CN105226085A - A kind of MOF thin-film material and preparation and application thereof with high dielectric property - Google Patents
A kind of MOF thin-film material and preparation and application thereof with high dielectric property Download PDFInfo
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- CN105226085A CN105226085A CN201510530875.7A CN201510530875A CN105226085A CN 105226085 A CN105226085 A CN 105226085A CN 201510530875 A CN201510530875 A CN 201510530875A CN 105226085 A CN105226085 A CN 105226085A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000463 material Substances 0.000 title abstract description 34
- 239000010409 thin film Substances 0.000 title abstract description 15
- 239000012621 metal-organic framework Substances 0.000 claims abstract description 31
- 239000011701 zinc Substances 0.000 claims abstract description 22
- 150000001875 compounds Chemical class 0.000 claims abstract description 21
- 229910052751 metal Inorganic materials 0.000 claims abstract description 10
- 239000002184 metal Substances 0.000 claims abstract description 10
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000012360 testing method Methods 0.000 claims description 3
- 239000007983 Tris buffer Substances 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000013110 organic ligand Substances 0.000 claims 1
- 239000010408 film Substances 0.000 abstract description 27
- 238000000034 method Methods 0.000 abstract description 7
- 239000003989 dielectric material Substances 0.000 abstract description 5
- 238000013461 design Methods 0.000 abstract description 4
- 239000012923 MOF film Substances 0.000 abstract description 2
- 238000009413 insulation Methods 0.000 abstract description 2
- 238000001338 self-assembly Methods 0.000 abstract 1
- 239000000758 substrate Substances 0.000 description 5
- 238000011156 evaluation Methods 0.000 description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- -1 polytetrafluoroethylene Polymers 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 0 CC(C(C(C)[C@](C)C(C1(C)C)OC(CC2)CCC2C(O)=O)OC2CCC(*)CC2)C1OC(C1)CC1C(O)=O Chemical compound CC(C(C(C)[C@](C)C(C1(C)C)OC(CC2)CCC2C(O)=O)OC2CCC(*)CC2)C1OC(C1)CC1C(O)=O 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 1
- 229910052809 inorganic oxide Inorganic materials 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000010583 slow cooling Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/40—Electrodes ; Multistep manufacturing processes therefor
- H01L29/43—Electrodes ; Multistep manufacturing processes therefor characterised by the materials of which they are formed
- H01L29/49—Metal-insulator-semiconductor electrodes, e.g. gates of MOSFET
- H01L29/51—Insulating materials associated therewith
- H01L29/518—Insulating materials associated therewith the insulating material containing nitrogen, e.g. nitride, oxynitride, nitrogen-doped material
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F3/00—Compounds containing elements of Groups 2 or 12 of the Periodic Table
- C07F3/06—Zinc compounds
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- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Ceramic Engineering (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Insulating Bodies (AREA)
- Inorganic Insulating Materials (AREA)
Abstract
The present invention relates to preparation and the purposes of metal-organic framework compound film.This thin-film material adopts electrochemical-assembly method, with metal-organic framework the compound { [H with novel structure of autonomous Design
2n (CH
3)
2] [Zn (TBTC)] 2DMFEtOH is main body, at metal zinc metal sheet self assembly MOF film on the surface.This thin-film material has shown good dielectric property, and has good mechanical performance and insulation property and higher puncture voltage after being assembled into film, in electronic device material especially grid dielectric material, have potential application foreground.
Description
Technical field
The invention belongs to the design field of Novel electronic devices material, be specifically related to metal-organic framework compound-material and be assembled into Application and Development in field of electronic devices after thin-film material, particularly relate to the exploitation aspect of the potential substitution material of grid dielectric material.
