CN109860390A - RRAM device and preparation method thereof based on graphene oxide - Google Patents
RRAM device and preparation method thereof based on graphene oxide Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000010410 layer Substances 0.000 claims abstract description 51
- 239000000758 substrate Substances 0.000 claims abstract description 31
- 239000011241 protective layer Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000003491 array Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- 239000010408 film Substances 0.000 claims description 14
- 238000004140 cleaning Methods 0.000 claims description 11
- 238000000576 coating method Methods 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000004528 spin coating Methods 0.000 claims description 8
- 241000446313 Lamella Species 0.000 claims description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 7
- 239000010409 thin film Substances 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 230000008020 evaporation Effects 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 4
- 235000019441 ethanol Nutrition 0.000 claims description 4
- 239000012528 membrane Substances 0.000 claims description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 4
- 238000000151 deposition Methods 0.000 claims description 3
- 230000008021 deposition Effects 0.000 claims description 3
- 238000005566 electron beam evaporation Methods 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims description 2
- 239000007772 electrode material Substances 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 238000007664 blowing Methods 0.000 claims 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims 1
- 239000010931 gold Substances 0.000 claims 1
- 229910052737 gold Inorganic materials 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000004506 ultrasonic cleaning Methods 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000007769 metal material Substances 0.000 description 3
- 239000013049 sediment Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 238000000231 atomic layer deposition Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 229960000935 dehydrated alcohol Drugs 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000010148 water-pollination Effects 0.000 description 2
- 238000013019 agitation Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000001552 radio frequency sputter deposition Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000011265 semifinished product Substances 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 239000008247 solid mixture Substances 0.000 description 1
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- 239000006228 supernatant Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
- Semiconductor Memories (AREA)
Abstract
A kind of RRAM device and preparation method thereof based on graphene oxide, belongs to technical field of electronic devices.The RRAM device based on graphene oxide includes the conductive substrates being stacked from the bottom to top, dielectric layer and top electrode layer；The top electrode layer includes the top electrode of several arrays on the dielectric layer, and the top electrode is equipped with protective layer on the surface far from dielectric layer.The present invention manufactures dielectric layer using solwution method, realizes that the preparation of inexpensive RRAM device, equipment and raw material investment are less, it can be achieved that large-scale industrial application.
Description
Technical field
The present invention relates to a kind of technology of field of electronic devices, specifically a kind of RRAM device based on graphene oxide
Part (Resistive random access memory, resistive formula random access memory) and preparation method thereof.
Background technique
The rapid development of information to information store and logic circuit in terms of more stringent requirements are proposed.It is traditional based on metal
The dielectric memory of oxide material due to storage density is low, processing cost is high, device preparation technology is complicated and material from
Body limitation etc. makes its development reach capacity, and has been unable to meet the fast-developing demand of information storage.Graphene and its oxide are made
The features such as better mechanical flexibility, faster fast response time, higher on-off ratio can be provided for storage material, and can be with
Realize the micromation of circuit.
The existing preparation process for RRAM dielectric layer is more traditional, such as magnetron RF sputtering system, chemical vapor deposition
(CVD), atomic layer deposition (ALD) etc., but the above method is limited to equipment, and high production cost is unable to satisfy large-scale low-cost
Industrialization demand.
Summary of the invention
The present invention In view of the above shortcomings of the prior art, propose a kind of RRAM device based on graphene oxide and
Preparation method can satisfy the industrialization demand of RRAM low cost.
The present invention is achieved by the following technical solutions:
The present invention relates to a kind of RRAM device based on graphene oxide, including be stacked from the bottom to top substrate, electricity
Dielectric layer and top electrode layer；
The top electrode layer includes the top electrode of several arrays on the dielectric layer, and the top electrode is far from dielectric layer
Surface be equipped with protective layer；
The dielectric layer is graphene oxide film；
The protective layer is metal nickel film, metallic titanium membrane, any one in metal W film.
The top electrode is cylindrical metal nickel film or titanium nitride membrane, with a thickness of 30~80nm, diameter is 0.1~
0.3mm。
The dielectric layer with a thickness of 20~80nm.
