CN109003887A - A kind of low temperature preparation ZrO2The method of insulating layer of thin-film and laminated construction - Google Patents
A kind of low temperature preparation ZrO2The method of insulating layer of thin-film and laminated construction Download PDFInfo
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- CN109003887A CN109003887A CN201810728835.7A CN201810728835A CN109003887A CN 109003887 A CN109003887 A CN 109003887A CN 201810728835 A CN201810728835 A CN 201810728835A CN 109003887 A CN109003887 A CN 109003887A
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- 239000010409 thin film Substances 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000010276 construction Methods 0.000 title claims abstract description 11
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000004528 spin coating Methods 0.000 claims abstract description 22
- 239000002243 precursor Substances 0.000 claims abstract description 16
- 238000000137 annealing Methods 0.000 claims abstract description 15
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000758 substrate Substances 0.000 claims abstract description 12
- 239000011521 glass Substances 0.000 claims abstract description 9
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 claims abstract description 7
- 230000032683 aging Effects 0.000 claims abstract description 7
- 229940031098 ethanolamine Drugs 0.000 claims abstract description 7
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 2
- ZZVUWRFHKOJYTH-UHFFFAOYSA-N diphenhydramine Chemical compound C=1C=CC=CC=1C(OCCN(C)C)C1=CC=CC=C1 ZZVUWRFHKOJYTH-UHFFFAOYSA-N 0.000 claims 1
- 239000003381 stabilizer Substances 0.000 claims 1
- 239000010408 film Substances 0.000 abstract description 9
- BNUDRLITYNMTPD-UHFFFAOYSA-N acetic acid;zirconium Chemical compound [Zr].CC(O)=O BNUDRLITYNMTPD-UHFFFAOYSA-N 0.000 abstract description 7
- 239000012535 impurity Substances 0.000 abstract description 4
- 238000007791 dehumidification Methods 0.000 abstract description 3
- 239000012528 membrane Substances 0.000 abstract description 3
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 239000004033 plastic Substances 0.000 abstract description 2
- 229920003023 plastic Polymers 0.000 abstract description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000052 vinegar Substances 0.000 description 1
- 235000021419 vinegar Nutrition 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
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
- H01L21/02112—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer
- H01L21/02172—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing at least one metal element, e.g. metal oxides, metal nitrides, metal oxynitrides or metal carbides
- H01L21/02175—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing at least one metal element, e.g. metal oxides, metal nitrides, metal oxynitrides or metal carbides characterised by the metal
- H01L21/02189—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing at least one metal element, e.g. metal oxides, metal nitrides, metal oxynitrides or metal carbides characterised by the metal the material containing zirconium, e.g. ZrO2
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
- H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
- H01L21/02282—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process liquid deposition, e.g. spin-coating, sol-gel techniques, spray coating
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02296—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer
- H01L21/02318—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer post-treatment
-
- 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
- H01L29/66—Types of semiconductor device ; Multistep manufacturing processes therefor
- H01L29/66007—Multistep manufacturing processes
- H01L29/66969—Multistep manufacturing processes of devices having semiconductor bodies not comprising group 14 or group 13/15 materials
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- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Ceramic Engineering (AREA)
- Formation Of Insulating Films (AREA)
Abstract
The present invention relates to a kind of low temperature preparation ZrO2The preparation step of insulating layer of thin-film and laminated construction, the film is as follows: acetic acid zirconium being dissolved in glycol monoethyl ether, ethanol amine is added, stands aging after stirring, obtains the precursor solution that acetic acid zirconium concentration is 0.3~0.6mol/L；The volume of the ethanol amine accounts for the 1/6 of the precursor solution total volume；Then the precursor solution described in spin coating on ito glass substrate, and the 1~2h that anneals at 200 DEG C, obtain ZrO2Insulating layer of thin-film.Again in gained ZrO2By magnetron sputtering circle Al electrode on insulating layer of thin-film, the laminated construction can be obtained.Organic impurities of the present invention in the based Dehumidification Membranes that go down compared with low temperature thermal oxidation, be conducive to insulating layer of thin-film to combine with flexible substrates such as plastics, make it possible low temperature preparation high-performance flexible electronic device, treatment with ultraviolet light needed for conventional cryogenic technique is avoided simultaneously, reduces the complexity of annealing process.
