CN113151902A - Method for producing organic ferroelectric crystal material and organic ferroelectric crystal material - Google Patents
Method for producing organic ferroelectric crystal material and organic ferroelectric crystal material Download PDFInfo
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- CN113151902A CN113151902A CN202110441375.1A CN202110441375A CN113151902A CN 113151902 A CN113151902 A CN 113151902A CN 202110441375 A CN202110441375 A CN 202110441375A CN 113151902 A CN113151902 A CN 113151902A
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- 239000013078 crystal Substances 0.000 title claims abstract description 62
- 239000000463 material Substances 0.000 title claims abstract description 31
- 238000004519 manufacturing process Methods 0.000 title description 2
- 239000000758 substrate Substances 0.000 claims abstract description 45
- 238000000576 coating method Methods 0.000 claims abstract description 18
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- 238000010008 shearing Methods 0.000 claims abstract description 6
- 238000007790 scraping Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 19
- 239000011248 coating agent Substances 0.000 claims description 12
- 229910052751 metal Inorganic materials 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 229920002120 photoresistant polymer Polymers 0.000 claims description 8
- 239000011651 chromium Substances 0.000 claims description 6
- 235000012239 silicon dioxide Nutrition 0.000 claims description 6
- 239000010931 gold Substances 0.000 claims description 5
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000000137 annealing Methods 0.000 claims description 3
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 238000003860 storage Methods 0.000 abstract description 8
- 238000001259 photo etching Methods 0.000 abstract description 5
- 238000002425 crystallisation Methods 0.000 abstract description 3
- 230000008025 crystallization Effects 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000000059 patterning Methods 0.000 abstract description 3
- 239000010408 film Substances 0.000 description 7
- 230000015654 memory Effects 0.000 description 6
- 230000001066 destructive effect Effects 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/54—Organic compounds
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B30/00—Production of single crystals or homogeneous polycrystalline material with defined structure characterised by the action of electric or magnetic fields, wave energy or other specific physical conditions
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10B—ELECTRONIC MEMORY DEVICES
- H10B53/00—Ferroelectric RAM [FeRAM] devices comprising ferroelectric memory capacitors
- H10B53/30—Ferroelectric RAM [FeRAM] devices comprising ferroelectric memory capacitors characterised by the memory core region
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- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
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- Semiconductor Memories (AREA)
Abstract
The invention provides a preparation method of an organic ferroelectric crystal material, which comprises the following steps: providing a substrate; forming a strip-shaped groove on the surface of the substrate; dropping the solution of the organic ferroelectric crystal material into the groove; and scraping the solution along the direction of the groove by adopting a scraper, and directionally growing the solution by utilizing the shearing force of the scraper on the solution to obtain the organic ferroelectric crystal single crystal array with the same orientation. The technical scheme provides an organic molecular single crystal film prepared by a blade coating method and an organic ferroelectric array storage device read in a photocurrent nondestructive mode, combines the traditional photoetching patterning technology with a blade coating process, successfully prepares an organic molecular single crystal and a micro-nano storage array device which are single in orientation, high in quality and uniform in crystallization, and promotes the application of the organic ferroelectric array storage device read in the photocurrent nondestructive mode.
Description
Technical Field
The invention relates to the field of semiconductor devices, in particular to a preparation method of an organic ferroelectric crystal material and the organic ferroelectric crystal material.
Background
The organic molecular single crystal is the best choice of the micro-nano photoelectric device due to long-range order of molecular arrangement, defect density and small crystal boundary. However, due to the entropy effect, the position and direction of the growth of the organic crystal are random. At present, the mainstream evaporation process of organic materials has disordered arrangement of prepared organic molecules, different orientations of microcrystals in films, difficult preferential orientation, complex process equipment, high temperature, high vacuum degree, long time and high preparation cost.
