CN112289926A - Preparation method of fully transparent nonlinear selector - Google Patents
Preparation method of fully transparent nonlinear selector Download PDFInfo
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- CN112289926A CN112289926A CN202010747684.7A CN202010747684A CN112289926A CN 112289926 A CN112289926 A CN 112289926A CN 202010747684 A CN202010747684 A CN 202010747684A CN 112289926 A CN112289926 A CN 112289926A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 32
- 239000002243 precursor Substances 0.000 claims abstract description 31
- 239000000758 substrate Substances 0.000 claims abstract description 25
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 238000004140 cleaning Methods 0.000 claims abstract description 4
- 230000001678 irradiating effect Effects 0.000 claims abstract description 4
- 238000004528 spin coating Methods 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 12
- 229910052751 metal Inorganic materials 0.000 claims description 12
- 239000002184 metal Substances 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 8
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 6
- 239000007800 oxidant agent Substances 0.000 claims description 6
- 230000001590 oxidative effect Effects 0.000 claims description 6
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 4
- 239000004020 conductor Substances 0.000 claims description 4
- 239000008103 glucose Substances 0.000 claims description 4
- 235000006408 oxalic acid Nutrition 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 229910052735 hafnium Inorganic materials 0.000 claims description 3
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 claims description 3
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 229910052715 tantalum Inorganic materials 0.000 claims description 3
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 229910052721 tungsten Inorganic materials 0.000 claims description 2
- 239000010937 tungsten Substances 0.000 claims description 2
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 8
- 230000008901 benefit Effects 0.000 abstract description 7
- 230000001939 inductive effect Effects 0.000 abstract description 4
- 238000003860 storage Methods 0.000 abstract description 3
- 239000000306 component Substances 0.000 description 15
- 238000004519 manufacturing process Methods 0.000 description 6
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 4
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- 230000000694 effects Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000002457 bidirectional effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N70/00—Solid-state devices having no potential barriers, and specially adapted for rectifying, amplifying, oscillating or switching
- H10N70/011—Manufacture or treatment of multistable switching devices
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10B—ELECTRONIC MEMORY DEVICES
- H10B63/00—Resistance change memory devices, e.g. resistive RAM [ReRAM] devices
- H10B63/20—Resistance change memory devices, e.g. resistive RAM [ReRAM] devices comprising selection components having two electrodes, e.g. diodes
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Semiconductor Memories (AREA)
- Optical Modulation, Optical Deflection, Nonlinear Optics, Optical Demodulation, Optical Logic Elements (AREA)
Abstract
The invention relates to the technical field of information storage, in particular to a preparation method of a fully transparent nonlinear selector, which comprises the following steps: s1: cleaning the surface of the substrate for later use; s2: preparing a precursor solution of an oxide, putting the precursor solution into a beaker, and fully stirring; s3: adding a component regulator into the beaker and fully stirring the solution; s4: spin-coating the solution obtained in the step S3 on a substrate and irradiating the substrate with ultraviolet light to obtain an intermediate layer; s5: and growing an electrode layer on the intermediate layer to finish the preparation. In the invention, the components of the intermediate layer are controlled by introducing the component regulator in the preparation process of the intermediate layer, and the ultraviolet light is used for inducing the precursor solution to form the film. The experimental process can be carried out at room temperature and normal pressure, and compared with the existing preparation method of the nonlinear selector, the method has the advantages of simple operation, low requirement on equipment, easy repeated test, strong compatibility and the like, and can be used as an ideal method for preparing the transparent nonlinear selector.
Description
Technical Field
The invention relates to the technical field of information storage, in particular to a preparation method of a fully transparent nonlinear selector.
Background
In recent years, transparent wearable electronic products are more and more popularized in the life of people, and have huge market prospects. The memory cell is used as a core component, and has a decisive effect on the performance of the product. However, after the memory cell is highly integrated, leakage current may occur between adjacent cells, which may cause cell cross-talk and induce data misreading. Therefore, it is necessary to connect the memory cell in series with a transparent switching cell or selector. The non-linear selector has a structure similar to that of the storage unit, and is convenient to integrate; in addition, the non-linear selector shows a continuous current-voltage (I-V) transition relation under an electric field, and has better stability compared with other switch units; in addition, the non-linear selector can pass larger current, and protective current is not required to be applied, so that the problem of hard breakdown is not worried about. Thus, the transparent non-linear selector has a unique advantage in addressing the problem of crosstalk in wearable electronics.