Background technology
In the past few decades, high dielectric constant material, also known as " high κ " material, due to they potential application in thin-film transistor and electron transfer pipe, has attracted the interest of numerous researchers.So-called " high κ " material refers to the material having dielectric constant and be greater than the features such as dioxide dielectric constant (3.9), Low dark curient electric current, high breakdown field strength.Traditional silicon-based electronic elements has almost ruled all grid dielectric materials.But in the application of thin-film transistor, the use of silica-base material also exists some defects, such as dielectric constant is low, not easily process etc. in the course of processing.Therefore the dielectric material of development of new is an instant problem.First the thickness of grid be can increase, and tunnel(l)ing current or leakage current do not increased.Oxide (the HfO of the conventional inorganic hafnium of researchers
2) and the oxide (ZrO of zirconium
2) as high κ material, but pure inorganic oxide is frangible and can not be well compatible with substrate, needs the comparatively exacting terms such as higher treatment temperature and ultra high vacuum technique.Subsequently, flexible organic polymer film presents with substrate well compatible, but they self often present lower dielectric constant and lower thermal stability.Recently, scientist combine the inorganic component material with high κ performance and with flexible, that there is with substrate the organic molecule of favorable compatibility performance formation inorganic-organic hybrid grid material.But assembling and compatibility are also prepare the very large challenge of of film between organic component and inorganic component.Weak compatibility result in the generation of the defect of film, thus produces certain flaw at aspect of performance.In addition, adjustment dielectric property are carried out in the aspect such as the unlikely preferred orientation by crystalline state of novel amorphous compound grid material or structure assembling.
Metal-organic framework compound (metal-organicframeworks, MOFs) is by organic component and metal ion (inorganic component) compounds by certain coordination mode coordination.For this reason, metal-organic framework compound has had the denominator of organic component and inorganic component concurrently, nor there is the problem of weak compatibility between inorganic component and organic component.But although there is the report of the dielectric property of many metal-organic framework compounds at present, great majority are utilized with the form of powder, and most be ferroelectric properties.In actual application, assembling MOFs material is by MOFs materials application condition required in electronic component to the surface of substrate and MOFs material and the good compatibility of substrate.At present, about the research of MOFs thin-film material of design dielectric constant and mechanical performance, there is not been reported.Assemble mutual interlude MOFs by electrochemical process to strengthen the correlative study of the dielectric property of MOFs film as the film of high preferred orientation also there is not been reported at present.
Summary of the invention
The object of the invention is to focus on the MOFs that design has novel structure, and the surface being assembled into solid matrix forms functional MOFs film, and inquire into it in the potential application in grid electrolyte.
The present invention proposes based on three tooth Carboxylic acid ligand 1,3,5-tris [4-(carboxyphenyl) oxamethyl]-2,4,6-trimethylbenzene (H
3tBTC) the { [H with novel structure
2n (CH
3)
2] [Zn (TBTC)] preparation method of 2DMFEtOH, the structural formula of part is as follows:
The surface that the present invention adopts electrochemical-assembly method MOFs to be assembled into metal zinc metal sheet forms MOFs film.
MOFs film prepared by the present invention has potential application in dielectric devices, especially gate dielectric devices field.
{ [H prepared by the present invention
2n (CH
3)
2] [Zn (TBTC)] 2DMFEtOH film synthesizes first.This material utilizes electrochemical-assembly method, by the compound { [H of interlude
2n (CH
3)
2] [Zn (TBTC)] the 2DMFEtOH surface that is assembled into metal zinc metal sheet forms MOFs film.The dielectric constant that this film shows is three times of its body phase material, and all higher than the dielectric constant of most of MOFs material.This shows, this film has good dielectric property.In addition, film prepared by the present invention has good mechanical performance, lower leakage current and higher puncture voltage.This thin-film material showing prepared by the present invention is expected to and is applied to field of electronic devices, the substitution material aspect of grid dielectric material time especially.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of prepared film
Fig. 2 is compound { [H
2n (CH
3)
2] [Zn (TBTC)] the measurement curve of 2DMFEtOH and film
Embodiment
Embodiment 1: compound { [H
2n (CH
3)
2] [Zn (TBTC)] preparation of 2DMFEtOH
Mol ratio is the Zn (NO of 1 ~ 3:0.5 ~ 2
3)
26H
2o and H
3tBTC is dissolved in the DMF/EtOH/H that volume ratio is 2.5 ~ 6:0.5 ~ 1.5:0.5 ~ 1.5
2stir in the mixed liquor of O and heat.Then solution being transferred to volume is in the airtight high pressure polytetrafluoroethylene reactor of liquor capacity twice.Polytetrafluoroethylene autoclave is placed in stainless steel autoclave, and then entirety is placed in 70 DEG C ~ 140 DEG C baking oven constant temperature 60 ~ 84h, and by polytetrafluoroethylene stainless steel cauldron Slow cooling, (speed is 0.02 ~ 0.06 DEG C of min subsequently
-1), finally obtain colourless crystalline compound.
