CN104030345A - Method for preparing different colors of mixed phase nano TiO2 - Google Patents
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Abstract
The invention relates to a method for preparing different colors of mixed phase nano TiO2. The key technology is carrying out thermal treatment on amorphous nano TiO2 which is synthesized by a water phase in one step at different temperature. The method concretely comprises the following steps: firstly, mixing and reacting a Ti(SO4)2 solution and ammonia water under an ice-water bath condition to obtain amorphous hydrate sol of TiO2, centrifugally washing, and then evaporating the sol at low temperature, so as to obtain amorphous phase nano TiO2; respectively carrying out thermal treatment on evaporated amorphous phase nano TiO2 solid at different temperature, so as to obtain different colors of amorphous and anatase mixed-phase nano TiO2. A series of different colors of mixed phase nano TiO2 can be prepared by adopting a gradient heat treatment method for the first time. The method is simple to operate, available in raw materials, low in cost and friendly to environment. Continuous regulation of an energy band structure is achieved by the prepared different colors of mixed phase nano TiO2, and the mixed phase nano TiO2 has excellent performances and positive significance in photocatalytic degradation of organic pollutants, and has a good application prospect.
Description
Technical field
The invention belongs to the preparation field of metal oxide functional material, particularly a kind of mixed phase nano-TiO of different colours
2preparation method.
Background technology
Nano-TiO
2be a kind of novel inorganic functional materials, there is unique performances such as specific surface area is large, surfactivity is high, absorbing properties is good.Nano-TiO
2valuable optical property makes it all demonstrate good development prospect in automotive industry and numerous areas.Nano-TiO
2also there is very high chemical stability, thermostability, nontoxicity, Superhydrophilic, non-migrating, and completely can with Food Contact, so be widely used in anti-ultraviolet material, weaving, photochemical catalysis catalyst, glass with clean, sunscreen, coating, ink, packaging material for food, paper industry, space industry, lithium cell.
Organic solvent mutually in synthesis of nano TiO
2, nanoparticle is adsorbed on organic macromolecule, and sluggish occurs, and is conducive to like this growth to particle in reaction process and controls, and obtains the nanocrystal of required desirable pattern, and therefore major part is synthesized TiO at present
2method how much all can be with an organic solvent.But the method often produces malicious byproduct, simultaneously because nanocrystal and the macromolecular combination of organism make the synthetic subsequent disposal of nanocrystal become complicated.And employing water synthesis of nano TiO
2method, easy and simple to handle, with low cost, toxic side effect is little, subsequent disposal is simple, but more difficult to the control ratio of product structure, at present the synthetic TiO of water
2because broad application prospect, receives increasing concern.
Anatase-phase nano TiO
2as a kind of optical function material, it is mainly employed photocatalyst.But common anatase octahedrite nano-TiO
2because energy gap is more than 3.3eV, only under the ultraviolet excitation that only accounts for solar radiation 5%, could produce transition of electron, lower to the efficiency of light energy utilization, and also light induced electron hole is fast to association rate, and all can be to nano-TiO
2photocatalytic activity exert an influence.For this problem, domestic and international many various terms of settlement of having researched and proposed, comprise to TiO
2in mix the impurity such as C, N, S, to TiO
2carry out hydrogen treatment and introduce grain surface nonsequential bed etc.These methods are to nano-TiO
2structure reinvent, what have can improve its photocatalytic activity really, but has all passed through more complicated step, and experiment condition is very harsh, natural cost is high.
Thermal treatment is as a kind of conventional means, to TiO
2modification in also have extensive utilization, but generally all just choose a specified temp (mostly being 400 DEG C-500 DEG C), as a transition step in experimentation, the not variation meeting nano-TiO synthetic to water of the simple thermal treatment temp of systematic study
2what kind of impact sample produces.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of mixed phase nano-TiO of different colours
2preparation method.
The technical solution used in the present invention is:
the mixed phase nano-TiO of a series of different colours
2, they are by the white armorphous nano TiO to after water one-step synthesis
2carry out obtaining after the thermal treatment of differing temps, described mixed phase is amorphous and anatase octahedrite mixed phase, and thermal treatment temp is higher, and unformed phase proportion is lower.
Described water one-step synthesis is titanium sulfate solution and ammoniacal liquor single step reaction in water.
Described thermal treatment temp is 200-800 DEG C, processes the pressed powder that obtains comprising palm fibre, Huang, ash, white colour under differing temps.
