CN109192750B - Flexible organic nonvolatile memory device with low voltage and high speed erasing and writing and preparation method thereof - Google Patents
Flexible organic nonvolatile memory device with low voltage and high speed erasing and writing and preparation method thereof Download PDFInfo
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- CN109192750B CN109192750B CN201810811310.XA CN201810811310A CN109192750B CN 109192750 B CN109192750 B CN 109192750B CN 201810811310 A CN201810811310 A CN 201810811310A CN 109192750 B CN109192750 B CN 109192750B
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Abstract
The invention provides a low-voltage high-speed erasing and writing flexible organic nonvolatile memory device and a preparation method thereof. The poly-alpha-methyl styrene organic polymer is used as the storage layer, and the poly-alpha-methyl styrene has high surface smoothness and good storage effect, so that a good foundation can be provided for the growth of the active layer, the carrier mobility of the active layer is improved, the retention and fatigue resistance of the storage device are effectively improved, and low-voltage high-speed erasing is realized.
Description
Technical Field
The invention belongs to the technical field of flexible organic electronics, and particularly relates to a low-voltage high-speed erasable flexible organic nonvolatile memory device and a preparation method thereof.
Background
Flexible organic electronic devices are organic material electronic devices fabricated on flexible/malleable substrates. Compared with the traditional silicon-based electronic device, the flexible organic electronic device has the advantages of light weight, low-temperature integration, flexibility, large-area manufacture in any shape and the like, and has wide application prospects in the fields of information, energy, medical treatment, national defense and the like, such as flexible organic nonvolatile memories, organic field effect transistors, organic solar cells, sensors, organic light emitting diodes and the like.
In which a flexible organic non-volatile memory device has a memory layer interposed between an insulating layer and a semiconductor layer of a conventional flexible transistor. According to different working principles and device structures, the currently studied organic nonvolatile memories at home and abroad can be classified into an electret type, a ferroelectric polymer type and a floating gate type based on an organic field effect transistor structure.
In the prior art, methods such as electron beam evaporation and pulse laser are generally adopted to prepare a metal oxide film as a storage layer of a flexible organic nonvolatile memory device, the preparation method is complex, and the problems of poor stability, high working voltage and the like of the metal oxide film as the storage layer still exist, so that the search for a new material to replace the metal oxide film storage layer is an important direction for developing the flexible organic nonvolatile memory device.
Disclosure of Invention
Based on the above, the invention provides a low-voltage high-speed erasing flexible organic nonvolatile memory device and a preparation method thereof, the memory device does not need to use a metal oxide film as a memory layer, the memory device has the advantages of low operation voltage, small erasing pulse width, excellent retention and fatigue resistance, and the preparation method has the advantages of simple operation, mild conditions and low cost.
The flexible organic nonvolatile memory device comprises a substrate, and a bottom electrode, an insulating layer, a memory layer, an active layer and a source drain electrode which are sequentially stacked on the substrate, wherein the memory layer is poly alpha-methyl styrene.
Compared with the prior art, the poly-alpha-methylstyrene organic polymer is used as the storage layer, the storage and retention characteristics of hydrophobic and nonpolar substances in the characteristics of the polymer electret are superior to those of hydrophilic and polar substances, and in addition, the weak-polarity substances are selected, so that a good organic semiconductor and electret storage layer interface can be formed, a good foundation can be provided for the growth of an active layer, the carrier mobility of the active layer is improved, and the retention and fatigue resistance of the memory device are effectively improved.
Further, the substrate is a flexible muscovite substrate, and the insulating layer is aluminum oxide. The alumina and the muscovite substrate can form firm chemical bonds such as O-Si-O, O-Al-O and the like near the interface, reduce the electron barrier height between the alumina and the muscovite substrate and are beneficial to improving the electron injection efficiency of the memory device.
Further, the active layer is pentacene.
The preparation method of the flexible organic nonvolatile memory device with low voltage and high speed erasing provided by the invention comprises the following steps:
s1: depositing a bottom electrode on a substrate;
s2: preparing an aluminum oxide insulating layer: depositing an alumina film on the surface of the bottom electrode, and then sequentially carrying out annealing treatment and UV/O3Surface activation treatment is carried out to prepare an aluminum oxide insulating layer;
s3: preparing a storage layer: spin-coating poly alpha-methylstyrene solution on the surface of the alumina insulating layer to form a film, and annealing to obtain a poly alpha-methylstyrene film as a storage layer;
s4: preparing an active layer: depositing pentacene on the poly alpha-methyl styrene film as an active layer;
s5: preparing a source drain electrode: and depositing metal on the pentacene to be used as a source drain electrode.