The conductive substrates are any one in metal platinum film or highly doped silicon thin film, with a thickness of 50~150nm；It is preferred that
The highly doped silicon thin film in ground uses the highly doped silicon thin film of N-type phosphorus doping.
The present invention relates to the preparation methods of above-mentioned RRAM device, comprising the following steps:
A) substrate is cleaned；
Conductive substrates are successively completely immersed in the beaker for holding deionized water, holds in the beaker of acetone solvent, hold
In the beaker of dehydrated alcohol and holds in the beaker of deionized water and be cleaned by ultrasonic；Substrate is rinsed simultaneously with deionized water later
With being dried with nitrogen；
B) dielectric layer is prepared；
Based on paper " chemical preparation process of graphene " (S.Park and R.S.Ruoff, " Chemical methods
for the production of graphenes,"Nature Nanotechnol,vol.4,no.4,pp.217-24,Apr
2009) the improvement Hummers method mentioned prepares lamella graphene oxide；It is molten that manufactured lamella graphene oxide is dissolved in ethyl alcohol again
In agent, it is configured to the solution that concentration is 0.05~0.25mg/mL；Configured solution is added dropwise in conductive substrates, is revolved
It applies, spin-coating time is no more than 100s, and revolving speed is 400~1200rpm；After spin coating, leading for graphene oxide solution will be coated with
Electric substrate is annealed under 50~200 DEG C of environment, and the time is no more than 1.5h；
C) top electrode layer is prepared；
Granular top electrode material is coated on the dielectric layer by evaporation coating method, forms top electrode layer；
D) protective layer is prepared；
Granular protective layer material is coated on top electrode far from the surface of dielectric layer by evaporation coating method, is made
Obtain the RRAM device based on graphene oxide.
Surface plasma cleaning is carried out to substrate again under vacuum environment after being cleaned by ultrasonic, to enhance lower electrode layer
Hydrophily, improve the filming performance of dielectric layer；The surface plasma cleaning process time need to continue at least 45min, complete
Dielectric layer preparation is carried out after cleaning at surface plasma in 10min.
Technical effect
Compared with prior art, the present invention has the following technical effect that
1) dielectric layer is manufactured using solwution method, realizes the preparation of low cost RRAM, equipment and raw material investment are less, can use
In the preparation of large area RRAM device, large-scale industrial application is realized；
2) resistive effect is good, and required energy consumption is less, is mainly shown as lower SET and RESET voltage；
3) lamella graphene oxide is prepared using improved Hummers method, further reduces graphene oxide dielectric layer
The cost and process flow of preparation.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of embodiment 1；
Fig. 2 is resistive characteristic variations figure of the embodiment 1 within the scope of 50~200 DEG C；
In figure: protective layer 100, top electrode 101, dielectric layer 200, conductive substrates 300.
Specific embodiment
With reference to the accompanying drawing and specific embodiment the present invention will be described in detail.
Embodiment 1
As shown in Figure 1, the present embodiment is related to a kind of RRAM device based on graphene oxide, including it is laminated sets from the bottom to top
Conductive substrates 300, dielectric layer 200 and the top electrode layer set, top electrode layer include top of several arrays on dielectric layer 200
Electrode 101, top electrode 101 are equipped with protective layer 100 on the surface far from dielectric layer 200.
Protective layer 100 uses metal W film.
Top electrode 101 uses cylindrical metal aluminium film, is 0.1~0.3mm with a thickness of 30~80nm, diameter, it is preferable that
With a thickness of 40nm, diameter 0.1mm.
Dielectric layer 200 uses graphene oxide film, with a thickness of 20~80nm.
Conductive substrates 300 use highly doped silicon thin film, with a thickness of 50~150nm, it is preferable that using the N-type with a thickness of 100nm
The highly doped silicon thin film of phosphorus doping.
