CN107129722A - A kind of inkjet printing zirconium oxide insulating barrier ink and preparation method thereof - Google Patents
A kind of inkjet printing zirconium oxide insulating barrier ink and preparation method thereof Download PDFInfo
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- CN107129722A CN107129722A CN201710399212.5A CN201710399212A CN107129722A CN 107129722 A CN107129722 A CN 107129722A CN 201710399212 A CN201710399212 A CN 201710399212A CN 107129722 A CN107129722 A CN 107129722A
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- inkjet printing
- ethylene glycol
- insulating barrier
- zirconium oxide
- oxide insulating
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/38—Inkjet printing inks characterised by non-macromolecular additives other than solvents, pigments or dyes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/36—Inkjet printing inks based on non-aqueous solvents
Abstract
The invention discloses a kind of inkjet printing zirconium oxide insulating barrier ink and preparation method thereof.The inkjet printing zirconium oxide insulating barrier ink, including solute and solvent, described solute are basic zirconium chloride；Described solvent is ethylene glycol monomethyl ether, ethylene glycol and polyethylene glycol.The ink prepares the method for solution age by the way that basic zirconium chloride to be dissolved into the in the mixed solvent of ethylene glycol monomethyl ether, ethylene glycol and polyethylene glycol after stirring.The inkjet printing zirconium oxide insulating barrier of the present invention is not interfered with the dissolving of basic zirconium chloride while the boiling point of solution and its viscosity is lifted, is made obtained stable system, be particularly suited for inkjet printing with polyethylene glycol and ethylene glycol is introduced in ink.
Description
Technical field
The invention belongs to flat display field, more particularly to a kind of inkjet printing zirconium oxide insulating barrier ink and its preparation
Method.
Background technology
Existing solwution method processing insulation layer process mainly has spin coating, inkjet printing and volume to volume etc..Wherein spin coating work
Skill is because process is simple, quality of forming film is excellent and is widely used in scientific research.It is molten that a kind of spin coating proceeding is commonly used
Liquid is that basic zirconium chloride is dissolved in ethylene glycol monomethyl ether, forms metal hydroxides as precursor, is heated with after the solution spin coating
Solvent is removed, while metal hydroxides occur polymerization and aoxidized, metal-oxygen-metal structure is formed, ultimately forms zirconium oxide thin
Film.Above-mentioned solution is successfully applied in spin coating proceeding, is all had been reported that in many documents.But the solution is in application
Many problems are but exposed when inkjet printing.First, the ink of printing must be the solution of slow curing type, and above-mentioned solution
Solvent ethylene glycol methyl ether boiling point and vapour pressure it is relatively low, printing when ink droplet could not often merge the figure as an entirety
Shape just has been cured；In addition, the solution causes overall viscosity relatively low because solvent viscosity is relatively low, its ink-jet shape during applied to printing
State is not good with pattern forming effect.
The content of the invention
The primary and foremost purpose of the present invention is to overcome the shortcoming and deficiency of prior art, and there is provided a kind of inkjet printing zirconium oxide is exhausted
Edge layer ink.
Another object of the present invention is to provide the preparation method of the inkjet printing zirconium oxide insulating barrier ink.
A further object of the present invention is the application for providing the inkjet printing zirconium oxide insulating barrier ink.
The purpose of the present invention is achieved through the following technical solutions：A kind of inkjet printing zirconium oxide insulating barrier ink, including
Solute and solvent, described solute are basic zirconium chloride；Described solvent is ethylene glycol monomethyl ether, ethylene glycol and polyethylene glycol.
The consumption of described ethylene glycol monomethyl ether by the cumulative volume ratio of ethylene glycol monomethyl ether and ethylene glycol and polyethylene glycol for 0.2~
2：1 proportioning is calculated.
The consumption of described ethylene glycol is 0.25~4 by the volume ratio of ethylene glycol and polyethylene glycol：1 proportioning is calculated.
The consumption of described polyethylene glycol is 0.25~4 by the volume ratio of polyethylene glycol and ethylene glycol monomethyl ether：1 proportioning meter
Calculate.