Compared with the prior art, the preparation method provided by the invention is simple to operate, mild in condition and low in cost, and can be used for preparing the organic nonvolatile charge trap type memory device which is low in operating voltage, small in erasing pulse width, excellent in maintaining and anti-fatigue characteristics, good in repeated erasing performance and bending-resistant. The poly alpha-methyl styrene is used as a storage layer, and the poly alpha-methyl styrene film has good storage effect and can realize low-voltage high-speed erasing on the flexible substrate.
Further, the substrate in step S1 is flexible muscovite with a thickness of 1-10 μm.
Further, the bottom electrode is deposited in step S1 by depositing 10-20nm of gold as the bottom electrode at a rate of 0.01-0.03nm/S by thermal evaporation.
Further, the alumina thin film is prepared by the atomic layer deposition technique in step S2, wherein the atomic layer deposition technique uses ozone and trimethylaluminum as reaction precursors, the pulse time of ozone is 0.3-0.7S, the pulse time of trimethylaluminum is 0.01-0.03S, the waiting time is 8-15S, the total number of cycles of pulsing trimethylaluminum and ozone is 80-360 times, and the substrate temperature is 80-300 ℃. The insulating layer of the aluminum oxide is made by using ozone and trimethylaluminum as precursor reactants, so that the insulating property of the thin film of the aluminum oxide can be improved, the working voltage of the device is reduced, and the erasing speed of the device is improved.
Further, the annealing treatment in the step S2 is carried out under the condition of oxygen flow, the oxygen flow is 1.5-2L/min, the treatment temperature is 80-400 ℃, and the treatment time is 10-60 min; the UV/O3The surface activation treatment condition is that the sample is irradiated for 1-10min at a distance of 10-40cm from the ultraviolet lamp by using ultraviolet light with the wavelength of 185-245 nm.
Further, in the step S3, the poly α -methylstyrene solution uses toluene as a solvent, and the mass concentration of poly α -methylstyrene is 0.05% -0.5%; the annealing temperature is 40-150 ℃.
Further, the deposition thickness of the pentacene in the step S4 is 30-50nm, the deposition rate is 0.01-0.05nm/S, and the substrate temperature during deposition is 50-120 ℃.
Drawings
FIG. 1 is a schematic diagram of a memory device;
FIG. 2 is a leakage current density curve of an alumina film at different growth temperatures under different field strengths;
FIG. 3 is a graph of absolute value of drain current versus gate voltage hysteresis for a memory device prepared in example 2;
FIG. 4 is a graph showing the on-state and off-state current holding characteristics of the memory device prepared in example 2;
FIG. 5 is a schematic diagram showing the repeated erasing and writing characteristics of the memory device prepared in example 2;
fig. 6 is a schematic view showing the flexible bending characteristics of the memory device prepared in example 2.
Detailed Description
According to the invention, poly-alpha-methylstyrene is used as a storage layer on the high-temperature-resistant flexible substrate, and the special storage effect of the poly-alpha-methylstyrene is utilized, so that the low-voltage high-speed erasing performance of the storage device is improved. By scientifically adjusting the thickness of the alumina insulating layer and reasonably controlling the spin coating condition of the poly alpha-methylstyrene storage layer, the leakage current of the storage device is reduced, and the storage window of the storage device is increased. The technical solution of the present invention will be described below with reference to specific examples.
The preparation method of the flexible organic nonvolatile memory device with low voltage and high speed erasing comprises the following steps:
s1: depositing a gate electrode on a cleaned substrate
Specifically, a flexible muscovite of 15X 15mm was selected, and separated and peeled off with a tape or a blade into a substrate sheet having a thickness of 10 μm. Gold electrodes with a thickness of 20nm were then deposited on the mica substrate using thermal evaporation at a deposition rate of 0.02 nm/s.
S2: preparation of alumina insulating layer
Specifically, the sample obtained in step S1 is heated to T (i.e., the growth temperature of the alumina thin film), the ozone and trimethylaluminum are used as precursor reactants, the ozone pulse time is set to 0.5S, the trimethylaluminum pulse time is set to 0.02S, the waiting time is set to 10S, and the total number of pulse cycles is set to X times, and the alumina thin film is deposited on the surface of the gate electrode by using the atomic layer deposition technique. Then annealing treatment is carried out in a rapid annealing furnace under the condition of oxygen introduction, the oxygen flow is 1.5L/min, the treatment temperature is 300 ℃, and the treatment time is 30 min. And finally, irradiating the sample for 5min at a position 10cm away from the ultraviolet lamp by using ultraviolet light with the wavelength of 220nm to prepare the aluminum oxide insulating layer.
