CN108389777A - A kind of method that solwution method prepares zirconium oxide insulating layer of thin-film and laminated construction - Google Patents
A kind of method that solwution method prepares zirconium oxide insulating layer of thin-film and laminated construction Download PDFInfo
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- CN108389777A CN108389777A CN201810060622.1A CN201810060622A CN108389777A CN 108389777 A CN108389777 A CN 108389777A CN 201810060622 A CN201810060622 A CN 201810060622A CN 108389777 A CN108389777 A CN 108389777A
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- zirconium oxide
- oxide insulating
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L28/00—Passive two-terminal components without a potential-jump or surface barrier for integrated circuits; Details thereof; Multistep manufacturing processes therefor
- H01L28/40—Capacitors
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- 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
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- 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
- H01L21/02205—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 the layer being characterised by the precursor material for deposition
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- 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
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- 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
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- Microelectronics & Electronic Packaging (AREA)
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- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Formation Of Insulating Films (AREA)
Abstract
The invention belongs to thin-film transistor technologies fields, disclose a kind of method that solwution method prepares zirconium oxide insulating layer of thin-film and laminated construction.By Zr (NO3)4·5H2O is dissolved in glycol monoethyl ether, and stirring aging obtains precursor solution；Then precursor solution on ito glass substrate obtained by spin coating makes annealing treatment 1~2h at 200 DEG C, obtains zirconium oxide insulating layer of thin-film.By magnetron sputtering circle Al electrodes on gained zirconium oxide insulating layer of thin-film, MIM laminated construction is obtained.The present invention passes through Zr (NO3)4·5H2O obtains ZrO containing nitrato2The precursor solution of insulating layer can require the heatproof of substrate relatively low in the organic impurities in the based Dehumidification Membranes that go down compared with low temperature thermal oxidation, while avoid treatment with ultraviolet light needed for conventional cryogenic technique, reduce the complexity of annealing process.
Description
Technical field
The invention belongs to thin-film transistor technologies fields, and in particular to a kind of solwution method prepare zirconium oxide insulating layer of thin-film and
The method of laminated construction.
Background technology
Thin film transistor (TFT) (Thin Film Transistor, abbreviation TFT), is a kind of widely used semiconductor devices,
Its most important purposes is to be used to drive liquid crystal arrangement to change in the display and OLED pixel is driven to shine.It insulate in TFT
The effects that layer can play storage capacitance and prevent signal cross-talk, had both influenced the transfer performance of TFT devices, while influencing its stability
And the service life.ZrO2There are high relative dielectric constant (~27), wider forbidden band (7.8eV), is a kind of common dielectric layer material.
ZrO is prepared using solwution method2During insulation film, it is often necessary to higher (>350 DEG C) annealing temperature make a return journey in based Dehumidification Membranes
Organic impurities etc., and so high annealing temperature makes ZrO2Insulation film is difficult to tie with flexible substrate (heatproof~200 DEG C)
It closes, is unfavorable for realizing Flexible Displays.In order to solve this problem, the method for mainstream is at present, passes through ultraviolet light spin coating
Wet film, to reduce required annealing temperature.But this mode needs complicated annealing process and annealing device, is unfavorable for simultaneously
Large-area treatment.
Invention content
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 solution
Method prepares ZrO2The method of insulating layer of thin-film.
It is still another object of the present invention to provide a kind of solwution methods to prepare ZrO2The method of insulating layer of thin-film laminated construction.
The object of the invention is achieved through the following technical solutions：
A kind of solwution method preparation ZrO2The method of insulating layer of thin-film, including following preparation process：
(1) by Zr (NO3)4·5H2O (five nitric hydrate zirconiums) is dissolved in glycol monoethyl ether (2-MOE), and stirring aging obtains
To precursor solution；
(2) precursor solution on ito glass substrate obtained by spin-coating step (1), then at 200 DEG C annealing 1~
2h obtains zirconium oxide insulating layer of thin-film.
