CN102992644B - Method for keeping anatase nmTiO2 crystal form at 800 DEG C and application of anatase nmTiO2 crystal form on glass brick - Google Patents
Method for keeping anatase nmTiO2 crystal form at 800 DEG C and application of anatase nmTiO2 crystal form on glass brick Download PDFInfo
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Abstract
The invention relates to a method for keeping anatase nmTiO2 crystal form at the temperature of 800 DEG C, and a technology for coating an anatase nmTiO2 film on a glass brick. The method comprises the following steps: preparing a 0.10mol phosphoric solution; slowly adding 25.000g of anatase nmTiO2 powder with the grain size of 20-25 nanometers into a 150ml solution containing 26.90ml 0.10 Mol phosphoric acid under the full stirring, further stirring for 15minutes; completely pouring the phosphoric solution containing anatase nmTiO2 powder into a porcelain crucible, putting the crucible in a muffle, heating up slowly to 800 DEG C and carrying out heat preservation for half hour; cooling to room temperature of 20-30DEG C naturally to obtain anatase nmTiO2 powder containing phosphorus oxide; and coating the anatase nmTiO2 powder on the glass brick by using a screen printing technique. A test method for testing the photocatalytic function of the anatase nmTiO2 membrane on the glass brick is set, and the functional test is carried out through XRD (X-Ray Diffraction), electron microscope, photocatalytic decomposition organism, bacteriostasis and super hydrophilicity.
Description
Technical field
The present invention relates to a kind of at 800 DEG C of maintenance nanometer anatase titania (nmTiO
2) method of crystal formation.Particularly disperse anatase titanium dioxide nmTiO on building and ornament materials surface
2after, make it keep anatase titanium dioxide nmTiO at 800 DEG C
2the method of crystal formation and the application on plate glass thereof.
Background technology
Anatase titanium dioxide nmTiO
2a kind of environment-friendly materials with performances such as photocatalysis Decomposition organism, antibacterial, Superhydrophilics.
Utilize optical excitation anatase titanium dioxide nmTiO
2what generation photocatalysis promoted chemical reaction is to come from Tokyo University's engineering research in last century professor of section, Doctor of engineering rattan Mr. island, is referred to as at that time " rattan island effect ".From finding to spend so far for four more than ten years, countries in the world are to anatase titanium dioxide nmTiO
2the research of photocatalytic applications also further deep.
Result of study is found anatase titanium dioxide nmTiO
2photocatalyst is under near-ultraviolet light (sunlight or luminescent lamp etc.) irradiates, electronics in molecule is excited, generate electron-hole pair, because the hole of positively charged has very strong oxidation capacity, can make airborne water molecules generate the strong oxidizer of hydroxyl free radical (OH); Electronegative electronic energy makes airborne oxygen (O
2) reduction, generate another kind of strong living radical O
2-.OH and O
2-the energy that the contained energy equivalence of living radical produces in the heat energy of 3600K high temperature, is enough to make most of organic substances " burning " to decompose.So the organic molecules such as its can Decomposition of benzene, formaldehyde, anti-bacteria, and to human body without injury.
In prior art, carry out the nmTiO of anatase crystal type
2the following technology that is scattered in ceramic tile surface klining sizing of crystalline transformation temperature is attempted, referring to " ceramic tile glaze TiO in " Shanghai Institute Of Technology's journal "
2the preparation of material and structure and morphology research thereof "; With Chinese patent CN101143763B.
Plate glass (glass Mosaic) is as finishing material, and it has abundant color and comprises the pattern of the demonstration metal quality such as gold and silver.Pattern on plate glass is all to print on the plate glass that 8mm is thick by the method monochrome of silk screen printing or chromatography, then by 800 DEG C of (glass softening point temperature) klining sizings, adheres to and become a useful person.Due to anatase crystal type nmTiO
2the limitation of thermostability, in the time that temperature exceedes 600 DEG C, it can be transformed into the nmTiO of rutile-type
2thereby, lose photocatalysis characteristic.If reduce klining temperature, the metallic substance such as pigment and gold and silver that forms pattern color can not adhere to thick on glass of 8mm, certainly can not make needed plate glass.The character of glass do not allow yet through 800 DEG C of burnings once after, reburn once in 500-600 DEG C.First plate glass pattern is formed by a firing the temperature of 800 DEG C, then at plate glass surface coverage anatase crystal type nmTiO
2film, and again at the temperature of 500-600 DEG C, this plate glass is carried out to klining again.