However, the fabrication of transparent nonlinear selectors faces a number of difficulties. Firstly, the preparation difficulty of the middle layer of the selector is high, the ultrathin film with the thickness of only a few nanometers needs to be prepared, the control of material components is very accurate, and the requirement on experimental equipment is high. In addition, the preparation process often requires a heat treatment, and the process is difficult to be compatible with many transparent substrates, especially flexible transparent substrates. There are also limitations on device structure, such as strict structural symmetry.
Chinese patent CN110752293A discloses a bidirectional threshold switch selection device and a method for manufacturing the same, wherein the difficulty in manufacturing the intermediate layer of the selector is high, a film with a thickness of only a few nanometers needs to be manufactured, the control of the material composition is very precise, and the requirement on the equipment is very high. Meanwhile, the preparation process needs to be subjected to heat treatment, and the process is difficult to be compatible with many transparent substrates, especially flexible transparent substrates.
Disclosure of Invention
The invention provides a preparation method of a fully transparent nonlinear selector, which has low requirements on equipment, small preparation difficulty and strong process compatibility, and aims to overcome the defects of high preparation difficulty and low process compatibility in the prior art.
In the technical scheme, a preparation method of a fully transparent nonlinear selector is provided, which comprises the following steps:
s1: cleaning the surface of the substrate for later use;
s2: preparing a precursor solution of an oxide, putting the precursor solution into a beaker, and fully stirring;
s3: adding a component regulator into the beaker and fully stirring the solution;
s4: spin-coating the solution obtained in the step S3 on a substrate and irradiating the substrate with ultraviolet light to obtain an intermediate layer;
s5: and growing an electrode layer on the intermediate layer to finish the preparation.
In the invention, the components of the intermediate layer are controlled by introducing the component regulator in the preparation process of the intermediate layer, and the ultraviolet light is used for inducing the precursor solution to form the film. The experimental process can be carried out at room temperature and normal pressure, and compared with the existing preparation method of the nonlinear selector, the method has the advantages of simple operation, low requirement on equipment, easy repeated test, strong compatibility and the like, and can be used as an ideal method for preparing the transparent nonlinear selector.
Preferably, the substrate is sequentially cleaned by ethanol and deionized water in the step 1, and then dried for later use.
Preferably, the above step S2 includes the steps of:
s21: weighing precursor metal powder by using an analytical balance, and placing the precursor metal powder in a clean beaker;
s22: and slowly dripping an oxidant into the precursor solution in the beaker to obtain the precursor solution, and fully stirring.
Preferably, the component regulator in step S3 is one or more of oxalic acid, glucose, thiourea, formaldehyde, ethanol, and hydrazine hydrate, and the ratio of the added component regulator to the precursor solution in step S22 is 1:25 to 1: 50.
Preferably, the power of the ultraviolet irradiation in step S4 is 60-200W, and the time is 30-120 min.
Preferably, the thickness of the intermediate layer in the step S4 is 10-100 nm, and the thickness of the electrode layer in the step S5 is 110-130 nm.
Preferably, the precursor metal powder in step S21 is one of tantalum, titanium, nickel, tungsten, and hafnium.
Preferably, the above step S4 is performed in a temperature environment of 20 ° to 30 °.
Preferably, the substrate in the step S1 is a transparent conductive material such as SnO2 conductive glass (FTO) doped with fluorine, and the electrode layer in the step S5 is a transparent conductive material such as an indium tin oxide semiconductor transparent conductive film (ITO).
Preferably, the oxidant added in step S22 is analytically pure hydrogen peroxide with a mass fraction of 30%.
Compared with the prior art, the beneficial effects are:
in the invention, the components of the intermediate layer are controlled by introducing the component regulator in the preparation process of the intermediate layer, and the ultraviolet light is used for inducing the precursor solution to form the film. The experimental process can be carried out at room temperature and normal pressure, and compared with the existing preparation method of the nonlinear selector, the method has the advantages of simple operation, low requirement on equipment, easy repeated test, strong compatibility and the like, and can be used as an ideal method for preparing the transparent nonlinear selector. The transparent non-linear selector prepared by the method has the advantages of no need of over precise control of the composition of the intermediate layer, high repetition rate, compatibility with various transparent substrates, and non-linear ratio higher than 104. The advantageous effects of the present invention will become more apparent in the following description.