The present embodiment is related to the preparation method of above-mentioned RRAM, comprising:
A) substrate is cleaned；
Conductive substrates are completely immersed in the beaker for holding deionized water, places the beaker and carries out in deionized water environment
25min ultrasonic cleaning；
After being cleaned by ultrasonic for the first time, conductive substrates are completely immersed in the beaker for holding acetone solvent, are placed the beaker
Second of 25min ultrasonic cleaning is carried out in ion water environment；
After second is cleaned by ultrasonic, with deionized water repeated flushing conductive substrates, cleaning thereon remaining acetone solvent and
Impurity continues for conductive substrates to be completely immersed in the beaker for holding dehydrated alcohol, places the beaker in deionized water environment and carries out
Third time 25min ultrasonic cleaning；
After third time is cleaned by ultrasonic, conductive substrates are pulled out and are suitably rinsed with deionized water, are continued conductive substrates are complete
Immersion is held in the beaker of deionized water, is placed the beaker and is carried out the 4th 25min ultrasonic cleaning in deionized water environment；
After 4th ultrasonic cleaning, conductive substrates are rinsed with deionized water and with being dried with nitrogen；
It will be put into the vacuum chamber of surface plasma cleaning machine through the substrate that above-mentioned ultrasonic cleaning is handled and is dried, carry out table
Face plasma cleaning is to enhance the hydrophily of top electrode 101；The surface plasma cleaning process time continues 50min, completes surface
The preparation of dielectric layer 200 is carried out after plasma cleaning in 10min；
B) dielectric layer 200 is prepared；
The reaction flask of 200~270mL is assembled in ice-water bath, 15~28mL concentrated sulfuric acid is added, and carries out magnetic agitation, together
When the solid mixture of 1~5g graphite powder and 1~5g sodium nitrate is added, and be slowly added to 2~8g potassium permanganate, while controlling anti-
It answers temperature to be no more than 10 DEG C, is taken out after stirring 1~3h under condition of ice bath；
Reaction is stirred at room temperature 3~5 days；Then it is diluted, is stirred using the concentrated sulfuric acid that mass fraction is 2%~7%
After mixing 2h, 3~8mL hydrogen peroxide is added, continues to be centrifuged after stirring 2h；
The dioxysulfate water mixed liquid and hydrochloric acid for being 5%~12% with concentration wash repeatedly, then it is washed with distilled water 3~
7 times, filemot graphene oxide sediment is obtained, graphene oxide sediment is filled in 20~60 DEG C of vacuum oven
Divide drying；
Graphene oxide sediment after abundant drying is put into deionized water, 40~70W power ultrasound is no more than 3h,
Precipitates overnight takes in the vacuum oven for be put into after supernatant liquor eccentric cleaning 20~60 DEG C and is sufficiently dried, obtains lamella
Graphene oxide；
Lamella graphene oxide obtained is dissolved in alcohol solvent, being configured to concentration is the molten of 0.05~0.25mg/mL
Liquid；By configured solution be added dropwise in conductive substrates 300, carry out spin coating, spin-coating time be no more than 100s, revolving speed be 400~
1200rpm；After spin coating, the conductive substrates 300 for being coated with graphene oxide solution are annealed under 50~200 DEG C of environment
Dielectric layer 200 is made in 1h, freezing film；
C) top electrode 101 is prepared；
Granulated metallic material aluminium is placed in the crucible of electron beam evaporation deposition machine, the exposure mask for being 0.1mm by aperture
Plate is covered on dielectric layer 200, and mask plate is lowered on the suction disc in coating machine cavity, is closed cavity and is evaporated plated film
Operation, metallic material of aluminum is coated on dielectric layer 200, forms the semi-finished product with top electrode 101；
D) protective layer 100 is prepared；
After top electrode 101 completes, granulated metallic material tungsten is placed in the crucible of electron beam evaporation deposition machine,
The mask plate that aperture is 0.1mm is covered on top electrode 101, mask plate is lowered on the suction disc in coating machine cavity, is closed
Closed chamber body carries out double evaporation-cooling coating operation, is coated with to form protective layer 100 on top electrode 101.
It is illustrated in figure 2 the resistive test result of the present embodiment RRAM device, using 0 point of abscissa as line of demarcation, negative axis is
RESET (reset) process, positive axis be SET (set) process, voltage bias absolute value all in 2V hereinafter, and resistive be held in
In a certain range, occurs the gradual change phenomenon of certain probability during RESET.