If ensure that the plate glass (glass Mosaic) of making has good pattern, shape and optical characteristics, makes the nmTiO disperseing simultaneously
2film water white transparency also has photocatalysis performance, just must make the anatase titanium dioxide nmTiO covering on plate glass
2klining completes together with pattern, simultaneously anatase titanium dioxide nmTiO
2in the time of 800 DEG C, must keep crystal formation constant.
Can together stand 800 DEG C of klining and ensure anatase titanium dioxide nmTiO with plate glass in the urgent need to one now
2in the constant method of 800 DEG C of crystal formations and the technique applying on plate glass thereof.
Summary of the invention
The object of this invention is to provide a kind of anatase titanium dioxide nmTiO that ensures
2keep the method for crystal formations and the application on plate glass thereof at 800 DEG C, select the one can be prior to anatase titanium dioxide nmTiO
2the energy of absorbing radiation and shielding protection anatase titanium dioxide nmTiO
2the material of crystal formation, makes anatase titanium dioxide nmTiO
2in the time that shaping, plate glass klining can keep crystal formation constant.
It is suitable for shielding protection anatase titanium dioxide nmTiO to select from the physicochemical property of compound
2do not change the material of crystal formation 800 DEG C of left and right.The present invention selects the oxide compound of phosphorus as anatase titanium dioxide nmTiO by many experiments
2shielding protection material.
Containing the anatase titanium dioxide nmTiO of phosphorous oxides
2the preparation method of powder: with distilled water, analytical pure (AR) phosphoric acid preparation 0.10mol phosphoric acid solution.In the phosphate aqueous solution that the volume that contains the 0.10Mol concentration of 26.90ml is 150ml, under abundant agitation condition, slowly adding particle diameter is the anatase titanium dioxide nmTiO of 20-25nm
2powder 25.000g continues to stir 15 minutes after all adding, and will contain anatase titanium dioxide nmTiO
2the phosphate aqueous solution of powder is all poured in the sweet pot of porcelain, puts into retort furnace, is slowly warming up to 800 DEG C, is incubated half an hour, is naturally down to room temperature 20-30 DEG C, makes the anatase titanium dioxide nmTiO containing phosphorous oxides
2powder.
Every gram of anatase titanium dioxide nmTiO
2in the content of corresponding phosphorus reach 3.05-3.33mg and can ensure nmTiO
2crystal formation can not change rutile-type into by anatase titanium dioxide in the time of 800 DEG C.
When envrionment temperature is room temperature 20-25 DEG C, (diameter is Φ 1mm and Φ 2mm in 2000-2500ml silk screen printing solution, to add zirconium pearl, ratio is 4: 6) 50g, use sand milling dispersion machine under the stirring velocity of 2500-3000r/min, slowly to add the anatase titanium dioxide nmTiO containing phosphorous oxides
2powder 20-25g (± 0.000g), continuously stirring 30 minutes, elimination zirconium pearl, generates the anatase titanium dioxide nmTiO containing phosphorous oxides
2silk screen printing colloidal sol.The plate glass of 8mm thickness is carried out to oil removing dust removal process, with screen printer print anatase titanium dioxide nmTiO
2colloidal sol, thickness approximately 5 μ m, can select 165T or 200T silk screen according to print speed, treat that film surface drying can enter the klining system of 800 DEG C and pattern one co-shaping on plate glass surface after printing.
Anatase titanium dioxide nmTiO
2the crystal formation of powder is to be determined by X-ray diffracting spectrum (XRD).
The present invention has overcome anatase titanium dioxide nmTiO
2in the time of the klining sizing of plate glass surface, because klining temperature makes anatase titanium dioxide nmTiO up to 800 DEG C
2be transformed into rutile-type nmTiO
2cause the problem that loses photocatalysis performance, and complete processing is easy, processed finished products rate is high, does not produce the three wastes in production process, with low cost.