Description
Technical field
The invention belongs to thin-film transistor technologies fields, and in particular to a kind of low temperature preparation ZrO2Insulating layer of thin-film and lamination
The method of structure.
Background technique
Thin film transistor (TFT) (Thin Film Transistor, abbreviation TFT), as a kind of widely used semiconductor device
Part, the arrangement variation and driving OLED pixel for being mainly used for liquid crystal in driving display shine.Insulating layer energy in TFT
The effects of playing storage capacitance and preventing signal cross-talk, influences the transfer performance, stability and service life of TFT device.ZrO2There is height
Relative dielectric constant (~27), wider forbidden band (7.8eV), be a kind of common dielectric layer material.Using preparation ZrO2Absolutely
During edge film, the impurity such as solvent for often annealing temperature of higher (> 350 DEG C) being needed to make a return journey in based Dehumidification Membranes, excessively high is moved back
Fiery temperature affects ZrO2The combination of insulation film and flexible substrate (heatproof~200 DEG C) is unfavorable for realizing Flexible Displays.In order to
This problem is solved, the method for mainstream is at present, by the wet film of ultraviolet light spin coating, thus the annealing temperature needed for reducing
Degree.But this mode needs complicated annealing process and annealing device, is unfavorable for large-area treatment.
Summary of the invention
In place of the above shortcoming and defect of the existing technology, the primary purpose of the present invention is that providing a kind of low temperature
Prepare ZrO2The method of insulating layer of thin-film.
Another object of the present invention is to provide a kind of to prepare ZrO2The method of insulating layer of thin-film laminated construction.
The purpose of the present invention is achieved through the following technical solutions:
A kind of low temperature preparation ZrO2The method of insulating layer of thin-film, includes the following steps:
(1) by Zr (CH3COO)4(acetic acid zirconium) is dissolved in glycol monoethyl ether (2-MOE), and ethanol amine is added as stabilization
Agent stands aging after stirring, obtains precursor solution；Zr (CH in the precursor solution3COO)4Concentration be 0.3~
0.6mol/L；The volume of the ethanol amine accounts for the 1/6 of the precursor solution total volume；
(2) spin-coating step (1) the resulting precursor solution on ito glass substrate, then 200 DEG C at a temperature of anneal
1~2h is handled, ZrO is obtained2Insulating layer of thin-film.
Preferably, step (1) mixing speed is 500rpm, and ageing time is 24 hours.
Preferably, the process conditions of spin coating described in step (2) are as follows: 4000~6000rpm of revolving speed, spin coating number 3~5
It is secondary, each 30~40s of spin-coating time, 200 DEG C of annealing temperature between each spin coating, 3~5min of time.
It is a kind of to prepare ZrO2The method of insulating layer of thin-film laminated construction, comprising the following steps: in gained ZrO2Insulating layer of thin-film
It is upper to pass through magnetron sputtering circle Al electrode, obtain MIM (ITO/ZrO2/ Al) laminated construction.
The principle of the present invention are as follows: by Zr (CH3COO)4(acetic acid zirconium) is dissolved in available containing acetate in glycol monoethyl ether
Presoma, wet film annealing during, as removal acetate needed for temperature it is lower, so as at a lower temperature
Impurity is removed, realizes ZrO2The low temperature preparation of film.
Compared with prior art, the invention has the following advantages and beneficial effects:
Removal temperature needed for acetate is lower in annealing process, using acetic acid zirconium as zirconates, glycol monoethyl ether (boiling point
It is 124.5 DEG C) it is solvent, solwution method preparation ZrO can be reduced2Temperature needed for film.The present invention passes through Zr (CH3COO)4(vinegar
Sour zirconium) obtain the ZrO containing acetate2The precursor solution of insulating layer, can having in the based Dehumidification Membranes that go down compared with low temperature thermal oxidation
Machine impurity is conducive to insulating layer of thin-film and combines with flexible substrates such as plastics, so that low temperature preparation high-performance flexible electronic device
It is possibly realized, while avoiding treatment with ultraviolet light needed for conventional cryogenic technique, reduce the complexity of annealing process.