And the preparation of the high-density micro-nano integrated device requires the preparation of organic molecular single crystals on the basis of the photoetching technology. Organic material molecules are combined by van der waals force, the original structure is easily damaged in a solution, photoetching is carried out after growth is impossible, and the application of an ordered integrated device is difficult to realize. At present, the method is to perform 'lift-off' photoetching and then perform selective area growth to pattern the single crystal film.
In addition to vapor deposition, there are processes that employ selective growth of organic molecules in solution to pattern single crystals. For example, a drop casting method, a dip-coating and pulling method and an ink-jet printing method can obtain crystals or even single crystals with certain orientation, but the yield is limited, the crystal growth direction cannot be controlled, the orientation of microcrystals in the film is different, the arraying and patterning area of the organic micro-nano single crystal material is small, and the uniformity and the stability of the device cannot be ensured for the organic photoelectric array device.
The ferroelectric random access memory FRAM integrates a ferroelectric capacitor on the prior CMOS circuit, and realizes the writing and reading of data by utilizing the polarization reversal of a ferroelectric film. Such a read is destructive and requires a re-write of data after the read. FRAM is accompanied by a large number of operations of erasing and rewriting during information reading, and the operating state of such Destructive Reading (DRO) is a source of fatigue failure of such ferroelectric memories. The other type of ferroelectric memory is a ferroelectric field effect transistor FFET, which uses a ferroelectric film to replace a gate dielectric layer in a conventional field effect transistor, and only needs to apply a reading pulse between a source and a drain when reading information, and the stored information can be read according to the magnitude of the source and drain currents without reversing the polarization state of a grid, so that the reading of the stored information is non-destructive and does not need refreshing. However, the ferroelectric-like memory does not utilize device integration, and it is difficult to realize high-density storage. And meanwhile, when information is read, pulses need to be applied, so that the power consumption of the device is increased.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of an organic ferroelectric crystal material and the organic ferroelectric crystal material, which can obtain organic molecular single crystals and micro-nano storage array devices with single orientation, high quality and uniform crystallization.
In order to solve the above problems, the present invention provides a method for preparing an organic ferroelectric crystal material, comprising the steps of: providing a substrate; forming a strip-shaped groove on the surface of the substrate; dropping the solution of the organic ferroelectric crystal material into the groove; and scraping the solution along the direction of the groove by adopting a scraper, and directionally growing the solution by utilizing the shearing force of the scraper on the solution to obtain the organic ferroelectric crystal single crystal array with the same orientation.
Optionally, an annealing step is included after the blade coating to improve crystallinity.
Optionally, in the step of forming a stripe-shaped trench on the substrate surface, a trench is further formed on the substrate surface by using a patterned photoresist.
Optionally, the organic ferroelectric crystal material is HDA-BiI5, and is configured as an organic solution with a concentration of 1 wt% to 10 wt%.
Optionally, the substrate is selected from any one of a silicon wafer, a silicon dioxide wafer, PET, PI, and quartz.
Optionally, the substrate is a substrate with a strip-shaped metal electrode, and the material of the metal electrode is selected from any one of indium tin oxide, chromium, and gold.
Optionally, the scraping is performed by controlling a horizontal scraper by a stepping motor, the scraper moves horizontally at a constant speed and a constant angle, the angle range between the scraper and the horizontal line is 5-50 degrees, the speed range between the scraper and the horizontal line is 15-45 μm, and the distance range between the scraper and the substrate is 20-200 μm.
Optionally, the substrate is heated to 40-80 ℃ before blade coating, and the temperature is kept constant during blade coating.
In order to solve the above problems, the present invention provides an organic ferroelectric crystal material comprising: a substrate; a strip-shaped groove on the surface of the substrate; an array of organic ferroelectric crystal single crystals having the same orientation in the trench.
Optionally, the organic ferroelectric crystal material is HDA-BiI 5.