Brief description of the drawings:
Fig. 1 is anatase titanium dioxide nmTiO
2plate glass X-ray diffracting spectrum (XRD) detected result;
Fig. 2 is anatase titanium dioxide nmTiO
2plate glass electron microscope collection of illustrative plates;
Fig. 3 is anatase titanium dioxide nmTiO
2plate glass benzene decomposition curve;
Fig. 4 is anatase titanium dioxide nmTiO
2plate glass bacteriostatic test.
Fig. 5 measures nmTiO with contact angle measurement
2water droplet contact angle on plate glass;
Fig. 6 nmTiO
2plate glass Superhydrophilic experimental result.
Embodiment
One, preparation is containing the anatase titanium dioxide nmTiO of phosphorous oxides
2powder.
1. the material and the equipment that adopt
Particle diameter is the anatase titanium dioxide nmTiO of 20-25nm
2powder, determines nmTiO by X ray diffracting spectrum (XRD)
2crystal formation, by specific surface area 104-120m
2/ g proves particle diameter;
Phosphoric acid: analytical pure (AR);
Distilled water;
Retort furnace;
Electronic balance: ± 0.001g;
Volumetric flask;
Transfer pipet.
2. implementation step
With distilled water configuration 0.10mol phosphoric acid solution, when use, dilute again as required.
In the phosphoric acid solution of different concns, (press every gram of anatase titanium dioxide nmTiO
2the phosphorus content meter Pmg/nmTiO needing
2g) fully under agitation condition, slowly adding anatase titanium dioxide nmTiO
2powder continues to stir 15 minutes after all adding.To contain anatase titanium dioxide nmTiO
2the phosphoric acid solution of powder is all poured in the sweet pot of porcelain, puts into retort furnace.Slowly be warming up to 800 DEG C, be incubated half an hour.Naturally be down to room temperature 20-30 DEG C, take out product and carry out respectively X-ray diffracting spectrum (XRD) and specific surface detection.
Experimental Comparison one
By implementation step operation, in the phosphate aqueous solution 150ml of the 0.10mol containing 12.60ml, add 25.000g anatase titanium dioxide nmTiO
2powder (P1.56mg/nmTiO
2g),, after 800 DEG C of roasting half an hour, detect to have an appointment with X-ray diffracting spectrum (XRD) and 5% change into rutile-type nmTiO
2, specific surface 37.2m
2/ g.
Experimental Comparison two
By implementation step operation, in the phosphate aqueous solution 150ml of the 0.10mol containing 14.20ml, add 25.000g anatase titanium dioxide nmTiO
2powder (P1.76mg/nmTiO
2g),, after 800 DEG C of roasting half an hour, detect to have an appointment with X-ray diffracting spectrum (XRD) and 5% change into rutile-type nmTiO
2, specific surface 53.8m
2/ g.
Experimental Comparison three
By implementation step operation, in the phosphate aqueous solution 150ml of the 0.10Mol containing 24.60ml, add 25.000g anatase titanium dioxide nmTiO
2powder (P3.05mg/nmTiO
2g),, after 800 DEG C of roasting half an hour, detect and do not find rutile nmTiO with X-ray diffracting spectrum (XRD)
2, specific surface 104m
2/ g-110m
2/ g.
Experimental Comparison four
By implementation step operation, in the phosphate aqueous solution 150ml of the 0.10Mol containing 26.90ml, add 25.000g anatase titanium dioxide nmTiO
2powder (P3.33mg/nmTiO
2g),, after 800 DEG C of roasting half an hour, detect and do not find rutile nmTiO with X-ray diffracting spectrum (XRD)
2, specific surface 115m
2/ g-120m
2/ g.
3. conclusion (of pressure testing)
1) testing data providing according to above Experimental Comparison, known anatase titanium dioxide nmTiO
2phosphorous oxides in powder can be prior to anatase titanium dioxide nmTiO
2the energy of absorbing radiation, to anatase titanium dioxide nmTiO
2play shielding protection.