Preferably, Zr (NO in precursor solution described in step (1)3)4·5H2A concentration of 0.3~0.6mol/L of O.
Preferably, the process conditions of spin coating described in step (2) are：4000~6000rpm of rotating speed, spin coating number 3~5
It is secondary, 30~40s of spin coating time, 200 DEG C of annealing temperature between each spin coating, 3~5min of time.
A kind of solwution method preparation ZrO2The method of insulating layer of thin-film laminated construction is led on gained zirconium oxide insulating layer of thin-film
Magnetron sputtering circle Al electrodes are crossed, MIM (ITO/ZrO are obtained2/ Al) laminated construction.
The principle of the present invention is：By Zr (NO3)4·5H2O (five nitric hydrate zirconiums) is dissolved in glycol monoethyl ether and can obtain
To the presoma containing nitrato, during wet film is annealed, due to removal nitrato needed for temperature it is relatively low, so as to
Lower temperature removing impurities realize ZrO2The low temperature preparation of film.
Compared with prior art, the invention has the advantages that and advantageous effect：
The present invention passes through Zr (NO3)4·5H2O obtains ZrO containing nitrato2The precursor solution of insulating layer, can be relatively low
Annealing temperature is gone down the organic impurities in based Dehumidification Membranes, requires the heatproof of substrate relatively low, while avoiding institute in conventional cryogenic technique
The treatment with ultraviolet light needed, reduces the complexity of annealing process.
Description of the drawings
Fig. 1 is ZrO prepared by the present invention2The polarisation figure of insulating layer of thin-film.
Fig. 2 is ZrO obtained by embodiment 1 (0.6mol/L rotating speed 6000rpm spin coatings 3 times)2The leakage current of insulating layer of thin-film is close
It writes music line chart.
Fig. 3 is ZrO obtained by embodiment 2 (0.3mol/L rotating speed 5000rpm spin coatings 5 times)2The leakage current of insulating layer of thin-film is close
It writes music line chart.
Specific implementation mode
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 2.576g Zr (NO3)4·5H2O (five nitric hydrate zirconiums) is dissolved in 10ml ethylene glycol list first
In ether (2-MOE), stirring aging obtains the precursor solution of 0.6mol/L.
(2) prepared by substrate：The ITO electrode of one layer of 150nm is deposited in glass baseplate surface, cleaning, drying obtains ito glass
Substrate.
(3) in ito glass substrate by the precursor solution obtained by selected technological parameter spin-coating step (1), spin coating rotating speed
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 zirconium oxide insulating layer of thin-film.
(4) it is prepared by the round Al electrodes of magnetron sputtering 100nm on the zirconium oxide insulating layer of thin-film of step (3)
MIM(ITO/ZrO2/ Al) laminated construction.
ZrO obtained by the present embodiment2The polarisation figure of insulating layer of thin-film is as shown in Figure 1.
ZrO obtained by the present embodiment2Test results are shown in figure 2 for the leakage current of insulating layer of thin-film.
Test result shows to anneal at 200 DEG C of the present embodiment the ZrO of preparation2Insulating layer of thin-film has preferable insulating properties
Can, the leakage current density under 5V voltages is 6.49 × 10-6A/cm2。
Embodiment 2
(1) presoma is prepared：By 1.288g Zr (NO3)4·5H2O (five nitric hydrate zirconiums) is dissolved in 10ml ethylene glycol list first
In ether (2-MOE), stirring aging obtains the precursor solution of 0.3mol/L.
(2) prepared by substrate：The ITO electrode of one layer of 150nm is deposited in glass baseplate surface, cleaning, drying obtains ito glass
Substrate.
(3) in ito glass substrate by the precursor solution obtained by selected technological parameter spin-coating step (1), spin coating rotating speed
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 zirconium oxide insulating layer of thin-film.
(4) it is prepared by the round Al electrodes of magnetron sputtering 100nm on the zirconium oxide insulating layer of thin-film of step (3)
MIM(ITO/ZrO2/ Al) laminated construction.
