CN105860955B - A kind of preparation method for indehiscent titanium oxide film layer of being heated - Google Patents
A kind of preparation method for indehiscent titanium oxide film layer of being heated Download PDFInfo
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- CN105860955B CN105860955B CN201610193273.1A CN201610193273A CN105860955B CN 105860955 B CN105860955 B CN 105860955B CN 201610193273 A CN201610193273 A CN 201610193273A CN 105860955 B CN105860955 B CN 105860955B
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 13
- 239000011521 glass Substances 0.000 claims abstract description 11
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 23
- 239000007788 liquid Substances 0.000 claims description 19
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 15
- 235000019441 ethanol Nutrition 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 2
- 238000007654 immersion Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims 1
- 239000010410 layer Substances 0.000 description 23
- 238000000034 method Methods 0.000 description 8
- 239000000243 solution Substances 0.000 description 7
- 238000005253 cladding Methods 0.000 description 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 239000005357 flat glass Substances 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- 241000790917 Dioxys <bee> Species 0.000 description 1
- 206010021703 Indifference Diseases 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010835 comparative analysis Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 125000005909 ethyl alcohol group Chemical group 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- -1 titanium dioxide Titanium forms lactone Chemical class 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Classifications
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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
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
- C03C17/23—Oxides
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/21—Oxides
- C03C2217/212—TiO2
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Luminescent Compositions (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Surface Treatment Of Glass (AREA)
Abstract
The invention discloses a kind of preparation method for indehiscent titanium oxide film layer of being heated, including following steps connected in order：1) collosol and gel titanium dioxide, is prepared；2) hydrothermal synthesis；3) it forms a film.The preparation method of the heated indehiscent titanium oxide film layer of this present invention can form room temperature on the surfaces such as fluorescent powder and glass and have stable high-temperature performance, uniformly indehiscent film layer, and preparation is simple.
Description
Technical field
The present invention relates to a kind of preparation methods for indehiscent titanium oxide film layer of being heated, and belong to superficial film technology of preparing
Field.
Background technology
Layer of transparent conductive material is formed on fluorescent powder grain surface using cladding process, can both improve electric conductivity, alleviate electricity
Saturation effect is flowed, but also as protective layer, improves resist degradation performance.It is seldom about the research work of this respect both at home and abroad.2005
Year Sang-Do Han etc., for El element, sol-gel method was used and in nitrogen at heat using tetraisopropyl titanate as presoma
Reason is in ZnS:Cu, Cl surface have coated TiO2, have studied the relationship of luminescence generated by light and electroluminescent properties and experiment condition.2007
Year Lihong Xue etc. uses the sol-gal process comprising butyl titanate hydrolytic polymerization process and through being made annealing treatment in argon gas,
ZnS:Cu, Au, Al surface have coated the TiO of 20-54nm2, and solution concentration, powder amount and reaction time are had studied to coating thickness
Influence.Chen Ping in 2010 is waited clearly using butyl titanate as raw material and is coated Ti0 in ZnS phosphor surfaces using sol-gel method2
(not being calcined), and have studied cladding after photoluminescent property, but the above method there are experiment condition it is very harsh the defects of,
Requirement of experiment is not achieved in common laboratory at all, it is more difficult to implement on a large scale in enterprise, and film layer obtained by the above method exists
Drying property is unstable, dry with it is easy to crack in thermal histories the defects of.
Invention content
Experiment condition harshness is formed, and the titanium oxide film layer of gained exists to solve titanium oxide film layer in the prior art
The defects of drying property is unstable under naturally dry or heating condition in air, easy cracking, the present invention provide it is a kind of it is heated not
The preparation method of the titanium oxide film layer of cracking.
In order to solve the above technical problems, the technical solution adopted in the present invention is as follows：
A kind of preparation method for indehiscent titanium oxide film layer of being heated, including following steps connected in order：
1) collosol and gel titanium dioxide is prepared：By the acetic acid of 0.9-1.1 parts of volumes and the distilled water of 1.4-1.6 parts of volumes according to
A liquid is stirred and evenly mixed to obtain in the secondary ethyl alcohol for adding in 9-11 parts of volumes；Positive four butyl ester of the metatitanic acid of 4-5 parts of volumes is added in into 9-11 parts of volumes
Ethyl alcohol in stir and evenly mix to obtain B liquid；B liquid is instilled with 2-3 drops/sec of speed in A liquid, light blue solution is formed, stands 22-
26h；
2) hydrothermal synthesis：Mixed liquor obtained by step 1) is put into hydrothermal synthesis tank, in a manner that every 5 minutes rise 4-6 DEG C
After being warming up to 155-165 DEG C, Heat preservation 15-17h, natural cooling, and by resulting material ethyl alcohol centrifuge washing, stay upper liquid
It is spare；
3) it forms a film：The fluorescent powder that is wrapped by or glass will be needed to be put into the upper liquid that step 2) is stayed, impregnate, lift into
Film, drying are to get heated indehiscent titanium oxide film layer.
