. After 20 minutes a bright yellow solution was obtained, which was then washed with hydrogen chloride (HCl) and Deionized (DI) water, followed by graphene oxide. Finally, the dispersed graphene oxide was dissolved in a mixed solution (deionized water/methanol: 1/5) and stirred uniformly to obtain a GO solution of 2 mg/ml.
In a further technical scheme, the dosage of the graphene oxide is 200 mu l.
According to the further technical scheme, the surface of the reduced graphene oxide lower electrode prepared by the spin coating method has a nano-fold structure.
In a further technical scheme, the intermediate functional layer in the step 3) is prepared by adopting a breathing diagram method, using chloroform as a solvent, preparing an MEH-PPV solution with the concentration of 5mg/ml, uniformly stirring, spin-coating on the surface of the lower electrode, and finally drying in humid air with the humidity of 35% for 30min at the drying temperature of 70 ℃. In a further technical scheme, the surface of the middle functional layer film prepared by adopting a respiratory map method is provided with nano holes.
In a further technical scheme, the dosage of the MEH-PPV solution is 150 mul.
Further, in the step 4), the lower electrode is prepared by evaporating metal aluminum to the surface of the middle functional layer in a thermal evaporation manner.
In a further technical scheme, the thickness of the upper electrode is 150 nm.
The Si/SiO2Is silicon/silicon dioxide; rGO is reduced graphene oxide; MEH-PPV is poly [ 2-methoxy-5- (2-ethylhexyloxy) -1, 4-phenylenevinylene]。
Advantageous effects
Compared with the prior art, the invention has the following advantages:
1. the technical scheme of the invention designs the memory to simultaneously have nonvolatile Flash and WORM dual-mode resistance change memory performance.
2. The device has the advantages of simple structure, sandwich structure, low cost and simple preparation process.
3. The device of the invention has universality.
4. The device has high stability and repeatability, and the on-off current ratio of Flash and WORM storage processes of the memory is respectively as high as 103And 105And the durability of the storage process is as long as 104For more than a second.
Drawings
Fig. 1 is a schematic diagram of a sandwich structure of a nonvolatile dual-mode resistive random access memory in embodiment 1 of the present invention;
fig. 2(a) is a scanning image of an atomic force microscope with a lower electrode reduced graphene oxide (rGO) as a nonvolatile dual-mode resistive random access memory in embodiment 1 of the present invention;
fig. 2(b) is a scanning picture of an atomic force microscope with an intermediate functional layer of poly [ 2-methoxy-5- (2-ethylhexyloxy) -1, 4-phenylenevinylene ] (MEH-PPV) in the nonvolatile dual-mode resistive random access memory according to embodiment 1 of the present invention;
FIG. 3 is an I-V test curve of a flash and WORM dual-mode storage process;
FIG. 4 is a endurance test curve of a flash and WORM dual-mode storage process;
FIG. 5 is a diagram illustrating the universality verification of flash and WORM dual-mode storage.
Detailed Description
The present invention will be described in further detail with reference to examples and the accompanying drawings.
The following description is only exemplary of the invention, and the details and applications of the invention can be easily understood by those skilled in the art from the description of the invention, and several improvements and modifications can be made without departing from the principle of the invention, and these improvements and modifications should also be construed as the protection scope of the invention.
Example 1
As shown in fig. 1, a structure of a nonvolatile dual-mode resistive random access memory is a sandwich structure, and has an upper electrode, a lower electrode, and an intermediate active layer. The memory adopts conductive reduced graphene oxide with nano-wrinkled surfaces as a lower electrode and evaporated metal aluminum as an upper electrode, and the intermediate functional layer is an intermediate active layer formed by coating an organic polymer material on the surface of the lower electrode in a rotating manner under certain humidity to form surface holes.
A preparation method of a nonvolatile dual-mode resistive random access memory comprises the following steps:
1) treatment of Si/SiO2 substrate: the substrate is ultrasonically treated for 15min by respectively adopting deionized water, ethanol, isopropanol and deionized water, nitrogen is blown dry, and then the substrate is placed into an oxygen plasma cleaning machine with the power of 80w and the time of 5min so as to enhance the hydrophilicity of the surface of the substrate.
2) Preparation of Graphene Oxide (GO) solution: 2g of expanded graphite and 1g of NaNO3、6g KMnO4With 46ml of concentrated H2SO4After mixing under ice-water bath conditions, stirring was carried out for 30 minutes, then heating was carried out to 35 ℃ and stirring was continued for 8 hours. Then, 92ml of ultrapure water at 40 ℃ was added, stirring was continued and the system was heated to 95 ℃ to react for 15 minutes. Finally, 280ml of deionized water at 40 ℃ and 20ml of hydrogen peroxide are added. And cooling to room temperature, centrifugally cleaning for 3 times by using a 5 wt% hydrochloric acid aqueous solution, and centrifugally cleaning for 5 times by using deionized water to obtain the graphene oxide. Dissolving dispersed graphene oxideThe graphene oxide solution of 2mg/ml is obtained by stirring uniformly in a mixed solution (deionized water/methanol ═ 1/5), ultrasonic dispersion is carried out for 15 minutes, and then extremely small and large particles in the solution are removed by centrifugation at 2500 rpm.