Drawings
FIG. 1 is a schematic flow chart of a method for fabricating a fully transparent non-linear selector according to an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of a fully transparent non-linear selector obtained by a method for manufacturing a fully transparent non-linear selector according to an embodiment of the present invention;
FIG. 3 is a schematic diagram of an I-V curve of a fully transparent non-linear selector obtained by a method for manufacturing the fully transparent non-linear selector according to an embodiment of the present invention.
Wherein, A-substrate; b-an intermediate layer; and C-electrode layer.
Detailed Description
The drawings are for illustrative purposes only and are not to be construed as limiting the patent; for the purpose of better illustrating the embodiments, certain features of the drawings may be omitted, enlarged or reduced, and do not represent the size of an actual product; it will be understood by those skilled in the art that certain well-known structures in the drawings and descriptions thereof may be omitted. The positional relationships depicted in the drawings are for illustrative purposes only and are not to be construed as limiting the present patent.
The same or similar reference numerals in the drawings of the embodiments of the present invention correspond to the same or similar components; in the description of the present invention, it should be understood that if there are terms such as "upper", "lower", "left", "right", "long", "short", etc., indicating orientations or positional relationships based on the orientations or positional relationships shown in the drawings, it is only for convenience of description and simplicity of description, but does not indicate or imply that the device or element referred to must have a specific orientation, be constructed in a specific orientation, and be operated, and therefore, the terms describing the positional relationships in the drawings are only used for illustrative purposes and are not to be construed as limitations of the present patent, and specific meanings of the terms may be understood by those skilled in the art according to specific situations.
The technical scheme of the invention is further described in detail by the following specific embodiments in combination with the attached drawings:
examples
Fig. 1 to 3 illustrate an embodiment of a method for manufacturing a fully transparent non-linear selector, which includes the following steps:
s1: cleaning the surface of the substrate A for later use;
s2: preparing a precursor solution of an oxide, putting the precursor solution into a beaker, and fully stirring;
s3: adding a component regulator into the beaker and fully stirring the solution;
s4: spin-coating the solution obtained in the step S3 on a substrate A and irradiating the substrate A by using ultraviolet light to obtain an intermediate layer B;
s5: and growing an electrode layer C on the intermediate layer B to finish the preparation.
In step 1 in this embodiment, the substrate a is sequentially cleaned with ethanol and deionized water, and then dried for later use.
Step S2 in the present embodiment includes the steps of:
s21: weighing 1g of precursor metal powder by using an analytical balance, and placing the precursor metal powder in a clean beaker;
s22: slowly dripping 10ml of analytically pure hydrogen peroxide oxidant with the mass fraction of 30% into the precursor solution in the beaker to obtain the precursor solution, and stirring for 3 hours to obtain a precursor metal oxide intermediate layer B.
The added precursor metal powder is tungsten powder to obtain a tungsten oxide intermediate layer B with the thickness of 50nm, and of course, other metal powder with good conductivity such as tantalum, titanium, nickel, hafnium and the like can be added, the quality can be of other values, the thicknesses of the intermediate layers B obtained by adopting the metal powder with different qualities are different, and the intermediate layer B can be only 10 nm-100 nm thick. It should be noted that the type, volume and mass fraction of the added oxidant are determined according to the added metal powder, and are only a preferred reference value, and are not to be construed as limiting the present solution; in addition, the stirring time of 3 hours is only a preferable value in this embodiment, and of course, other stirring time may be adopted as long as the solution is sufficiently stirred.
The component regulator in step S3 in this example is 0.4g of 80% hydrazine hydrate, but it is needless to say that one of oxalic acid, glucose, thiourea, formaldehyde and ethanol or a combination of oxalic acid, glucose, thiourea, formaldehyde, ethanol and hydrazine hydrate can be used, and it should be noted that the addition of 80% hydrazine hydrate in 0.4g of mass fraction in this example is only a preferred embodiment, and is not to be construed as a limitation to this embodiment, which is for the preparation of linear hydrazine hydrate higher than 104Of course, other qualities and types of ingredient modifiers may be used to make selectors of varying linearity ratios; in addition, the weight of the added component regulator is not fixed, and the mass ratio of the component regulator to the precursor solution in the step S22 is 1: 25-1: 50.