Film layer room temperature, heat preservation are not cracked obtained by the above method, and performance is stablized, and uniformity is good.
In step 3) drying can dry under field conditions (factors) or baking oven heating condition under it is dry；Immersion, pulling film forming are specific
For method with reference to the prior art, operation temperature is room temperature (15-30 DEG C).
In order to further improve gained film layer stability, it is preferable that in step 1), by the acetic acid of 0.9-1.1 part volumes with
The distilled water of 1.4-1.6 parts of volumes sequentially adds the item that low whipping speed in the ethyl alcohol of 9-11 parts of volumes is 3800-4000r/min
Under part, stir 9-11 minutes, obtain A liquid.In step 1), positive four butyl ester of the metatitanic acid of 4-5 parts of volumes is added in the second of 9-11 parts of volumes
Low whipping speed is under conditions of 3800-4000r/min, stirs 9-11 minutes, obtains B liquid in alcohol.
In order to further improve the stability of gained film layer, in step 2), centrifuge washing 2 times, centrifugal rotational speed 3800-
4000r/min, a centrifugation time are 7-9min.
The titanium dioxide prepared using the application above method not only can form good clad in phosphor surface,
Stablize in the cladding film layer same performance that glass surface is formed, do not crack uniformly.
The unmentioned technology of the present invention is with reference to the prior art.
The preparation method of the heated indehiscent titanium oxide film layer of the present invention, can form on the surfaces such as fluorescent powder and glass
It room temperature and has stable high-temperature performance, uniform indehiscent film layer, and preparation is simple.
Description of the drawings
Fig. 1 is that the scanning electron microscope (SEM) photograph in phosphor surface cladding titanium dioxide, drying means are with the application preparation method
Baking oven heat drying；
Fig. 2 is the scanning electron microscope (SEM) photograph in glass surface cladding titanium dioxide with the application preparation method, and drying means is dries
Case heat drying；
Fig. 3 is in the scanning electron microscope (SEM) photograph of glass surface cladding titanium dioxide with the application preparation method, and drying means is normal
It is stood in warm air.
Specific embodiment
For a better understanding of the present invention, with reference to the embodiment content that the present invention is furture elucidated, but the present invention
Content is not limited solely to the following examples.
Embodiment 1
1. preparation work：Beaker, glass bar, graduated cylinder are taken, is dried with baking oven；Stir magneton soaking and washing in alcohol；It is dry
Net sheet glass, with hydrofluoric acid dips 4min, taking-up is rinsed well with deionized water, spare.
2. prepare collosol and gel titanium dioxide
2 beakers is taken to be separately added into 10.00mL ethyl alcohol, marked as A, B, are sequentially added in A beakers with rubber head dropper
1.00mL acetic acid, 1.50mL distilled water, then low whipping speed is under conditions of 3900r/min, stirs 10 minutes；In B beakers
Middle addition positive four butyl ester of 4.50mL metatitanic acids, then low whipping speed is under conditions of 3900r/min, stirs 9-11 minutes；B is burnt
Solution is added in 3 drops/sec of speed in A beakers dropwise in cup, and after being added dropwise, room temperature magnetic agitation stirring 30min is formed light
Blue solution is stood for 24 hours.
3. hydrothermal synthesis is handled
Above-mentioned mixed liquor is divided into two parts, is tested as a comparison, portion does not do hydrothermal synthesis processing, stands 16h, dilution is simultaneously
It is centrifuged, centrifuge speed setting 3900r/min, 8min centrifuge 2 times, stay upper liquid spare；Another is put into
In hydrothermal synthesis tank, 160 DEG C, continuous heating 16h are warming up in a manner that every 5 minutes rise 5 DEG C, is taken out after natural cooling, it will be molten
Liquid is washed with ethyl alcohol, and centrifuge speed setting 3900r/min, 8min centrifuge 2 times, stay upper liquid spare.