3) Preparing a wrinkled lower electrode: and (3) dropping a drop of 200 mu l of graphene oxide solution on a substrate treated by oxygen plasma, carrying out spin coating at 2500rpm for 15s, then dropping a drop of solution, carrying out spin coating to form a film, until the 200 mu l of solution is completely spin-coated, finally placing the film in a tube furnace, introducing argon-hydrogen mixed gas, and carrying out high-temperature thermal reduction to obtain rGO, wherein the reduction temperature is 1000 ℃ and the time is 120 min.
4) Preparing an intermediate functional layer with holes on the surface: adopting a respiring method, using chloroform as a solvent, preparing an MEH-PPV solution with the concentration of 5mg/ml, fully and uniformly stirring, taking 150 mu l of the solution to be spin-coated on the surface of a lower electrode, and finally placing the solution in humid air with the humidity of 35% for drying for 30min at the drying temperature of 70 ℃.
5) Preparing an upper electrode: and evaporating the metal aluminum to the surface of the intermediate functional layer in a thermal evaporation mode. By using a semiconductor tester, the memory obtained by testing shows two memory functions of flash and WORM along with the change of the applied voltage.
As can be seen from fig. 2(a), the reduced graphene oxide (rGO) surface of the lower electrode has nano-wrinkles.
As can be seen from FIG. 2(b), the surface of the middle functional layer poly [ 2-methoxy-5- (2-ethylhexyloxy) -1, 4-phenylenevinylene ] (MEH-PPV) has nano-pores.
As can be seen from fig. 3, when a forward 4V scan voltage is applied, the device is transitioned from a High Resistance State (HRS) to a low resistance state (LRS1), and when a reverse 4V scan voltage is applied, the device is again transitioned to the High Resistance State (HRS), exhibiting flash memory performance; when a forward scanning voltage of 5V is applied, the device is converted from a high-resistance state (HRS) to an ultra-low-resistance state (LRS2), and is maintained in the ultra-low-resistance state without changing with the change of the applied voltage, and WORM storage performance is shown.
It can be seen from fig. 4 that the high resistance state, the low resistance state and the ultra-low resistance state of the device are respectively subjected to pressure test, no obvious attenuation occurs at 10000s, which proves that the flash and WORM dual-mode storage process has good durability, the on-off ratio of the device in the flash storage process is up to more than 1000, the on-off ratio of the WORM storage process is up to 100000, and the device has a higher on-off ratio, thereby being beneficial to reducing the misreading rate in the data storage process.
As can be seen from fig. 5, fig. 5(a) is an electrical property curve of the semiconductor polymer 3-hexyl substituted polythiophene (P3HT) as the intermediate functional layer, which also exhibits flash and WORM dual-mode storage performance, which illustrates that the dual-mode storage performance is independent of the specific material of the intermediate semiconductor functional layer and is only related to the upper and lower electrode interface regulation;
fig. 5(b) is an electrical property curve of an insulator polymer polymethyl methacrylate (PMMA) as an intermediate functional layer, which also shows dual-mode flash and WORM storage performance, and illustrates that the dual-mode storage performance is independent of the specific material of the intermediate layer, and is only related to the interface regulation of the upper and lower electrodes, and it can be seen that the device structure has universality.
Claims (1)
1. A preparation method of a nonvolatile dual-mode resistive random access memory is characterized by comprising the following steps:
1) silicon/silicon dioxide (Si/SiO)2) Cleaning the substrate, namely sequentially placing the substrate in deionized water, ethanol, isopropanol and deionized water, respectively carrying out ultrasonic treatment for 10-30 min, and drying the substrate by nitrogen; finally, putting the substrate into an oxygen plasma cleaning machine, wherein the power of the oxygen plasma cleaning machine is set to be 80w, and the time is 5 min;
2) preparing a reduced graphene oxide lower electrode with a nano-fold structure on the surface by adopting a spin coating method; firstly, spin-coating a Graphene Oxide (GO) solution on a substrate, then placing the substrate in a tubular furnace, and introducing argon-hydrogen mixed gas to carry out high-temperature thermal reduction at 1000 ℃ for 120 min;
the preparation method of the graphene oxide solution comprises the steps of dissolving graphene oxide in a mixed solvent to obtain a Graphene Oxide (GO) solution of 2 mg/ml; the proportion of the mixed solvent is deionized water: the methanol is 1: 5;
3) preparing an intermediate functional layer with nano holes on the surface by adopting a respiration diagram method, wherein the intermediate functional layer is an organic polymer material which is formed by coating an organic polymer material on the surface of a lower electrode in a rotating manner under certain humidity to form the holes on the surface, and the organic polymer material is 3-hexyl substituted polythiophene or polymethyl methacrylate; the preparation of the intermediate functional layer adopts a breathing diagram method, namely, MEH-PPV solution with chloroform as a solvent and the concentration of 5mg/ml is coated on the surface of the lower electrode in a rotating way, and finally, the lower electrode is placed in humid air with the humidity of 35 percent and dried for 30min, and the drying temperature is 70 ℃;
4) and preparing an upper electrode, wherein the upper electrode is metal aluminum deposited by evaporation.
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| CN105820371A (en) * | 2016-06-02 | 2016-08-03 | 厦门大学 | Method for preparing nano-porous material through reactive atmosphere |
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