Embodiment 2:{ [H
2n (CH
3)
2] [Zn (TBTC)] preparation of 2DMFEtOH film
Mol ratio is the Zn (NO of 1 ~ 3:0.5 ~ 2:0.5 ~ 3
3)
26H
2o,H
3tBTC and ammonium fluoride are dissolved in the DMF/EtOH/H that volume ratio is 2.5 ~ 6:0.5 ~ 1.5:0.5 ~ 1.5
2in O mixed solution, under the environment of heating, stir 10 ~ 30min.Subsequently, solution is led to nitrogen 1 ~ 2 hour, to remove the oxygen in solution.After this, by wide for the long * of the area sheared be that 1 ~ 5cm*1 ~ 2cm metallic zinc plate electrode inserts in solution.Added the voltage of 0.5V ~ 3V to electrode two ends by electrochemical operation, reaction 30s ~ 15min, obtains the film of 5 μm ~ 25 μm of thickness.A straight-through nitrogen is needed in the process of electrolysis and reaction.After film preparation is good, clean film respectively with DMF and water, to remove excessive part and unstable MOF particulate.
Embodiment 3:{ [H
2n (CH
3)
2] [Zn (TBTC)] sign of 2DMFEtOH thin-film dielectric performance
The dielectric constant of film obtains on TH2828PrecisionLCRMeter; The preparation of electrode is the two ends by silver slurry being coated in MOF film, then by copper wire contact silver slurry; Characterize the correction yardstick error range of electric capacity to be less than ± 5%.Electrochemical growth film uses Epsilon electrochemical workstation, uses two-electrode system.
By evaluating, the dielectric constant of the body phase of the compound synthesized by this patent is 5 ~ 6.5, but after this compound is prepared into film by the surface that electrochemical method deposits to metal zinc metal sheet, the dielectric constant of thin-film material is 15 ~ 20, is 3 ~ 3.1 times of body phase material.In addition, by investigation, the dielectric constant of the non-ferroelectric MOF material that the thin-film material that this patent is invented arrives than similar report is all high.This evaluation shows that the thin-film material of invention has good dielectric property.
Embodiment 4:{ [H
2n (CH
3)
2] [Zn (TBTC)] 2DMFEtOH film mechanical performance and electric leakage performance evaluation
The leakage current of film and puncture voltage obtain on KEITHLETY-2400 type instrument.Nano-indenter test obtains on MTSXP type instrument.Poisson's ratio be set to 0.3.By evaluating, the thin-film material of invention has good mechanical performance, and modulus of elasticity is 32.00 (± 1.71) GPa, and hardness is 0.33 (± 0.02) GPa.By electric leakage and the evaluation of puncture voltage, the thin-film material that this patent is invented has good insulation property and higher puncture voltage, at 1KVcm
-1electric field under leakage current be 10
-7acm
-1, the puncture voltage of film can reach 10KVcm
-1.
Claims (7)
1. a metal-organic framework compound film, is characterized in that, this film is by metal-organic framework compound { [H
2n (CH
3)
2] [Zn (TBTC)] 2DMFEtOH formation.
2. metal-organic framework compound film as claimed in claim 1, is characterized in that, the compound { [H described in it
2n (CH
3)
2] [Zn (TBTC)] 2DMFEtOH is by organic ligand 1,3,5-tris [4-(carboxyphenyl) oxamethyl]-2,4,6-trimethylbenzene, H
3tBTC and metallic zinc ion coordination are formed.
3. metal-organic framework compound film as claimed in claim 1 or 2, it is characterized in that, the thickness range of described film is 5 μm ~ 25 μm.
4. a preparation method for metal-organic framework compound film according to claim 1, is characterized in that: adopt electrochemical production, comprise the steps:
(1) Zn (NO
3)
26H
2o, H
3tBTC and ammonium fluoride are dissolved in the DMF/EtOH/H of certain volume ratio by certain mol ratio
2in O mixed solution, under the environment of heating, stir 10 ~ 30min;
(2) nitrogen is led to 1 ~ 2 hour in solution;
(3) metallic zinc plate electrode to be inserted in mixed solution and to add certain voltage at electrode two ends, the reaction regular hour, obtaining the metal-organic framework compound film of the different-thickness of metal zinc metal sheet load.
5. preparation method as claimed in claim 4, is characterized in that, Zn (NO in described step (1)
3)
26H
2o, H
3the mol ratio of TBTC and ammonium fluoride is: 1 ~ 3:0.5 ~ 2:0.5 ~ 3, DMF/EtOH/H
2the volume ratio of O is 2.5 ~ 6:0.5 ~ 1.5:0.5 ~ 1.5.