Detailed description of the invention
Fig. 1 is 1 gained ZrO of embodiment2The leakage current density curve graph of insulating layer of thin-film.
Fig. 2 is 2 gained ZrO of embodiment2The leakage current density curve graph of insulating layer of thin-film.
Specific embodiment
Present invention will now be described in further detail with reference to the embodiments and the accompanying drawings, but embodiments of the present invention are unlimited
In this.
Embodiment 1
(1) presoma is prepared: by 1ml acetic acid zirconium (liquid, density 1.279g/ml, Zr content are 15%~16wt%)
It is dissolved in 2ml glycol monoethyl ether (2-MOE), adds 12ul ethanol amine, aging for 24 hours is stirred and stood at 500r/min,
Obtain the precursor solution of 0.6mol/L.
(2) prepared by substrate: depositing the ITO electrode of one layer of 150nm in glass baseplate surface, cleaning, drying obtains ito glass
Substrate.
(3) the resulting precursor solution of selected technological parameter spin-coating step (1), spin coating revolving speed are pressed in ito glass substrate
6000rpm, spin coating time 40s, spin coating number 3 times, 200 DEG C of annealing temperature between each spin coating, time 4min, then 200
DEG C annealing 1h, obtain ZrO2Insulating layer of thin-film.
(4) in the ZrO of step (3)2The round Al electrode of 100nm is plated on insulating layer of thin-film by magnetron sputtering, is prepared
MIM(ITO/ZrO2/ Al) laminated construction.
ZrO obtained by the present embodiment2Leakage current test result such as Fig. 1 of insulating layer of thin-film shows.It can be seen that with electricity is applied
The increase of pressure, ZrO2The leakage current density of film is gradually increased, but remains at lesser level, when voltage is ± 4V, leakage
Current density is 1.5 × 10-4A/cm2。
Test result shows ZrO manufactured in the present embodiment2Insulating layer of thin-film has preferable insulation performance.
Embodiment 2
(1) presoma is prepared: by 0.5ml acetic acid zirconium (liquid, density 1.279g/ml, Zr content are 15%~16%)
It is dissolved in 2.5ml glycol monoethyl ether (2-MOE), adds the ethanol amine of 6ul, stirred at 500r/min and stand aging
For 24 hours, the precursor solution of 0.3mol/L is obtained.
(2) prepared by substrate: depositing the ITO electrode of one layer of 150nm in glass baseplate surface, cleaning, drying obtains ito glass
Substrate.
(3) the resulting precursor solution of selected technological parameter spin-coating step (1), spin coating revolving speed are pressed in ito glass substrate
5000rpm, spin coating time 40s, spin coating number 5 times, 200 DEG C of annealing temperature between each spin coating, time 4min, then 200
DEG C annealing 1h, obtain ZrO2Insulating layer of thin-film.
(4) in the ZrO of step (3)2The round Al electrode of 100nm is plated on insulating layer of thin-film by magnetron sputtering, is prepared
MIM(ITO/ZrO2/ Al) laminated construction.
ZrO obtained by the present embodiment2Leakage current test result such as Fig. 2 of insulating layer of thin-film shows.It can be seen that with electricity is applied
The increase of pressure, ZrO2The leakage current density of film is gradually increased, but remains at lesser level, when voltage is ± 4V, leakage
Current density is 1.8 × 10-5A/cm2。
Test result shows ZrO manufactured in the present embodiment2Insulating layer of thin-film has preferable insulation performance.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (4)
1. a kind of low temperature preparation ZrO2The method of insulating layer of thin-film, which comprises the steps of:
(1) by Zr (CH3COO)4It is dissolved in glycol monoethyl ether (2-MOE), and ethanol amine is added as stabilizer, it is quiet after stirring
Aging is set, precursor solution is obtained；Zr (CH in the precursor solution3COO)4Concentration be 0.3~0.6mol/L；The second
The volume of hydramine accounts for the 1/6 of the precursor solution total volume；
(2) spin-coating step (1) the resulting precursor solution on ito glass substrate, then 200 DEG C at a temperature of make annealing treatment
1~2h obtains ZrO2Insulating layer of thin-film.