2) as every gram of anatase titanium dioxide nmTiO
2when the content of corresponding phosphorus reaches 3.05-3.33mg, anatase titanium dioxide nmTiO
2can be to rutile-type nmTiO in the time of 800 DEG C of high temperature
2change.
Two, by the phosphorous anatase titanium dioxide nmTiO of above-mentioned preparation
2be dispersed in plate glass surface, and this plate glass klining shaped:
Contain anatase titanium dioxide nmTiO
2the method that the plate glass of film is made of silk screen printing:
1) prepare silk screen printing solution.
Printing with solution material proportioning following (by weight, unit is g):
A) distilled water: 100;
B) Vltra tears: food grade, 2.6;
C) Virahol: technical grade, 30;
D) cyclodextrin: analytical pure (AR), 0.5;
E) ethylene glycol monobutyl ether: analytical pure (AR), 0.3;
Print with solution preparation program (carrying out under 20-25 DEG C of room temperature):
Vltra tears is dissolved in distilled water, be stirred to completely after dissolving and add Virahol with 2500-3000r/min speed with sand milling dispersion machine, continue to stir and successively add cyclodextrin, ethylene glycol monobutyl ether.By the solution left standstill configuring 12 hours, after solution is transparent, can use.
2) preparation is containing the anatase titanium dioxide nmTiO of phosphorous oxides
2silk screen printing colloidal sol.
Material and equipment:
A) containing the anatase titanium dioxide nmTiO of phosphorous oxides
2powder;
B) solution that silk screen printing is used;
C) sand milling dispersion machine SDF-400;
D) zirconium pearl mixture (diameter is Φ 1mm and Φ 2mm, and blending ratio is 4: 6);
Preparation is containing the anatase titanium dioxide nmTiO of phosphorous oxides
2silk screen printing colloidal sol
Envrionment temperature is that room temperature (20-25 DEG C) adds 50g zirconium pearl in 2000-2500ml silk screen printing solution, uses sand milling dispersion machine under the stirring velocity of 2500-3000r/min, slowly to add the anatase titanium dioxide nmTiO containing phosphorous oxides
2powder 20-25g, continuously stirring 30 minutes, elimination zirconium pearl, makes the anatase titanium dioxide nmTiO containing phosphorous oxides
2silk screen printing colloidal sol is for silk screen printing.
3) silk screen printing and the klining technique to plate glass
A) plate glass to be printed must carry out oil removing dust removal process, makes to print the dustless nothing oil in plate glass surface of nanometer film.
B) the thickness approximately 5 μ m of printing nanometer film, select 165T or 200T silk screen according to print speed.
C) can select manual, semi-automatic or automatic printing machine according to condition.
D) after printing, treat film surface drying, plate glass can enter klining system.
Three, the anatase titanium dioxide nmTiO of the plate glass surface coverage of klining sizing
2the Performance Detection of film: the anatase titanium dioxide nmTiO of plate glass (glass Mosaic) surface coverage
2five of the total X-ray diffracting spectrum (XRD) of the Performance Detection of film, electron microscope, photocatalysis Decomposition organism-benzene, antibacterial, Superhydrophilics etc.
The preparation of check sample
Five check samples be unified preparation containing anatase titanium dioxide nmTiO
2printing colloidal sol and typography printing, the thick plate glass of 8mm of making through 800 DEG C of klining.During for disparity items inspection, need do different treatment to sample.
1. inspection embodiment mono-: X-ray diffracting spectrum (XRD) inspection
Thick 8mm 20 × 50 plate glasss are milled to 0.1-0.3mm thick, are broken to powdery with ball mill, for X-ray diffracting spectrum (XRD) inspection, the results are shown in accompanying drawing 1:
2. inspection embodiment bis-: scanning electronic microscope inspection
To apply anatase titanium dioxide nmTiO
2the plate glass of powder is cut into the microscopical determination of 20 × 50mm supplied for electronic, the results are shown in Figure 2:
3. inspection embodiment tri-: the inspection of decomposing organic matter-benzene
According to anatase titanium dioxide nmTiO
2absorb luminous energy and produce the reaction mechanism that hydroxyl free radical decomposes organic molecule.Can be by this method as scribbling anatase titanium dioxide nmTiO
2the main test method of plate glass product function and quality.