S3: preparation of the storage layer
Dissolving poly alpha-methyl styrene in toluene to prepare poly alpha-methyl styrene solution with mass concentration of C, spin-coating poly alpha-methyl styrene solution on the surface of an alumina insulating layer to form a film, and then carrying out annealing treatment at 120 ℃ for Y min to obtain a poly alpha-methyl styrene film as a storage layer.
S4: preparation of active layer
The sample obtained in step S3 (gold electrode, alumina insulating layer, and poly α -methylstyrene memory layer laminated in this order on a muscovite substrate) was heated to 100 ℃, and a pentacene film having a thickness of 40nm was deposited as an active layer on the poly α -methylstyrene film at a rate of 0.02nm/S by thermal evaporation.
S5: preparing source-drain electrode
And depositing a gold electrode with the thickness of 40nm on the pentacene film at the speed of 0.02nm/s by adopting a thermal evaporation method to be used as a source electrode and a drain electrode.
Wherein, the alumina film growth temperature T, the total number of cycles X of the ozone and the trimethylaluminum pulses in step S2, the annealing treatment time Y of the poly α -methylstyrene film in step S3, and the mass concentration C of the poly α -methylstyrene solution are shown in table 1:
table 1.
| T/℃ | X/times | Y/min | C/％ | |
| Example 1 | 250 | 167 | 5 | 0.05 |
| Example 2 | 250 | 167 | 5 | 0.1 |
| Example 3 | 250 | 167 | 5 | 0.2 |
| Example 4 | 250 | 167 | 5 | 0.3 |
| Example 5 | 250 | 167 | 5 | 0.4 |
| Example 6 | 250 | 167 | 5 | 0.5 |
| Example 7 | 200 | 167 | 5 | 0.1 |
| Example 8 | 150 | 167 | 5 | 0.1 |
| Example 9 | 80 | 167 | 5 | 0.1 |
| Comparative example 1 | 250 | 84 | 20 | 0.1 |
| Comparative example 2 | 250 | 84 | 5 | 0.1 |
Please refer to fig. 1, which is a schematic structural diagram of a memory device prepared by the present invention, and the memory device includes a flexible muscovite substrate 1, and a bottom electrode 2, an aluminum oxide insulating layer 3, a poly α -methylstyrene storage layer 4, a pentacene active layer 5, and a source/drain electrode 6 stacked in sequence thereon.
See table 2, which is a table of the memory windows at different voltages for memory devices made using different poly alpha methylstyrene concentrations. The table reflects that at the same voltage, at C below 0.1%, the memory window increases with increasing concentration; when C is higher than 0.1%, the storage window decreases with increasing concentration; the storage window is maximized at 0.1% C. At the same concentration, the memory window increases with increasing voltage.
Table 2.
Referring to fig. 2, the leakage current density of an alumina film at different field strengths is shown at different growth temperatures. Fig. 2 reflects that the leakage current of the alumina film decreases with the increase of the growth temperature, especially below 200 ℃, the leakage current of the alumina film with the same thickness significantly decreases with the increase of the temperature, and the leakage current of the alumina film above 200 ℃ has smaller temperature variation.
Referring to fig. 3, a graph of absolute value of drain current versus gate voltage hysteresis for a low voltage high speed erasable flexible organic non-volatile memory device prepared in example 2 is shown. A counterclockwise loop is evident from fig. 3, and such a loop is typical of charge trapping memory devices. When the voltage range of the scanning is 5V, a relatively obvious storage effect appears, and the window is about 0.95V; the memory window of the loop line becomes gradually larger along with the expansion of the scanning voltage range, and when the scanning voltage range is 15V, the memory window is about 18.29V, and the memory device shows a great memory effect.
Referring to fig. 4, the figure shows the on-state and off-state current retention characteristics of the low-voltage high-speed erasable flexible organic nonvolatile memory device prepared in example 2. As can be seen from fig. 4, after holding for 3h, the switching ratio of the memory device still exceeds 103(ii) a Using the method of linear extrapolation, extrapolated to ten years, the switching ratio of the memory device is still 102And the excellent retention property is shown.
Referring to fig. 5, the repeated erasure characteristics of the low-voltage high-speed erasable flexible organic nonvolatile memory device prepared in example 2 are shown. FIG. 5 shows that after 3000 times of erasing and writing, the on-off ratio of the memory device has only slight change from 1.29 × 103Becomes 9.53 × 102It shows excellent repeated erasing and writing characteristics.
Referring to fig. 6, the flexible bending characteristics obtained by the flexible bending test of the flexible organic nonvolatile memory device subjected to low-voltage high-speed erasing of embodiment 2 are shown. When the memory device is bent to 3000 times under the conditions that the bending radius is sequentially from 10 mm, 8 mm and 5mm, the storage window of the memory device is not changed excessively, and the memory device can work normally, which shows that the memory device has excellent storage performance under the bending condition.