Molar concentration of the consumption of described basic zirconium chloride by basic zirconium chloride in final system is based on 0.3~0.6mol/L
Calculate, preferably calculated by 0.5mol/L；Described basic zirconium chloride is preferably eight water oxygen zirconium chlorides.
Described polyethylene glycol is preferably polyethylene glycol 200.
The preparation method of described inkjet printing zirconium oxide insulating barrier ink, comprises the following steps：Basic zirconium chloride is molten
The in the mixed solvent of ethylene glycol monomethyl ether, ethylene glycol and polyethylene glycol is solved, makes solution age after being well mixed, obtains inkjet printing
Zirconium oxide insulating barrier ink.
Described mixing is mixed by the way of magnetic force concussion；Preferably magnetic rotor is added in finger bottle to use
The mode of magnetic force concussion is mixed.
The time of described magnetic force concussion is 1~5h, preferably 2h.
The cleaning of described finger bottle is preferably realized by the following method：Finger Bottle and bottle cap to be washed is sunk into isopropanol
Middle carry out ultrasonic vibration, then deionized water progress ultrasonic vibration is changed, drying obtains the finger bottle of cleaning.
The frequency of described progress ultrasonic vibration is preferably 53kHz；Time is preferably 15min.
Described drying is preferably to be put into baking oven to be dried.
The cleaning of described magnetic rotor is preferably realized by the following method：Magnetic rotor to be washed is sequentially placed into and is equipped with
Cleaned, dried in isopropanol, tetrahydrofuran, deionized water, the container of isopropanol, obtain the magnetic rotor of cleaning.
Described container is preferably glass container, more preferably beaker.
Described cleaning is preferably to be cleaned by the way of ultrasonic vibration.
The time of described ultrasonic vibration is preferably 5min.
Described drying is preferably to be put into baking oven to be dried.
The number of times that described deionized water is cleaned is preferably 2 times.
The time of described solution age is 24~72h, preferably 24h.
Application of the described inkjet printing zirconium oxide insulating barrier ink in flat display field.
Principle analysis：It is because there occurs that metal ion replaces solvent molecule hydroxyl that basic zirconium chloride, which is dissolved in ethylene glycol monomethyl ether,
The hydroxylation reaction of hydrogen on base.Add after polyethylene glycol 200, because polyethylene glycol 200 molecule contains multiple ethers, these ethers
With the hydroxyl formation hydrogen bond of ethylene glycol monomethyl ether, destroy the progress of metal hydroxylation reaction so that basic zirconium chloride can not dissolve, formed
Precipitation；And the addition of ethylene glycol make it that solution system hydroxy radical content is greatly increased, therefore, it is possible to regenerate metal hydroxides, make
It must precipitate and dissolve again.
The present invention has the following advantages and effect relative to prior art：
1st, the present invention relates to the solwution method processing of thin film transistor (TFT) zirconium oxide insulating barrier in flat display field, emphasis is solved
The problem of be how by add other reagents adjust solution physical property while will not also destroy inorganic salts organic molten
Dissolving in agent.Improve the physical properties such as boiling point, the viscosity of solution used in existing spin coating using the method for the present invention, make it
Inkjet printing can be applied to.Due to polyethylene glycol 200 have higher boiling point (>250 DEG C), larger viscosity (>20cps),
And property is stable, typically not with other solvent reactions, can preferably be dissolved each other with many commonly-used solvent, but ethylene glycol monomethyl ether and poly- second
Just basic zirconium chloride can not be dissolved after glycol 200 is miscible, by adding ethylene glycol, basic zirconium chloride can be improved in the mixed solvent
Dissolubility, solution is being lifted boiling point and is not also being interfered with the dissolving of solute while viscosity.
2nd, the present invention makes it be applied to inkjet printing by carrying out composition adjustment to the solution used in spin coating.
3rd, the present invention in more ripe spin coating by, with conventional reagent polyethylene glycol 200 is introduced in solution system, carrying
The boiling point and its viscosity of solution have been risen, it is particularly suited for inkjet printing；Then proceed to introduce second in mixed solvent system
Glycol, enables basic zirconium chloride to be dissolved in the mixed solvent system.