Because benzene has good conjugated structure, decompose the energy that its needs is larger.So can use it as the organic target compound of inspection photocatalysis Decomposition.
This inspection is benzene vapour static check, will apply anatase titanium dioxide nmTiO
2plate glass 150*150*8mm is placed in closed reactor (220 × 220 × 30mm), and reactor sensitive surface is silica glass (220 × 220 × 3mm) illumination parameter: wavelength 385nm, light intensity 0.15mW/cm
2.
This light-catalyzed reaction is the anatase titanium dioxide nmTiO on plate glass
2the hydroxyl free radical that absorbs luminous energy generation reacts with benzene molecular.Reaction is at anatase titanium dioxide nmTiO
2carry out at the interface of particle, and when reaction conditions is fixed, in reactor, organic molecule is the important factor that impact reaction is carried out to plate glass surface diffusion speed.Will produce the small molecules after cracking when benzene molecular starts cracking, they and benzene molecular exist simultaneously.At this moment in reactor, be the gas of a mixing, because benzene molecular quality is relatively large, so and nmTiO
2interface contact probability must reduce.The decomposition of benzene also must be slow by easing up.Therefore this inspection can illustrate and apply anatase titanium dioxide nmTiO
2plate glass has the function of decomposing organic matter.Blank sample survey, removes on plate glass without anatase titanium dioxide nmTiO
2outward, other condition for surveyss are identical.
Checking procedure: the reactor that plate glass to be tested is housed is placed in to the thermostat of 100 DEG C ± 1 DEG C, (reactor benzene vapour concentration is about 8.3 × 10 to inject 10 μ l benzene in reactor
-3mg/cm
3), balance started irradiation after 14 hours.After stabilized intensity, start sampling (C
0), later every one hour once (C of sampling
t), get three parallel sample at every turn, detected the degraded of benzene by GC-9800 gas chromatograph.Inspection is not to apply anatase titanium dioxide nmTiO
2blank glass brick compare.The results are shown in Figure 3:
4. inspection embodiment tetra-: bacteriologic test
Detect with equipment, reagent and bacterial classification: culture dish, magnificent test tube, suction pipe, phosphoric acid buffer, basic medium, soft agar, golden yellow staphylococcus (ATCC), intestinal bacteria (ATCC)
Detection method: golden yellow staphylococcus, 24 hours broth cultures of intestinal bacteria are diluted into about 200 bacterium/plates with phosphoric acid buffer, drawing bacterium liquid and soft agar mixes, water through UV-lamp (30w, apart from 48cm) irradiate (be respectively 2 minutes, 4 minutes, 8 minutes, after 16 minutes) scribble anatase titanium dioxide nmTiO
2on glass, culture dish is put in 37 DEG C of constant incubators and is cultivated 24 hours, counting bacterium number.Assay is shown in Fig. 4:
Conclusion: after UV-lamp is irradiated, experimental group plate glass is better to golden yellow staphylococcus, intestinal bacteria fungistatic effect, irradiates and has effect in 2 minutes, and bacteriostasis rate reaches 80%.Irradiate after 4 minutes effect more obvious; And blank group poor to golden yellow staphylococcus, intestinal bacteria fungistatic effect, bacterial number reduces slightly.
5. inspection embodiment five: Superhydrophilic inspection
Inspection machine: contact angle measurement-JC2000C1
Measure nmTiO with contact angle measurement
2water droplet contact angle on plate glass, referring to Fig. 5:
Checking procedure: get and apply anatase titanium dioxide nmTiO
2some of plate glass 50 × 50 × 8mm, are positioned over respectively wavelength 385nm, light intensity 0.15mW/cm
2illumination 90,180,270 minutes under condition.Then measure water droplet contact angle on plate glass with contact angle measurement, the results are shown in Figure 6:
Although illustrate by way of example above-mentioned, described the embodiment of the best of the present invention, protection scope of the present invention is not limited in above-mentioned explanation, uses method of the present invention to make anatase titanium dioxide nmTiO
2be attached to the body surface (as glassware etc.) that need to fire and play fungistatic effect; persons skilled in the art are understandable that; do not deviating under the prerequisite of essence that the present invention instructs and marrow, any modifications and variations all fall into protection scope of the present invention.
