CN109266099A - A kind of zirconium oxide ink-jet printing ink and the method for preparing zirconium oxide nano crystal film - Google Patents
A kind of zirconium oxide ink-jet printing ink and the method for preparing zirconium oxide nano crystal film Download PDFInfo
- Publication number
- CN109266099A CN109266099A CN201810958604.5A CN201810958604A CN109266099A CN 109266099 A CN109266099 A CN 109266099A CN 201810958604 A CN201810958604 A CN 201810958604A CN 109266099 A CN109266099 A CN 109266099A
- Authority
- CN
- China
- Prior art keywords
- ink
- zirconium oxide
- jet printing
- printing ink
- nano crystal
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
- C23C18/1208—Oxides, e.g. ceramics
- C23C18/1216—Metal oxides
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1254—Sol or sol-gel processing
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Thermal Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Dispersion Chemistry (AREA)
- Ceramic Engineering (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention belongs to printed electronic field of material technology, a kind of disclose zirconium oxide ink-jet printing ink and prepare zirconium oxide nano crystal film method.The ink-jet printing ink is made of ethylene glycol, eight water oxygen zirconium chlorides and polyacrylamide.Zirconium oxide ink-jet printing ink is prepared into liquid film by inkjet printing, is stood, after the complete gel of liquid film, film is placed in baking oven dry 5~10h at 70~80 DEG C, 300~400 DEG C of annealings is then heated to, obtains zirconium oxide nano crystal film.The present invention makes ink gelation reaction occur after heating to form gel network, provides reaction site for oxide precursor, make it easier to form oxide structure or even crystallization at low temperature by introducing polymer poly acrylamide in system.The thermal decomposition of polymer can generate localized hyperthermia simultaneously, further promote the crystallization of oxide.
Description
Technical field
The invention belongs to printed electronic field of material technology, and in particular to a kind of zirconium oxide ink-jet printing ink and prepare oxygen
Change the method for zirconium nano-crystal film.
Background technique
The method of induced oxidation object crystalline orientation is generally divided into several aspects such as depositing operation, substrate, addition inducing substance.
Depositing operation refers to that some vacuum equipments can realize specific knot by accurately controlling with high precision deposition material
Crystalline form.Substrate, which refers to, selects some scripts just to have the crystalline material of certain crystal orientations as substrate, so that being deposited on
The material in face is also according to given orientation preferential growth, or modifies substrate surface, produces it to the growth of oxide
Raw effect.Addition inducing substance is common in solwution method technique, has the substance of specific structure by adding, usually high poly-
Object has an impact the crystalline orientation of oxide.
In the above method, the accurate vacuum equipment cost for controlling deposition materials structure is extremely high, and energy consumption is high, and current green
The purport that colour circle is protected is runed counter to.Substrate is extremely limited the influence depth of material, therefore will limit the thickness of growth material.Addition
Inducing substance extensive application in solwution method, and a variety of inductions can be realized as a result, but should according to the difference of selection substance
Method is at present in the rare report in inkjet printing field.
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 oxidation
Zirconium ink-jet printing ink.
A further object of the present invention is to provide the preparation methods of above-mentioned zirconium oxide ink-jet printing ink.
Another object of the present invention is to provide a kind of using above-mentioned zirconium oxide ink-jet printing ink and prepares zirconium oxide and receives
The method of the brilliant film of rice.
The object of the invention is achieved through the following technical solutions:
A kind of zirconium oxide ink-jet printing ink is made of ethylene glycol, eight water oxygen zirconium chlorides and polyacrylamide.
Preferably, the average molecular weight of the polyacrylamide is 20000~40000.
Preferably, the mass fraction of the polyacrylamide is 0.3%~0.5%, the molar concentration of eight water oxygen zirconium chlorides
For 0.3~0.5M.
The preparation method of above-mentioned zirconium oxide ink-jet printing ink, including following preparation step:
Polyacrylamide is added in ethylene glycol solvent, at 40~50 DEG C stir 3~5h dissolve it sufficiently, then plus
Enter chlorine hydrate zirconium oxide stirring and dissolving, ageing 10~obtain zirconium oxide ink-jet printing ink afterwards for 24 hours.