Brief description of the drawings
Fig. 1 is solution viscosity and the change curve of ethylene glycol monomethyl ether and the volume ratio of polyethylene glycol 200；Wherein, V1 and
V3 is respectively ethylene glycol monomethyl ether and the volume of polyethylene glycol 200.
Fig. 2 be addition or without polyethylene glycol 200 basic zirconium chloride ethylene glycol monomethyl ether solution result figure；Wherein, 1
It is the oxychloride of addition polyethylene glycol 200 for the ethylene glycol monomethyl ether solution for the basic zirconium chloride for being not added with polyethylene glycol 200,2,3,4
The ethylene glycol monomethyl ether solution of zirconium.
Fig. 3 is the result figure after the ethylene glycol monomethyl ether solution left standstill for the basic zirconium chloride for adding polyethylene glycol 200.
Fig. 4 is added after the solution left standstill that polyethylene glycol 200 becomes cloudy, and is added ethylene glycol, is precipitated the knot dissolved again
Fruit is schemed.
Fig. 5 is added after the solution left standstill that polyethylene glycol 200 becomes cloudy, and adds ethylene glycol, then stand the knot after one month
Fruit is schemed.
Embodiment
With reference to embodiment, the present invention is described in further detail, but the implementation of the present invention is not limited to this.
Embodiment 1
1st, medicine and reagent prepare
Solution preparation raw material prepares：Eight water oxygen zirconium chlorides, analyze pure, content >=99.0%, and profit prompt chemical reagent in Shanghai has
Limit company；Ethylene glycol monomethyl ether, analyzes pure, content >=99.0%, Tianjin Fu Yu Fine Chemical Co., Ltd；Polyethylene glycol 200,
Chemical pure, molecular weight 190~210, Shanghai Run Jie chemical reagent Co., Ltd；Ethylene glycol, analyzes pure, content >=99.0%, on
Hai Runjie chemical reagent Co., Ltd.
2nd, substrate, cleaning container
Finger bottle cleaning：Finger bottle cap to be washed is backed out, sunk in the large beaker equipped with isopropanol, bottle cap is also in the lump
It is put into, it should be noted that need to be completely filled with by isopropanol in bottle, it is impossible to have bubble, then ultrasonic (53kHz) vibration 15min, then change
Same ultrasonic (53kHz) the vibration 15min of deionized water.It should be noted that tweezers should be avoided to contact in bottle when shifting bottle using tweezers
Wall.Bottle is put into drying in oven by cleaning after finishing.
Magnetic rotor is cleaned：By magnetic rotor to be washed be sequentially placed into equipped with isopropanol, tetrahydrofuran, alkaline detergent solution,
Ultrasonic (53kHz) vibration is carried out in deionized water, the beaker of isopropanol, cleaning every time continues 5min, and wherein deionized water is clear
Wash needs twice.Cleaning is put into baking oven after finishing and dried.
3rd, solution is prepared
Ten part of eight water oxygen zirconium chloride is weighed in balance, every part of 0.58g is transferred in finger bottle respectively.The three of every part of solution
The cumulative volume of kind of solvent (ethylene glycol monomethyl ether, ethylene glycol, polyethylene glycol 200) is 6ml, measured with glue head dropper ethylene glycol monomethyl ether,
The ratio between ethylene glycol, volume of polyethylene glycol 200 are respectively 1:1:4、1:2:3、1:3:2、1:4:1、2:1:3、2:2:2、2:3:1、
3:1:2、3:2:1、4:1:1, it is separately added into correspondence finger bottle, and progress magnetic force concussion 2h after magnetic rotor is added, it is last quiet
Putting makes solution age 24h.
The molar concentration of the zirconium oxychloride of each solution is identical (being all 0.5mol/L) above.