Claims (2)
1. one kind keeps anatase titanium dioxide nmTiO at 800 DEG C
2the method of crystal formation, anatase titanium dioxide nmTiO
2in powder systems, have phosphorous oxides, described phosphorous oxides is by by anatase titanium dioxide nmTiO
2powder is placed in phosphoric acid solution and fires and form at 800 DEG C, every gram of anatase titanium dioxide nmTiO
2need the content of phosphorus to be not less than 3.05mg; Described phosphoric acid solution is taken 0.10mol phosphoric acid and is done basis; Preparation is containing the anatase titanium dioxide nmTiO of phosphorous oxides
2in process, by nmTiO
2amount calculate the consumption of the required phosphoric acid solution of content of phosphorus; It is characterized in that: utilize every gram of anatase titanium dioxide nmTiO
2in powder, the phosphorous oxides of corresponding content keeps anatase titanium dioxide nmTiO
2thermostability, use distilled water, AR level phosphoric acid preparation 0.10mol phosphate aqueous solution, in the phosphate aqueous solution of the 0.10Mol concentration containing 26.90ml, fully under agitation condition, slowly add anatase titanium dioxide nmTiO
2powder continues to stir 15 minutes after all adding, and will contain anatase titanium dioxide nmTiO
2the phosphate aqueous solution of powder is all poured in porcelain crucible, puts into retort furnace, is slowly warming up to 800 DEG C, is incubated half an hour, is naturally down to room temperature 20-30 DEG C, makes the anatase titanium dioxide nmTiO containing phosphorous oxides
2powder, the described anatase titanium dioxide nmTiO containing phosphorous oxides
2powder can keep anatase titanium dioxide nmTiO
2under 800 DEG C of states, crystal formation is constant; The volume of described phosphate aqueous solution is 150ml, described in the anatase titanium dioxide nmTiO that adds
2the quality of powder is 25.000g; Described anatase titanium dioxide nmTiO
2the particle diameter of powder is 20-25nm, and specific surface area is 104-120m
2/ g; Described anatase titanium dioxide nmTiO
2the crystal formation of powder is determined by X-ray diffracting spectrum XRD; The phosphorous oxides of described corresponding content is every gram of anatase titanium dioxide nmTiO
2in the content of corresponding phosphorus reach 3.05-3.33mg.
2. the anatase titanium dioxide nmTiO containing phosphorous oxides
2the application of powder on plate glass, it is characterized in that: when envrionment temperature is room temperature 20-25 DEG C, in 2000-2500ml silk screen printing solution, add appropriate zirconium pearl, use sand milling dispersion machine under the stirring velocity of 2500-3000r/min, slowly to add the anatase titanium dioxide nmTiO containing phosphorous oxides manufacturing as the method in claim 1
2powder, and continue to stir 30 minutes, elimination zirconium pearl, forms the anatase titanium dioxide nmTiO containing phosphorous oxides
2silk screen printing colloidal sol; The plate glass of 8mm thickness is carried out to oil removing dust removal process, and the thickness approximately 5 μ M of printing nanometer film, select 165T or 200T silk screen according to print speed, treat that film surface drying can enter the klining formulation type of 800 DEG C after printing; Described zirconium pearl diameter is Φ 1mm and Φ 2mm, and zirconium pearl usage ratio is 4: 6, and add-on is 50g.
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Effective date of registration: 20130724 Address after: 100081, No. 21, building 1, No. 12, Zhongguancun South Avenue, Beijing, Haidian District, 2511 Applicant after: RUIFU JINGFENG (BEIJING) TECHNOLOGY CO., LTD. Address before: 100192 Beijing city Haidian District Junan home small business Qinghe East 4-906 room Applicant before: Xu Boyu |
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