It is emphasized that: the above is only presently preferred embodiments of the present invention, not make in any form to the present invention
Limitation, any simple modification, equivalent change and modification to the above embodiments according to the technical essence of the invention,
All of which are still within the scope of the technical scheme of the invention.
Claims (10)
1. a kind of RRAM device based on graphene oxide, which is characterized in that including be stacked from the bottom to top conductive substrates,
Dielectric layer and top electrode layer；
The top electrode layer includes the top electrode of several arrays on the dielectric layer, and the top electrode is in the table far from dielectric layer
Face is equipped with protective layer；
The dielectric layer is graphene oxide film.
2. according to claim 1 based on the RRAM device of graphene oxide, characterized in that the protective layer is that metallic nickel is thin
Film, metallic titanium membrane, any one in metal W film.
3. according to claim 1 based on the RRAM device of graphene oxide, characterized in that the top electrode is cylindrical gold
Belong to nickel film or titanium nitride membrane, with a thickness of 30~80nm, diameter is 0.1~0.3mm.
4. according to claim 1 based on the RRAM device of graphene oxide, characterized in that the dielectric layer with a thickness of
20~80nm.
5. according to claim 1 based on the RRAM device of graphene oxide, characterized in that the conductive substrates are metal platinum
Any one in film or highly doped silicon thin film, with a thickness of 50~150nm.
6. a kind of preparation method of any one of Claims 1 to 5 RRAM device characterized by comprising
A) substrate is cleaned；
Conductive substrates are successively completely immersed in the beaker for holding deionized water, are held in the beaker of acetone solvent, hold it is anhydrous
In the beaker of ethyl alcohol and holds in the beaker of deionized water and be cleaned by ultrasonic；Substrate is rinsed with deionized water later and uses nitrogen
Air-blowing is dry；
B) dielectric layer is prepared；
Lamella graphene oxide is prepared by improved Hummers method, manufactured lamella graphene oxide is dissolved in alcohol solvent
In, it is configured to the solution that concentration is 0.05~0.25mg/mL；Configured solution is added dropwise in conductive substrates, spin coating is carried out,
Spin-coating time is no more than 100s, and revolving speed is 400~1200rpm；After spin coating, the conductive base of graphene oxide solution will be coated with
Bottom is annealed under 50~200 DEG C of environment, and the time is no more than 1.5h；
C) top electrode layer is prepared；
Granular top electrode material is coated on the dielectric layer by evaporation coating method, forms top electrode layer；
D) protective layer is prepared；
Granular protective layer material is coated on top electrode far from the surface of dielectric layer by evaporation coating method, base is made
In the RRAM device of graphene oxide.
7. the preparation method of RRAM device according to claim 6, characterized in that after being cleaned by ultrasonic, in vacuum ring
Surface plasma cleaning is carried out to conductive substrates again under border；The surface plasma cleaning process time need to continue at least 45min,
It completes to carry out dielectric layer preparation in 10min after surface plasma cleans.
8. the preparation method of RRAM device according to claim 6, characterized in that the graphene oxide solution at 20 DEG C extremely
It is configured under 30 DEG C of environment, is at the uniform velocity stirred to clarify, 5min or more need to be stood after stirring under room temperature environment.
9. the preparation method of RRAM device according to claim 8, characterized in that the graphene oxide solution passes through 0.85
μm aperture, PES material filter tip syringe be added dropwise in conductive substrates.
10. the preparation method of RRAM device according to claim 6, characterized in that the evaporation coating method will be granular
Top electrode layer material or protective layer material are placed in crucible, and the mask plate that aperture is 0.1~0.3mm is covered in dielectric layer
On, it is put into electron beam evaporation deposition machine and is evaporated coating operation.
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| CN111668253A (en) * | 2020-06-22 | 2020-09-15 | 中国科学院微电子研究所 | Resistive random access memory and preparation method thereof |
| CN112382723A (en) * | 2020-11-13 | 2021-02-19 | 西交利物浦大学 | Resistive random access memory doped with two-dimensional material and preparation method thereof |
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Application publication date: 20190607 |