4th, solution physical property is characterized
(1) using the viscosity of viscosity meter solution obtained as above, measurement result is：Ethylene glycol monomethyl ether, ethylene glycol, poly- second
The ratio between volume of glycol 200 is respectively 1:1:4、1:2:3、1:3:2、1:4:1、2:1:3、2:2:2、2:3:1、3:1:2、3:2:1、
4:1:1, corresponding viscosity is respectively 31.6,22.2,19.8,16.1,15.7,12.0,14.9,10.7,8.94,5.57 (units
cps)。
As can be seen that as ethylene glycol monomethyl ether and the volume ratio of polyethylene glycol 200 constantly increase, solution viscosity gradually under
Drop.Using ethylene glycol monomethyl ether volume as V1, ethylene glycol volume is V2, and polyethylene glycol 200 volume is V3, ethylene glycol and polyethylene glycol
200 cumulative volumes are V0.When V1 and V0 ratio is changing between 0.2~2, can by solution viscosity control 6~32cps it
Between.Solution viscosity can be adjusted in smaller range by the ratio for adjusting V2 and V3：V1 and V0 ratio is bigger, V2 and V3's
The effect of ratio regulation viscosity is weaker.As V1/V0=0.2, the effect of V2 and V3 ratio regulation viscosity is most strong, works as V2/V3
When changing between 0.25~4, solution viscosity changes between 16~32cps.As V1/V0=2, with V2/V3 change,
Solution viscosity can only be fluctuated in 6cps or so small ranges.
(2) present invention in more ripe spin coating by, with conventional reagent polyethylene glycol 200 is introduced in solution system, carrying
The boiling point and its viscosity of solution have been risen, it is particularly suited for inkjet printing, when ethylene glycol given volume, solution viscosity and second
The change curve of the volume ratio of glycol methyl ether and polyethylene glycol 200 as shown in figure 1, wherein V1 and V3 be respectively ethylene glycol monomethyl ether with
The volume of polyethylene glycol 200.It can be seen that polyethylene glycol has significant effect for the viscosity regulation of system, lead to
Cross the appropriate adjustment to volume ratio and can obtain wanted viscosity.
(3) due to the introducing of ethylene glycol so that the mixed system still has good solvability to zirconium chloride.
Basic zirconium chloride is dissolved in ethylene glycol monomethyl ether (spin coating stoste, 0.5mol/L), polyethylene glycol 200 but not is added
Add and precipitation is generated in ethylene glycol, solution, as a result as shown in Fig. 2 wherein, the leftmost side (numbering is 1) is not add polyethylene glycol
Spin coating stoste；Three bottles of right side (numbering is 2,3,4) is the solution after addition polyethylene glycol 200, it is seen that solution becomes muddy.
Stand after a period of time, as a result as shown in figure 3, precipitating coagulation in turbid liquid as we can see from the figure, layering illustrates body
It is unstable.
Add after ethylene glycol, as a result disappeared as shown in figure 4, being precipitated as we can see from the figure in solution, illustrate precipitation weight
New dissolving.
After standing one month, as a result as shown in figure 5, solution is still clarified as we can see from the figure, it is steady to illustrate the system
Fixed.
Above-described embodiment is preferably embodiment, but embodiments of the present invention are not by above-described embodiment of the invention
Limitation, other any Spirit Essences without departing from the present invention and the change made under principle, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
1. a kind of inkjet printing zirconium oxide insulating barrier ink, including solute and solvent, it is characterised in that：Described solute is chlorine
Zirconium oxide；Described solvent is ethylene glycol monomethyl ether, ethylene glycol and polyethylene glycol.
2. inkjet printing zirconium oxide insulating barrier ink according to claim 1, it is characterised in that：Described ethylene glycol first
The consumption of ether is 0.2~2 by the cumulative volume ratio of ethylene glycol monomethyl ether and ethylene glycol and polyethylene glycol：1 proportioning is calculated；Described second two
The consumption of alcohol is 0.25~4 by the volume ratio of ethylene glycol and polyethylene glycol：1 proportioning is calculated.
3. inkjet printing zirconium oxide insulating barrier ink according to claim 2, it is characterised in that：Described polyethylene glycol
Consumption by the volume ratio of polyethylene glycol and ethylene glycol monomethyl ether be 0.25~4：1 proportioning is calculated.