6. preparation method as claimed in claim 4, is characterized in that, the voltage in described step (3) added by electrode two ends is 0.5V ~ 3V, and the long * of electrode area is wide is 1 ~ 5cm*1 ~ 2cm, and the time of reaction is 30s ~ 15min.
7. the application of metal-organic framework compound film according to claim 1 in electronic device, is characterized in that, the described application being applied as gate dielectric device, the test of modulus of elasticity and hardness test and electric leakage and puncture voltage.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510530875.7A CN105226085A (en) | 2015-08-26 | 2015-08-26 | A kind of MOF thin-film material and preparation and application thereof with high dielectric property |
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|---|---|---|---|
| CN201510530875.7A CN105226085A (en) | 2015-08-26 | 2015-08-26 | A kind of MOF thin-film material and preparation and application thereof with high dielectric property |
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|---|---|
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ID=54994928
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|---|---|---|---|
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105801606A (en) * | 2016-04-13 | 2016-07-27 | 江苏科技大学 | Metal-organic coordination compound with reversible dielectric property, preparation method and application |
| CN107398187A (en) * | 2017-07-26 | 2017-11-28 | 华南理工大学 | It is a kind of to utilize the supper-fast method for preparing metal organic framework film of electric field poling |
| CN107469643A (en) * | 2017-07-26 | 2017-12-15 | 华南理工大学 | A kind of high-performance metal organic framework film and its application in propylene and propane efficiently separate |
| CN107602474A (en) * | 2017-07-26 | 2018-01-19 | 华南理工大学 | A kind of method that template prepares the metal organic framework film with specific orientation |
| CN108130574A (en) * | 2018-01-03 | 2018-06-08 | 苏州大学 | Method for depositing metal organic framework material by oxygen-assisted cathode |
| CN109467072A (en) * | 2017-09-07 | 2019-03-15 | 中国科学院福建物质结构研究所 | Carbon quantum dot, the preparation method of carbon quantum dot and MOFs laminated film and its product and purposes |
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| US20110144367A1 (en) * | 2009-12-10 | 2011-06-16 | Northwestern University | Activation of porous MOF materials |
| CN102516274A (en) * | 2011-04-25 | 2012-06-27 | 中国科学院福建物质结构研究所 | Cadmium metal organic frame compound with catalytic performance and preparation method and use thereof |
-
2015
- 2015-08-26 CN CN201510530875.7A patent/CN105226085A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20110144367A1 (en) * | 2009-12-10 | 2011-06-16 | Northwestern University | Activation of porous MOF materials |
| CN102516274A (en) * | 2011-04-25 | 2012-06-27 | 中国科学院福建物质结构研究所 | Cadmium metal organic frame compound with catalytic performance and preparation method and use thereof |
Non-Patent Citations (1)
| Title |
|---|
| WEI-JIN LI ET AL.: "Electrochemical synthesis of metal-organic framework thin film", 《中国化学会第九届全国无机化学学术会议》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105801606A (en) * | 2016-04-13 | 2016-07-27 | 江苏科技大学 | Metal-organic coordination compound with reversible dielectric property, preparation method and application |
| CN105801606B (en) * | 2016-04-13 | 2017-05-10 | 江苏科技大学 | Metal-organic coordination compound with reversible dielectric property, preparation method and application |
| CN107398187A (en) * | 2017-07-26 | 2017-11-28 | 华南理工大学 | It is a kind of to utilize the supper-fast method for preparing metal organic framework film of electric field poling |
| CN107469643A (en) * | 2017-07-26 | 2017-12-15 | 华南理工大学 | A kind of high-performance metal organic framework film and its application in propylene and propane efficiently separate |
| CN107602474A (en) * | 2017-07-26 | 2018-01-19 | 华南理工大学 | A kind of method that template prepares the metal organic framework film with specific orientation |
| CN107469643B (en) * | 2017-07-26 | 2021-03-30 | 华南理工大学 | High-performance metal organic framework membrane and application thereof in efficient separation of propylene and propane |
| CN109467072A (en) * | 2017-09-07 | 2019-03-15 | 中国科学院福建物质结构研究所 | Carbon quantum dot, the preparation method of carbon quantum dot and MOFs laminated film and its product and purposes |
| CN108130574A (en) * | 2018-01-03 | 2018-06-08 | 苏州大学 | Method for depositing metal organic framework material by oxygen-assisted cathode |
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