The method for preparing zirconium oxide nano crystal film using above-mentioned zirconium oxide ink-jet printing ink, includes the following steps:
Zirconium oxide ink-jet printing ink is prepared into liquid film by inkjet printing, is stood, it, will be thin after the complete gel of liquid film
Film is placed in baking oven dry 5~10h at 70~80 DEG C, then heats to 300~400 DEG C of annealings, obtains zirconia nanopowder
Brilliant film.
Preferably, the inkjet printing condition are as follows: substrate temperature is 25~30 DEG C, and spray head voltage is 30~40V, spray head temperature
Degree is 55~65 DEG C, and ink droplet spacing is 30~45 μm.
Preferably, the time of repose is 20~40min, and the time of annealing is 1h.
Compared with the existing technology, the invention has the following advantages and beneficial effects:
The present invention by system introduce polymer poly acrylamide, make ink occurs after heating gelation reaction thus
Form gel network, provide reaction site for oxide precursor, make it easier to be formed at low temperature oxide structure or even
Crystallization, and make presoma that polymerization reaction occur along specific orientation, to realize the preferred orientation of crystallization.While polymer
Thermal decomposition can generate localized hyperthermia, further promote the crystallization of oxide.The ink system can be with more cheap equipment
Cost realizes the deposition preparation of particular orientation sull.
Detailed description of the invention
Fig. 1 is high resolution TEM (HRTEM) figure of 1 gained zirconium oxide nano crystal film of the embodiment of the present invention.
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) polyacrylamide (average molecular weight 30000) that mass fraction is 0.4% is added to ethylene glycol solvent
In, at 50 DEG C stir 4h dissolve it sufficiently, then be added chlorine hydrate zirconium oxide stirring and dissolving, chlorine hydrate zirconium oxide it is dense
Degree is 0.4M, obtains zirconium oxide ink-jet printing ink after being aged 12h.
(2) prepared ink is filling into ink-jet printer (Dimatix 2800) clip, substrate used is glass, lining
Bottom uses UV irradiation pretreatment 60s.Printer substrate temperature is 30 DEG C when printing, and spray head voltage is 40V, nozzle temperature 60
DEG C, ink droplet spacing is 40 μm.After the completion of printing, 30min is stood on substrate, and after the complete gel of liquid film, film is placed in baking
70~80 DEG C of case dry 10h are placed in thermal station, in 350 DEG C of annealing 1h.Obtain zirconium oxide nano crystal film.
High resolution TEM (HRTEM) figure of zirconium oxide nano crystal film obtained by the present embodiment is as shown in Figure 1.With
Gatan Digital Micrograph software carries out crystal analysis to obtained image, as seen from Figure 1 oxygen obtained by the present embodiment
Changing zirconium nano-crystal film has obvious crystallization, and crystallizes more regular.
The crystallization temperature of zirconium oxide is usually at 400 DEG C or more, but zirconia film prepared by the present invention occurs at 350 DEG C
Obvious crystallization, and crystallize more regular.Therefore ink system constructed by the present invention can not increase extras cost
In the case of, promote the generation of oxide structure under low temperature, and be not particularly limited to presoma raw material, system can be dissolved in
And it keeps stablizing.
By comparing with JCPDS standard card, the letter such as interplanar distance, indices of crystallographic plane of zirconium oxide nano crystal film is obtained
Breath.The results are shown in Table 1:
Table 1
As can be seen from Table 1, the crystallization degree of different zones is different, and crystalline orientation is also relatively more mixed and disorderly, but can send out
Its existing entirety shows preferred orientation on crystal face (211) and crystal face (1-11), and especially preferred orientation is more bright on (211)
It is aobvious.As can be seen that the reticular structure formed after polymer poly acrylamide gel provides a large amount of reaction position for presoma
Point, compared to the free crowd of presoma in the solution, the direction of growth will receive limitation, thus finally be embodied in oxide
Crystalline growth have very strong inducing action.
Embodiment 2
(1) polyacrylamide (average molecular weight 20000) that mass fraction is 0.3% is added to ethylene glycol solvent
In, at 40 DEG C stir 5h dissolve it sufficiently, then be added chlorine hydrate zirconium oxide stirring and dissolving, chlorine hydrate zirconium oxide it is dense
Degree is 0.5M, and ageing obtains zirconium oxide ink-jet printing ink afterwards for 24 hours.