4. inkjet printing zirconium oxide insulating barrier ink according to claim 1, it is characterised in that：Described basic zirconium chloride
Consumption by molar concentration of the basic zirconium chloride in final system be 0.3~0.6mol/L calculating.
5. inkjet printing zirconium oxide insulating barrier ink according to claim 1, it is characterised in that：Described basic zirconium chloride
Consumption be by molar concentration of the basic zirconium chloride in final system be 0.5mol/L calculate.
6. inkjet printing zirconium oxide insulating barrier ink according to claim 1, it is characterised in that：Described polyethylene glycol
For polyethylene glycol 200；Described basic zirconium chloride is eight water oxygen zirconium chlorides.
7. the preparation method of the inkjet printing zirconium oxide insulating barrier ink described in any one of claim 1~6, its feature exists
In comprising the following steps：Basic zirconium chloride is dissolved into the in the mixed solvent of ethylene glycol monomethyl ether, ethylene glycol and polyethylene glycol, mixed
Make solution age after uniform, obtain inkjet printing zirconium oxide insulating barrier ink.
8. the preparation method of inkjet printing zirconium oxide insulating barrier ink according to claim 7, it is characterised in that：It is described
Solution age time be 24~72h.
9. the preparation method of inkjet printing zirconium oxide insulating barrier ink according to claim 7, it is characterised in that：It is described
Mixing using magnetic force shake by the way of mixed；The time of described magnetic force concussion is 1~5h.
10. the answering in flat display field of the inkjet printing zirconium oxide insulating barrier ink described in any one of claim 1~6
With.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710399212.5A CN107129722B (en) | 2017-05-31 | 2017-05-31 | Ink for ink-jet printing of zirconia insulating layer and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710399212.5A CN107129722B (en) | 2017-05-31 | 2017-05-31 | Ink for ink-jet printing of zirconia insulating layer and preparation method thereof |
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| Publication Number | Publication Date |
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| CN107129722A true CN107129722A (en) | 2017-09-05 |
| CN107129722B CN107129722B (en) | 2020-10-27 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108022828A (en) * | 2017-11-13 | 2018-05-11 | 华南理工大学 | A kind of method that UV pre-processed substrates improve printing sull pattern |
| CN108396313A (en) * | 2018-01-26 | 2018-08-14 | 华南理工大学 | A kind of heat treatment method reducing inkjet printing film surface crackle |
| CN109244237A (en) * | 2018-07-26 | 2019-01-18 | 华南理工大学 | A kind of multi-sheet printed method for improving solwution method zirconium oxide insulating layer performance |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103804993A (en) * | 2013-11-27 | 2014-05-21 | 佛山市明朝科技开发有限公司 | Extra-white aqueous ceramic ink-jet ink and preparation method thereof |
| CN104892029A (en) * | 2015-05-19 | 2015-09-09 | 吴权武 | A preparing method of ceramic inkjet ink |
| 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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2017
- 2017-05-31 CN CN201710399212.5A patent/CN107129722B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103804993A (en) * | 2013-11-27 | 2014-05-21 | 佛山市明朝科技开发有限公司 | Extra-white aqueous ceramic ink-jet ink and preparation method thereof |
| CN104892029A (en) * | 2015-05-19 | 2015-09-09 | 吴权武 | A preparing method of ceramic inkjet ink |
| 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 |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108022828A (en) * | 2017-11-13 | 2018-05-11 | 华南理工大学 | A kind of method that UV pre-processed substrates improve printing sull pattern |
| CN108022828B (en) * | 2017-11-13 | 2021-05-14 | 华南理工大学 | Method for improving morphology of printed oxide film by UV pretreatment of substrate |
| CN108396313A (en) * | 2018-01-26 | 2018-08-14 | 华南理工大学 | A kind of heat treatment method reducing inkjet printing film surface crackle |
| CN109244237A (en) * | 2018-07-26 | 2019-01-18 | 华南理工大学 | A kind of multi-sheet printed method for improving solwution method zirconium oxide insulating layer performance |
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| CN107129722B (en) | 2020-10-27 |
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