In conclusion, the memory device prepared in the embodiment 2 of the present invention has low operating voltage (6V to 4V), small erasing pulse width (100 μ s), good retention characteristics (10 years) and outstanding repeated erasing performance (more than 3000 times).
In contrast, the memory devices prepared in comparative example 1 and comparative example 2 were also tested using an agilent B1500A high precision semiconductor analyzer in a room temperature environment. The results show that the memory device prepared in the comparative example 1 has the defects that the film is cracked due to overlong annealing time of the poly-alpha-methylstyrene film, the growth of a semiconductor unit cell is not facilitated, the leakage current of the device is too large, and the memory window is smaller; comparative example 2 the leakage current of the device is too large and the memory window is small due to the too thin alumina barrier layer.
The prior art generally only uses poly alpha-methylstyrene organic polymers as tunneling layers to improve the carrier mobility of the active layer. Compared with the prior art, the poly-alpha-methylstyrene organic polymer is used as the storage layer, an oxide semiconductor layer does not need to be additionally prepared, the good storage effect of the poly-alpha-methylstyrene organic polymer is utilized to effectively reduce the working voltage and the erasing pulse width of the storage device, and the retention characteristic and the repeated erasing performance of the storage device are improved. Meanwhile, the aluminum oxide film in the memory device is generally prepared from water and trimethylaluminum, and the invention is changed into that ozone and trimethylaluminum react and deposit on the flexible muscovite substrate, so that the aluminum oxide film has better insulation property.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
Claims (1)
1. A preparation method of a flexible organic nonvolatile memory device with low voltage and high speed erasing is characterized in that: the method comprises the following steps:
s1: depositing a bottom electrode on a substrate, wherein the substrate is flexible muscovite and has the thickness of 1-10 mu m; the deposition method of the bottom electrode is that a thermal evaporation method is adopted to deposit a 10-20nm gold layer at a speed of 0.01-0.03nm/s as the bottom electrode;
s2: preparing an aluminum oxide insulating layer: depositing an alumina film on the surface of the bottom electrode by an atomic layer deposition technology, and then sequentially carrying out annealing treatment and UV/O3Surface activation treatment is carried out to prepare an aluminum oxide insulating layer; the atomic layer deposition technology takes ozone and trimethylaluminum as reaction precursors, wherein the pulse time of the ozone is 0.3-0.7s, the pulse time of the trimethylaluminum is 0.01-0.03s, the waiting time is 8-15s, the total pulse cycle number of the trimethylaluminum and the ozone is 80-360 times, and the substrate temperature is 80-300 ℃; the annealing treatment is carried out under the condition of oxygen introduction, the oxygen flow is 1.5-2L/min, the treatment temperature is 80-400 ℃, and the treatment time is 10-60 min; the UV/O3The surface activation treatment condition is that the sample is placed at a distance of 10-40cm from the ultraviolet lampIrradiating for 1-10min by using ultraviolet light with the wavelength of 185-245 nm;
s3: preparing a storage layer: spin-coating poly alpha-methylstyrene solution on the surface of the alumina insulating layer to form a film, and annealing to obtain a poly alpha-methylstyrene film as a storage layer; the poly alpha-methyl styrene solution takes toluene as a solvent, and the mass concentration of the poly alpha-methyl styrene is 0.05-0.5%; the annealing temperature is 40-150 ℃;
s4: preparing an active layer: depositing pentacene on the poly alpha-methyl styrene film as an active layer; the deposition thickness of the pentacene is 30-50nm, the deposition rate is 0.01-0.05nm/s, and the substrate temperature during deposition is 50-120 ℃;
s5: preparing a source drain electrode: and depositing metal on the pentacene to be used as a source drain electrode.
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| TW200945591A (en) * | 2008-04-28 | 2009-11-01 | Ind Tech Res Inst | Memory cell |
| SG183900A1 (en) * | 2010-03-04 | 2012-10-30 | Univ Florida | Semiconductor devices including an electrically percolating source layer and methods of fabricating the same |
| KR102089347B1 (en) * | 2013-10-08 | 2020-03-16 | 경북대학교 산학협력단 | Non-volatile memory device and manufacturing method of the same |
| CN105591029B (en) * | 2016-03-24 | 2018-01-09 | 华南师范大学 | A kind of memory device of organic non-volatile based on hafnium and preparation method thereof |
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| CN101211759A (en) * | 2006-12-28 | 2008-07-02 | 中芯国际集成电路制造(上海)有限公司 | Capacitor, random memory cell and method for forming same |
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