In this embodiment, the power of the ultraviolet light irradiation in step S4 is 100W, and the time is 60min, which is only a preferred value in this embodiment and cannot be understood as a limitation to this embodiment, and the power of the ultraviolet light is 60 to 200W, and the irradiation time is 30min to 120 min.
In this embodiment, in step S5, an electrode layer C is grown by magnetron sputtering with a thickness of 120nm, and is covered with a mask plate with an aperture of 100 μm. It should be noted that this is only a preferable value in this embodiment, and it is needless to say that another aperture value or thickness of the electrode layer C may be adopted as long as the aperture is 80 to 120 μm and the thickness of the electrode layer C is 110 to 130 mm.
Step S4 in this example is performed under an atmosphere of 20 ° to 30 ° and normal pressure.
The substrate a in step S1 is SnO2 conductive glass (FTO) doped with fluorine, and the electrode layer C in step S5 is an indium tin oxide semiconductor transparent conductive film (ITO), although other transparent conductive materials may be used.
As shown in FIG. 3, the semiconductor analyzer was used for characterization, and when the read voltage was 3V, the current was 1.76X 10-4A; the half voltage value is 1.5V, the corresponding current magnitude is 5.07 multiplied by 10-9A, and the nonlinear ratio is 1.76 multiplied by 10-4A/5.07 multiplied by 10-9A which is 35200.
In the invention, the component regulator is introduced in the preparation process of the intermediate layer B to control the component B of the intermediate layer, and the ultraviolet light is used for inducing the precursor solution to form the film. The experimental process can be carried out at room temperature and normal pressure, and compared with the existing preparation method of the nonlinear selector, the method has the advantages of simple operation, low requirement on equipment, easy repeated test, strong compatibility and the like, and can be used as an ideal method for preparing the transparent nonlinear selector. The transparent nonlinear selector prepared by the method has the advantages that the composition of the intermediate layer B does not need to be controlled too accurately, the repetition rate is high, the transparent nonlinear selector can be compatible with various transparent substrates A, and the nonlinear ratio is higher than 104. The advantageous effects of the present invention will become more apparent in the following description.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (10)
1. A preparation method of a full-transparent nonlinear selector is characterized by comprising the following steps:
s1: cleaning the surface of the substrate for later use;
s2: preparing a precursor solution of an oxide, putting the precursor solution into a beaker, and fully stirring;
s3: adding a component regulator into the beaker and fully stirring the solution;
s4: spin-coating the solution obtained in the step S3 on a substrate and irradiating the substrate with ultraviolet light to obtain an intermediate layer;
s5: and growing an electrode layer on the intermediate layer to finish the preparation.
2. The method as claimed in claim 1, wherein the substrate is sequentially cleaned with ethanol and deionized water in step 1, and then dried for use.
3. The method as claimed in claim 1, wherein the step S2 comprises the steps of:
s21: weighing precursor metal powder by using an analytical balance, and placing the precursor metal powder in a clean beaker;
s22: and slowly dripping an oxidant into the precursor solution in the beaker to obtain the precursor solution, and fully stirring.
4. The method for preparing a fully transparent non-linear selector as claimed in claim 1, wherein the component regulator in step S3 is one or more of oxalic acid, glucose, thiourea, formaldehyde, ethanol, and hydrazine hydrate, and the mass ratio of the added component regulator to the precursor solution in step S22 is 1:25 to 1: 50.
5. The method as claimed in claim 1, wherein the power of the uv irradiation in step S4 is 60-200W for 30-120 min.
6. The method as claimed in claim 1, wherein the thickness of the middle layer in step S4 is 10-100 nm, and the thickness of the electrode layer in step S5 is 110-130 nm.
7. The method as claimed in claim 3, wherein the precursor metal powder in step S21 is one of tantalum, titanium, nickel, tungsten, and hafnium.
8. The method as claimed in claim 5, wherein the step S4 is performed at a temperature of 20 ° to 30 °.
9. The method as claimed in claim 1, wherein the substrate in step S1 and the electrode layer in step S5 are both made of transparent conductive materials.
10. The method for preparing a fully transparent nonlinear selector according to claim 1, wherein the oxidant added in step S22 is analytically pure hydrogen peroxide with a mass fraction of 30%.
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