(2) prepared ink is filling into ink-jet printer (Dimatix 2800) clip, substrate used is glass, lining
Bottom uses UV irradiation pretreatment 80s.Printer substrate temperature is 25 DEG C when printing, and spray head voltage is 30V, nozzle temperature 65
DEG C, ink droplet spacing is 30 μm.After the completion of printing, 40min is stood on substrate, and after the complete gel of liquid film, film is placed in baking
70~80 DEG C of case dry 5h are placed in thermal station, in 300 DEG C of annealing 1h.Obtain zirconium oxide nano crystal film.
Zirconium oxide nano crystal film obtained by the present embodiment has obvious crystallization, and crystallization is more regular, and shows in crystal face
(211) and the preferred orientation on crystal face (1-11).
Embodiment 3
(1) polyacrylamide (average molecular weight 40000) that mass fraction is 0.5% is added to ethylene glycol solvent
In, at 45 DEG C stir 3h dissolve it sufficiently, then be added chlorine hydrate zirconium oxide stirring and dissolving, chlorine hydrate zirconium oxide it is dense
Degree is 0.3M, obtains zirconium oxide ink-jet printing ink after being aged 10h.
(2) prepared ink is filling into ink-jet printer (Dimatix 2800) clip, substrate used is glass, lining
Bottom uses UV irradiation pretreatment 50s.Printer substrate temperature is 30 DEG C when printing, and spray head voltage is 35V, nozzle temperature 55
DEG C, ink droplet spacing is 45 μm.After the completion of printing, 20min is stood on substrate, and after the complete gel of liquid film, film is placed in baking
70~80 DEG C of case dry 8h are placed in thermal station, in 400 DEG C of annealing 1h.Obtain zirconium oxide nano crystal film.
Zirconium oxide nano crystal film obtained by the present embodiment has obvious crystallization, and crystallization is more regular, and shows in crystal face
(211) and the preferred orientation on crystal face (1-11).
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 (7)
1. a kind of zirconium oxide ink-jet printing ink, it is characterised in that: the ink-jet printing ink is by ethylene glycol, eight water oxygen zirconium chlorides
It is formed with polyacrylamide.
2. a kind of zirconium oxide ink-jet printing ink according to claim 1, it is characterised in that: the polyacrylamide is put down
Average molecular weight is 20000~40000.
3. a kind of zirconium oxide ink-jet printing ink according to claim 1, it is characterised in that: the matter of the polyacrylamide
Measuring score is 0.3%~0.5%, and the molar concentration of eight water oxygen zirconium chlorides is 0.3~0.5M.
4. a kind of described in any item preparation methods of zirconium oxide ink-jet printing ink of claims 1 to 3, it is characterised in that including
Following preparation step:
Polyacrylamide is added in ethylene glycol solvent, 3~5h is stirred at 40~50 DEG C dissolves it sufficiently, is then added eight
It is hydrated basic zirconium chloride stirring and dissolving, ageing 10~obtain zirconium oxide ink-jet printing ink afterwards for 24 hours.
5. preparing the side of zirconium oxide nano crystal film using the described in any item zirconium oxide ink-jet printing inks of claims 1 to 3
Method, it is characterised in that include the following steps:
Zirconium oxide ink-jet printing ink is prepared into liquid film by inkjet printing, stands, after the complete gel of liquid film, film is set
5~10h is dried at 70~80 DEG C in baking oven, then heats to 300~400 DEG C of annealings, it is thin to obtain zirconium oxide nano crystal
Film.
6. the method that zirconium oxide ink-jet printing ink according to claim 5 prepares zirconium oxide nano crystal film, feature
It is the inkjet printing condition are as follows: substrate temperature is 25~30 DEG C, and spray head voltage is 30~40V, and nozzle temperature is 55~65
DEG C, ink droplet spacing is 30~45 μm.