4. Film forming operations
The sheet glass that hydrofluoric acid treatment is crossed is put into the titania solution without hydrothermal synthesis in 25-30 DEG C of temperature model
It encloses and impregnates 3min, then film balance forms sample 1 with the even speed pulling film forming of 0.70mm/min；The glass that will equally handle
Glass piece is put into the titania solution after hydrothermal synthesis impregnates 3min in 25-30 DEG C of temperature range, then film balance with
The even speed pulling film forming of 0.70mm/min forms sample 2.
1) sample 1,2 is statically placed at ambient temperature in air, observes the state and stability of its film layer afterwards for 24 hours.
2) sample 1,2 is respectively put into different clean beakers, be placed in baking oven, by oven temperature since room temperature,
5 DEG C are increased with every 5min, not more than 250 DEG C, observes the state and stability of its film layer after cooling for 24 hours.
5. comparative analysis
It is preferable in the film quality that glass surface is formed by the titanium dioxide of collosol and gel shape after hydrothermal synthesis is handled,
Indifference is estimated with film layer character in the state of oven drying spontaneously drying, under the microscope without slight crack, is not fallen off, explanation
Membranous layer property is highly stable reliable, and gained film layer is highly uniform.Possible cause is：Hydrothermal synthesis handles so that titanium dioxide
Titanium forms lactone shape, in this process collosol and gel progress secondary response, structure rearrangement, particle smaller, at this time dioxy
Change titanium property states to have stablized, external environment will not have an impact film layer in use.Without passing through hydrothermal synthesis
Then visual homogeneity is significantly worse than sample 2 to the film layer of gained, and has the phenomenon that protrusion and crackle after the red drying of baking oven.
Embodiment 2
With being that embodiment 1 is essentially identical, except that：It forms a film in phosphor surface, gained even film layer does not crack.
Claims (2)
1. a kind of preparation method for indehiscent titanium oxide film layer of being heated, it is characterised in that：Including following step connected in order
Suddenly：
1) collosol and gel titanium dioxide, is prepared：By the acetic acid of 0.9-1.1 parts of volumes and the distilled water of 1.4-1.6 parts of volumes successively
It adds in the ethyl alcohol of 9-11 parts of volumes and stirs and evenly mixs to obtain A liquid；By the metatitanic acid of 4-5 parts of volumes 9-11 parts of volumes of positive four butyl esters addition
B liquid is stirred and evenly mixed to obtain in ethyl alcohol；B liquid is instilled with 2-3 drops/sec of speed in A liquid, light blue solution is formed, stands 22-26h；
2) hydrothermal synthesis：Mixed liquor obtained by step 1) is put into hydrothermal synthesis tank, is heated up in a manner that every 5 minutes rise 4-6 DEG C
To after 155-165 DEG C, Heat preservation 15-17h, natural cooling, and by resulting material ethyl alcohol centrifuge washing, stay upper liquid standby
With；
3) it forms a film：The fluorescent powder that is wrapped by or glass will be needed to be put into the upper liquid that step 2) is stayed, immersion, pulling film forming,
Drying is to get heated indehiscent titanium oxide film layer；
In step 1), the distilled water of the acetic acid of 0.9-1.1 parts of volumes and 1.4-1.6 parts of volumes is sequentially added into 9-11 parts of volumes
Low whipping speed is under conditions of 3800-4000r/min, stirs 9-11 minutes, obtains A liquid in ethyl alcohol；
In step 1), it is 3800- that positive four butyl ester of the metatitanic acid of 4-5 parts of volumes is added in low whipping speed in the ethyl alcohol of 9-11 parts of volumes
Under conditions of 4000r/min, stir 9-11 minutes, obtain B liquid.
2. the preparation method for indehiscent titanium oxide film layer of being heated as described in claim 1, it is characterised in that：Step 2)
In, centrifuge washing 2 times, centrifugal rotational speed 3800-4000r/min, a centrifugation time is 7-9min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610193273.1A CN105860955B (en) | 2016-03-30 | 2016-03-30 | A kind of preparation method for indehiscent titanium oxide film layer of being heated |
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| CN201610193273.1A CN105860955B (en) | 2016-03-30 | 2016-03-30 | A kind of preparation method for indehiscent titanium oxide film layer of being heated |
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| CN105860955B true CN105860955B (en) | 2018-06-26 |
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| CN101698937B (en) * | 2009-09-25 | 2011-05-11 | 湖北大学 | Preparation method of columnar monocrystal nano-TiO2 array film |
| CN102617044B (en) * | 2012-03-05 | 2014-08-06 | 湖北大学 | Method for preparing vertical orientation anatase titanium oxide film by using hydrothermal method and gas sensor thereof |
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