The technical scheme provides an organic molecular single crystal film prepared by a blade coating method and an organic ferroelectric array storage device read in a photocurrent nondestructive mode, combines the traditional photoetching patterning technology with a blade coating process, successfully prepares an organic molecular single crystal and a micro-nano storage array device which are single in orientation, high in quality and uniform in crystallization, and promotes the application of the organic ferroelectric array storage device read in the photocurrent nondestructive mode.
Drawings
FIG. 1 is a schematic diagram illustrating the steps of one embodiment of the present invention.
Fig. 2A to 2D are schematic diagrams illustrating steps according to an embodiment of the present invention.
Detailed Description
The following will explain the preparation method of the organic ferroelectric crystal material and the specific implementation of the organic ferroelectric crystal material in detail with reference to the accompanying drawings.
The following description of the present invention is provided in connection with the accompanying drawings. FIG. 1 is a schematic diagram illustrating the steps of the present embodiment, including: step S10, providing a substrate; step S11, forming a strip-shaped groove on the surface of the substrate; step S12 of dropping a solution of the organic ferroelectric crystal material into the groove; and step S13, adopting a scraper to scrape the solution along the direction of the groove, and utilizing the shearing force of the scraper to the solution to ensure that the solution grows directionally to obtain the organic ferroelectric crystal single crystal array with the same orientation.
Referring to step S10, shown in fig. 2A, the substrate 20 is provided. The substrate 20 is selected from any one of a silicon wafer, a silicon dioxide wafer, PET, PI, and quartz. In this embodiment, the substrate is selected from a substrate on which the stripe-shaped metal electrodes 21 are grown in advance, and the material of the metal electrodes 21 is selected from any one of indium tin oxide, chromium, and gold. For example, a double layer metal of Cr/Au, with Cr as the bonding metal and thicknesses of 5nm Cr and 50nm Au, respectively, may be used.
Referring to step S12, as shown in fig. 2B, a stripe-shaped trench 22 is formed on the surface of the substrate 20. And forming a groove on the surface of the substrate by using the patterned photoresist. Further, the substrate 20 with the strip-shaped metal electrode 21 is placed on a spin coater chuck, photoresist is spin-coated, and photoresist stripes with the width of 2 μm and the distance are obtained through pre-baking, exposure, post-baking, development and hardening, wherein the overall size is 3 x 3 mm.
As shown in fig. 2C, referring to step S12, the solution 23 of the organic ferroelectric crystal material is dropped into the trench 22. Preferably, 2-10 μ L of the implant is formed in each trench. In this embodiment, the solution 23 is a solvent selected to be suitable for dissolving the organic molecules in the solvent. The organic ferroelectric crystal material is HDA-BiI5, has the property of visible light wave band absorption, and is prepared into 1-10 wt% concentration organic solution.
Referring to step S13, as shown in fig. 2D, the solution 23 is scraped along the trench 22 by the scraper 24, and the solution 23 is directionally grown by the shearing force of the scraper 24 on the solution 23, so as to obtain the same-orientation organic ferroelectric crystal single crystal array. In one embodiment, the substrate may be heated to 40-80 ℃ prior to draw down, maintaining the temperature constant during draw down. Preferably, the blade coating is performed by controlling a horizontal blade with a stepping motor (not shown), and the blade moves horizontally at the same speed and angle. The angle between the scraper and the horizontal line is controlled to be 5-50 degrees, the speed of the scraper is 15-45 mu m, and the distance between the scraper and the substrate is 20-200 mu m. An annealing step may also be performed after the draw down to increase crystallinity
The process adopts a blade coating method to prepare a single crystal array of HDA-BiI5 and a non-destructive memory device for photocurrent reading, prepares organic ferroelectric molecular solution, patterns a substrate with a bottom electrode to obtain an array pattern, and grows the single crystal array and the micro-nano array memory device in a certain direction at a specified position by blade coating and heating the substrate. The solution grows directionally by using the viscosity and the tension of the solution and the shearing force of a scraper to the solution, and the solution grows on the patterned graph controllably, so that the organic molecular single crystal array with the same orientation can be obtained, and the prepared organic ferroelectric memory has the advantages of photocurrent reading, nondestructive information reading, no need of applying extra voltage pulse and low power consumption.