7. the method that zirconium oxide ink-jet printing ink according to claim 5 prepares zirconium oxide nano crystal film, feature
Be: the time of repose is 20~40min, and the time of annealing is 1h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810958604.5A CN109266099A (en) | 2018-08-22 | 2018-08-22 | A kind of zirconium oxide ink-jet printing ink and the method for preparing zirconium oxide nano crystal film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810958604.5A CN109266099A (en) | 2018-08-22 | 2018-08-22 | A kind of zirconium oxide ink-jet printing ink and the method for preparing zirconium oxide nano crystal film |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109266099A true CN109266099A (en) | 2019-01-25 |
Family
ID=65153975
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810958604.5A Pending CN109266099A (en) | 2018-08-22 | 2018-08-22 | A kind of zirconium oxide ink-jet printing ink and the method for preparing zirconium oxide nano crystal film |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109266099A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112795241A (en) * | 2021-01-11 | 2021-05-14 | 季华实验室 | Mixed insulating ink, insulating film, flexible thin film transistor and preparation method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110143038A1 (en) * | 2008-06-13 | 2011-06-16 | Ceres Intellectual Property Company Limited | Method for deposition of ceramic films |
| CN103828018A (en) * | 2011-01-28 | 2014-05-28 | 西北大学 | Low-temperature fabrication of metal oxide thin films and nanomaterial-derived metal composite thin films |
| CN107955459A (en) * | 2017-11-22 | 2018-04-24 | 华南理工大学 | A kind of ink-jet printing ink and the method for metal-oxide film is prepared by it |
-
2018
- 2018-08-22 CN CN201810958604.5A patent/CN109266099A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110143038A1 (en) * | 2008-06-13 | 2011-06-16 | Ceres Intellectual Property Company Limited | Method for deposition of ceramic films |
| CN103828018A (en) * | 2011-01-28 | 2014-05-28 | 西北大学 | Low-temperature fabrication of metal oxide thin films and nanomaterial-derived metal composite thin films |
| CN107955459A (en) * | 2017-11-22 | 2018-04-24 | 华南理工大学 | A kind of ink-jet printing ink and the method for metal-oxide film is prepared by it |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112795241A (en) * | 2021-01-11 | 2021-05-14 | 季华实验室 | Mixed insulating ink, insulating film, flexible thin film transistor and preparation method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107151483B (en) | Ink for ink-jet printing, preparation method thereof and zirconia film printed by same | |
| Liu et al. | Recent advances in inkjet printing synthesis of functional metal oxides | |
| TWI353808B (en) | Method for fabricating conductive pattern on flexi | |
| CN103203468B (en) | A kind of preparation method of nano silver wire | |
| CN107573761A (en) | A kind of zirconium oxide ink-jet printing ink and its preparation method and application | |
| CN107955459B (en) | Ink for ink-jet printing and method for preparing metal oxide film by using ink | |
| CN108396313B (en) | A kind of heat treatment method reducing inkjet printing film surface crackle | |
| CN104761952B (en) | The ceramic ink jet printing ink and method of a kind of adjustable penetration depth | |
| CN105131747B (en) | A kind of environmentally-frieweak weak solvent type inkjet medium and preparation method thereof | |
| CN109266099A (en) | A kind of zirconium oxide ink-jet printing ink and the method for preparing zirconium oxide nano crystal film | |
| CN102071540A (en) | Gas sensor fiber membrane and preparation method thereof | |
| Soleimani-Gorgani et al. | In situ production of nano-CoAl2O4 on a ceramic surface by ink-jet printing | |
| Milanović et al. | Preparation of low cost alumina nanofibers via electrospinning of aluminium chloride hydroxide/poly (vinyl alcohol) solution | |
| CN105378895A (en) | Impurity-diffusing composition and method for producing semiconductor element | |
| CN107098700A (en) | A kind of high solids content BMN suspension inks printed suitable for direct write and preparation method thereof | |
| CN104987774A (en) | Preparation method of ZnO-based nano material ink-jet printing water-based ink | |
| JP6260990B2 (en) | Multi-component oxide semiconductor precursor coating solution and method for producing multi-component oxide semiconductor film using the coating solution | |
| CN104030689B (en) | A kind of preparation method of boride ultra-temperature pottery | |
| CN104080862B (en) | Ink, printing base, printing equipment, printing process, the manufacture method of printing base | |
| CN109130493A (en) | A method of improving ink-jet printing ink deposition uniformity | |
| CN109251587A (en) | A kind of method that gel template method prepares inkjet printing sull | |
| JP5871201B2 (en) | Method for producing conductive metal particles and conductive paste | |
| CN107620102B (en) | One kind (Gd1-xLnx)2(MoO4)3The direct preparation method of film | |
| CN107620101B (en) | One kind (La1-xLnx)2(MoO4)3The direct preparation method of film | |
| CN106548978B (en) | A kind of production method of functional graphic, array substrate and display device |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190125 |
|
| RJ01 | Rejection of invention patent application after publication |