ZrO obtained by the present embodiment2Test results are shown in figure 3 for the leakage current of insulating layer of thin-film.
Test result shows to anneal at 200 DEG C of the present embodiment the ZrO of preparation2Insulating layer of thin-film has preferable insulating properties
Can, the leakage current density under 5V voltages is 6.71 × 10-5A/cm2。
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by changes, modifications, substitutions, combinations, simplifications,
Equivalent substitute mode is should be, is included within the scope of the present invention.
Claims (4)
1. a kind of solwution method prepares ZrO2The method of insulating layer of thin-film, it is characterised in that including following preparation process：
(1) by Zr (NO3)4·5H2O is dissolved in glycol monoethyl ether, and stirring aging obtains precursor solution；
(2) precursor solution on ito glass substrate obtained by spin-coating step (1) then makes annealing treatment 1~2h at 200 DEG C, obtains
To zirconium oxide insulating layer of thin-film.
2. a kind of solwution method according to claim 1 prepares ZrO2The method of insulating layer of thin-film, it is characterised in that：Step (1)
Described in Zr (NO in precursor solution3)4·5H2A concentration of 0.3~0.6mol/L of O.
3. a kind of solwution method according to claim 1 prepares ZrO2The method of insulating layer of thin-film, it is characterised in that step (2)
Described in the process conditions of spin coating be：4000~6000rpm of rotating speed, spin coating number 3~5 times, 30~40s of spin coating time, every time
200 DEG C of annealing temperature between spin coating, 3~5min of time.
4. a kind of solwution method prepares ZrO2The method of insulating layer of thin-film laminated construction, it is characterised in that：It is any in claims 1 to 3
By magnetron sputtering circle Al electrodes on zirconium oxide insulating layer of thin-film obtained by, MIM laminated construction is obtained.
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| CN201810060622.1A CN108389777A (en) | 2018-01-22 | 2018-01-22 | A kind of method that solwution method prepares zirconium oxide insulating layer of thin-film and laminated construction |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810060622.1A CN108389777A (en) | 2018-01-22 | 2018-01-22 | A kind of method that solwution method prepares zirconium oxide insulating layer of thin-film and laminated construction |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109616525A (en) * | 2018-11-28 | 2019-04-12 | 华南理工大学 | A kind of method that solwution method prepares zirconium aluminum oxide insulating layer of thin-film and laminated construction |
| CN110534434A (en) * | 2019-07-15 | 2019-12-03 | 华南理工大学 | A kind of method that solwution method prepares metal oxide TFD |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102222761A (en) * | 2011-04-12 | 2011-10-19 | 西南交通大学 | Preparation method of high temperature superconductive coating conductor La2Zr2O7 buffer layer film |
| 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
- 2018-01-22 CN CN201810060622.1A patent/CN108389777A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102222761A (en) * | 2011-04-12 | 2011-10-19 | 西南交通大学 | Preparation method of high temperature superconductive coating conductor La2Zr2O7 buffer layer film |
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| LI XIFENG 等: "Low-Temperature Solution-Processed Zirconium Oxide Gate Insulators for Thin-Film Transistors", 《IEEE TRANSACTIONS ON ELECTRON DEVICES》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109616525A (en) * | 2018-11-28 | 2019-04-12 | 华南理工大学 | A kind of method that solwution method prepares zirconium aluminum oxide insulating layer of thin-film and laminated construction |
| WO2020108140A1 (en) * | 2018-11-28 | 2020-06-04 | 华南理工大学 | Method for preparing zirconium-aluminium oxide insulating layer thin film and laminated structure using solution method |
| CN110534434A (en) * | 2019-07-15 | 2019-12-03 | 华南理工大学 | A kind of method that solwution method prepares metal oxide TFD |
| CN110534434B (en) * | 2019-07-15 | 2021-11-19 | 华南理工大学 | Method for preparing metal oxide TFD (thin film transistor) by solution method |
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Application publication date: 20180810 |