One example is given below.
(1) Preparing organic ferroelectric molecular solution.
The selected area growth of the knife coating method is firstly to prepare the required solution, wherein the solute is organic molecule ferroelectric material HDA-BiI 5. The solvent is DMF which has higher viscosity and slower volatilization, so that on one hand, the viscosity is higher, the scraper can more easily drive the solution to move, and the solution is more easily selected between the photoresists; on the other hand, the coating rate is slow, and the solvent is volatilized too fast, so that the solution is crystallized after the coating is not finished, and the coating cannot realize the controllable growth of the solution.
(2) Patterned photoresist stripes are prepared.
The conventional photolithography process using SU 82000.5 uses SU8 photoresist instead of a positive resist such as 1805 because SU8 is more compatible with DMF solvent. Firstly, a layer of SU8 photoresist is coated on a substrate, and the substrate is baked for 2min at 100 ℃ in a hot plate after spin coating. After the substrate is cooled, the exposure reaction is carried out, and the substrate is pre-baked for 2min for the second time on a hot plate at the temperature of 100 ℃. After development and hardening, a stripe array pattern having a width of 2 μm and a pitch was obtained. And (4) treating for 15min under UV Ozone to remove residual photoresist, so as to ensure that the grown ferroelectric single crystal is in better contact with the substrate.
(3) And (3) growing an organic molecule ferroelectric film in a selected area by a blade coating method.
Taking organic molecule ferroelectric HDA-BiI5 as an example, the substrate is placed on a heating table at 50 ℃, the included angle between a scraper and the horizontal direction is adjusted to be 30 ℃, the distance between the scraper and the substrate is kept stable at 100 mu m, 5 mu L of prepared 3OQ solution is dripped into the gap by a liquid transfer gun, and a horizontal moving platform is started to ensure that the scraper scrapes along the horizontal direction at the speed of 30 mu m. After the end of the blade coating, the substrate was moved to a 120 ℃ heating stage and annealed for 2h to increase crystallinity.
(4) And preparing a ferroelectric array memory device.
Covering a mask plate on the surface of the prepared HDA-BiI5 single crystal array, putting the mask plate into a thermal evaporation coating machine, and depositing an upper electrode metal array with the width of 100 multiplied by 100 mu m and the distance to obtain the capacitive organic ferroelectric array memory device.
By the method, a 100% single crystal thin film array with millimeter size can be prepared, and the prepared HDA-BiI5 single crystal array is proved to have single crystal property and orientation through a polarization microscope (CPOM) and a TEM, so that the ferroelectric property is optimized. The prepared organic ferroelectric memory array device can read the memory information under the photocurrent switch, realizes the non-destructive reading of the ferroelectric without applying pulse voltage, and reduces the power consumption of the device.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of an organic ferroelectric crystal material is characterized by comprising the following steps:
providing a substrate;
forming a strip-shaped groove on the surface of the substrate;
dropping the solution of the organic ferroelectric crystal material into the groove;
and scraping the solution along the direction of the groove by adopting a scraper, and directionally growing the solution by utilizing the shearing force of the scraper on the solution to obtain the organic ferroelectric crystal single crystal array with the same orientation.
2. The method of claim 1, further comprising an annealing step after blade coating to increase crystallinity.
3. The method of claim 1, wherein the step of forming the stripe-shaped trench on the substrate surface further comprises forming a trench on the substrate surface using a patterned photoresist.
4. The method of claim 1, wherein the organic ferroelectric crystal material is HDA-BiI5 and is formulated as an organic solution having a concentration of 1 wt% to 10 wt%.
5. The method of claim 1, wherein the substrate is selected from any one of a silicon wafer, a silicon dioxide wafer, PET, PI, and quartz.