2. a kind of ZrO is prepared according to claim 12The method of insulating layer of thin-film, which is characterized in that step (1) is described to be stirred
Mixing speed is 500rpm, and ageing time is 24 hours.
3. a kind of low temperature preparation ZrO according to claim 12The method of insulating layer of thin-film, which is characterized in that in step (2)
The process conditions of the spin coating are as follows: 4000~6000rpm of revolving speed, spin coating number 3~5 times, each 30~40s of spin-coating time, often
200 DEG C of annealing temperature between secondary spin coating, 3~5min of time.
4. a kind of prepare ZrO2The method of insulating layer of thin-film laminated construction, which is characterized in that obtained by any one of claims 1 to 3
ZrO2By magnetron sputtering circle Al electrode on insulating layer of thin-film, MIM (ITO/ZrO is obtained2/ Al) laminated construction.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810728835.7A CN109003887A (en) | 2018-07-05 | 2018-07-05 | A kind of low temperature preparation ZrO2The method of insulating layer of thin-film and laminated construction |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810728835.7A CN109003887A (en) | 2018-07-05 | 2018-07-05 | A kind of low temperature preparation ZrO2The method of insulating layer of thin-film and laminated construction |
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| CN109003887A true CN109003887A (en) | 2018-12-14 |
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| CN201810728835.7A Pending CN109003887A (en) | 2018-07-05 | 2018-07-05 | A kind of low temperature preparation ZrO2The method of insulating layer of thin-film and laminated construction |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110543056A (en) * | 2019-08-27 | 2019-12-06 | 华南理工大学 | Inorganic all-solid-state electrochromic device and preparation method thereof |
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|---|---|---|---|---|
| CN1342783A (en) * | 2001-09-14 | 2002-04-03 | 中国科学院上海硅酸盐研究所 | Process for preparing functional gradient film of lead zirconate titanate ceramics |
| US20120049181A1 (en) * | 2010-08-26 | 2012-03-01 | Industry-Academic Cooperation Foundation, Yonsei University | Composition for oxide thin film, method of preparing the composition, method of forming the oxide thin film, and electronic device using the composition |
| US20120080678A1 (en) * | 2009-05-26 | 2012-04-05 | Industry-Academic Cooperation Foundation, Yonsei University | Compositions for solution process, electronic devices fabricated using the same, and fabrication methods thereof |
| US20120168747A1 (en) * | 2010-12-31 | 2012-07-05 | Industry-Academic Corporation Foundation, Yonsei University | Composition for oxide thin film, preparation method of the composition, methods for forming the oxide thin film using the composition, and electronic device using the composition |
| CN106431397A (en) * | 2016-09-14 | 2017-02-22 | 齐鲁工业大学 | Low-temperature solution preparation method of high-dielectric zirconium oxide thin film |
-
2018
- 2018-07-05 CN CN201810728835.7A patent/CN109003887A/en active Pending
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| CN1342783A (en) * | 2001-09-14 | 2002-04-03 | 中国科学院上海硅酸盐研究所 | Process for preparing functional gradient film of lead zirconate titanate ceramics |
| US20120080678A1 (en) * | 2009-05-26 | 2012-04-05 | Industry-Academic Cooperation Foundation, Yonsei University | Compositions for solution process, electronic devices fabricated using the same, and fabrication methods thereof |
| US20120049181A1 (en) * | 2010-08-26 | 2012-03-01 | Industry-Academic Cooperation Foundation, Yonsei University | Composition for oxide thin film, method of preparing the composition, method of forming the oxide thin film, and electronic device using the composition |
| US20120168747A1 (en) * | 2010-12-31 | 2012-07-05 | Industry-Academic Corporation Foundation, Yonsei University | Composition for oxide thin film, preparation method of the composition, methods for forming the oxide thin film using the composition, and electronic device using the composition |
| CN106431397A (en) * | 2016-09-14 | 2017-02-22 | 齐鲁工业大学 | Low-temperature solution preparation method of high-dielectric zirconium oxide thin film |
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| KYUNG HYUN CHOI等: "《Versatile resistive switching (memristive) behavior in an ITO-ZRO2-AG sandwich fabricated using electrohydrodynamic printing》", 《JOURNAL OF THE KOREAN PHYSICAL SOCIETY》 * |
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Application publication date: 20181214 |