6. The method according to claim 1, wherein the substrate is selected from a substrate with a strip-shaped metal electrode, and the material of the metal electrode is selected from any one of indium tin oxide, chromium, and gold.
7. The method of claim 1, wherein the coating comprises controlling a doctor blade by a stepper motor, the doctor blade moving horizontally at a constant speed and constant angle, the doctor blade having an angle in the range of 5 ° to 50 ° with respect to the horizontal, the doctor blade having a speed in the range of 15 μm to 45 μm, and the doctor blade having a distance from the substrate in the range of 20 μm to 200 μm.
8. The method of claim 1, wherein the substrate is heated to 40-80 ℃ prior to the doctor blade, and the temperature is kept constant during the doctor blade.
9. An organic ferroelectric crystal material, comprising:
a substrate;
a strip-shaped groove on the surface of the substrate;
an array of organic ferroelectric crystal single crystals having the same orientation in the trench.
10. The material of claim 9, wherein the organic ferroelectric crystal material is HDA-BiI 5.
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| CN202110441375.1A CN113151902A (en) | 2021-04-23 | 2021-04-23 | Method for producing organic ferroelectric crystal material and organic ferroelectric crystal material |
| PCT/CN2021/111178 WO2022222307A1 (en) | 2021-04-23 | 2021-08-06 | Preparation method for organic ferroelectric crystal material, and organic ferroelectric crystal material |
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| CN202110441375.1A CN113151902A (en) | 2021-04-23 | 2021-04-23 | Method for producing organic ferroelectric crystal material and organic ferroelectric crystal material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113644224A (en) * | 2021-08-09 | 2021-11-12 | 光华临港工程应用技术研发(上海)有限公司 | Preparation method of organic light-emitting diode and organic light-emitting diode |
| WO2022222307A1 (en) * | 2021-04-23 | 2022-10-27 | 光华临港工程应用技术研发(上海)有限公司 | Preparation method for organic ferroelectric crystal material, and organic ferroelectric crystal material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2016088790A (en) * | 2014-10-31 | 2016-05-23 | 国立研究開発法人産業技術総合研究所 | Method for manufacturing organic ferroelectric crystal thin film |
| CN109841737A (en) * | 2019-02-27 | 2019-06-04 | 苏州大学 | A kind of preparation method of organic semiconductor array crystals |
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| JP6926475B2 (en) * | 2015-11-25 | 2021-08-25 | 東レ株式会社 | Ferroelectric memory elements, their manufacturing methods, memory cells using them, and wireless communication devices using them. |
| CN111564558B (en) * | 2020-05-14 | 2022-07-29 | 苏州大学 | Preparation method of organic crystalline film and organic field effect transistor |
| CN113151902A (en) * | 2021-04-23 | 2021-07-23 | 光华临港工程应用技术研发(上海)有限公司 | Method for producing organic ferroelectric crystal material and organic ferroelectric crystal material |
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| JP2016088790A (en) * | 2014-10-31 | 2016-05-23 | 国立研究開発法人産業技術総合研究所 | Method for manufacturing organic ferroelectric crystal thin film |
| CN109841737A (en) * | 2019-02-27 | 2019-06-04 | 苏州大学 | A kind of preparation method of organic semiconductor array crystals |
Non-Patent Citations (1)
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| HAN-YUE ZHANG等人: "The Narrowest Band Gap Ever Observed in Molecular Ferroelectrics: Hexane-1,6-diammonium Pentaiodobismuth(III)", 《ANGEWANDTE CHEMIE》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022222307A1 (en) * | 2021-04-23 | 2022-10-27 | 光华临港工程应用技术研发(上海)有限公司 | Preparation method for organic ferroelectric crystal material, and organic ferroelectric crystal material |
| CN113644224A (en) * | 2021-08-09 | 2021-11-12 | 光华临港工程应用技术研发(上海)有限公司 | Preparation method of organic light-emitting diode and organic light-emitting diode |
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