When described thermal treatment temp is 700 DEG C, the mixed phase nano-TiO obtaining
2under solar irradiation, there is the highest photocatalytic activity.
When described thermal treatment temp is 600 DEG C, the mixed phase nano-TiO obtaining
2under shining, visible ray there is the highest photocatalytic activity.
Nano-TiO
2energy gap with thermal treatment temp raise increase, specific surface area with thermal treatment temp raise reduce.
Concrete steps are:
1) under ice-water bath condition, titanium sulfate solution and ammoniacal liquor are joined in deionized water, this single step reaction, through being uniformly mixed 2h, obtains TiO
2the colloidal sol of unformed hydrate;
2) colloidal sol centrifugation step 1) being obtained, solid precipitation deionized water wash;
3) by step 2) in washing after colloidal sol evaporate to dryness at low temperatures, obtain white armorphous nano TiO
2solid, passes through respectively heat treatments at different, obtains the mixed phase nano-TiO of different colours
2.
In step 1), the concentration of titanium sulfate solution is 8.0g/100mL, and the concentration of ammoniacal liquor is 4mol/L, and the pH of reaction system maintains 9-10.
Step 2) middle at least 5500rpm of centrifugation rate, more than washing time 20min.
Low temperature evaporate to dryness described in step 3) is 60-80 DEG C of constant temperature evaporate to dryness in air dry oven, then the solid of evaporate to dryness is put into retort furnace, respectively at 200 DEG C, 300 DEG C, 400 DEG C, 500 DEG C, 600 DEG C, 700 DEG C and 800 DEG C of thermal treatment 3h, 10 DEG C/min of temperature rise rate, obtains the mixed phase nano-TiO of different colours
2.
Beneficial effect of the present invention: adopted first gradient temperature heat-treating methods, to the white armorphous nano TiO of water one-step synthesis
2crystallization degree control, obtained the unformed of different colours and anatase octahedrite mixed phase nano-TiO
2, along with thermal treatment temp raises, nano-TiO
2degree of crystallinity increase, color shoals gradually.The method preparation technology is simple, with low cost, and experimental result shows, TiO
2the hydroxyl of nanocrystal surface is the major reason that causes crystalline structure unordered.Unformed TiO
2hydroxy radical content is large, causes band curvature, and energy gap is narrowed.Thermal treatment temp is higher, and hydroxyl is sloughed with the form of water gradually, TiO
2changed to the anatase octahedrite of complete rule by height disordering, band curvature fades away, thereby has realized nano-TiO
2structure and the continuous regulation and control that can be with.TiO after thermal treatment
2photoabsorption enhancing in the scope of visible and near infrared light, consistent with the result of different colours in their macroscopic views and band curvature.Nano-TiO prepared by heat treatments at different
2aspect photocatalysis degradation organic contaminant, there is different activity, wherein 700 DEG C of heat treated TiO
2there is the highest sunlight catalytic activity; 600 DEG C of heat treated TiO
2have the highest visible light catalysis activity, this method is prepared good photocatalyst material, efficient extn nano-TiO
2range of application.
Brief description of the drawings
Fig. 1 is the different colours nano-TiO that thermal treatment obtains
2sample photo;
Fig. 2 is the different colours mixed phase nano-TiO that thermal treatment obtains
2xRD figure spectrum.Collection of illustrative plates shows along with thermal treatment temp raises, nano-TiO
2anatase degree of crystallinity increase;
Fig. 3 is the different colours mixed phase nano-TiO that thermal treatment obtains
2part HRTEM photo: (a) before thermal treatment; (b) 200 DEG C of thermal treatments; (c) 400 DEG C of thermal treatments; (d) 800 DEG C of thermal treatments.Photo shows along with thermal treatment temp raises, nano-TiO
2occur being grown up by unformed middle Anatase crystal forming core mutually, until the process that all unformed phases are all replaced by regular lattice;
Fig. 4 is the different colours mixed phase nano-TiO that thermal treatment obtains
2o 1s XPS collection of illustrative plates: (a) before thermal treatment; (b) 200 DEG C of thermal treatments; (c) 400 DEG C of thermal treatments; (d) 500 DEG C of thermal treatments; (e) 600 DEG C of thermal treatments; (f) 700 DEG C of thermal treatments; (g) 800 DEG C of thermal treatments; .The Gaussian peak that is positioned at 530eV after collection of illustrative plates swarming represents Ti-O key, and another Gaussian peak represents Ti-OH key, and peak area size shows along with thermal treatment temp raises, mixed phase nano-TiO
2the ratio of middle Ti-O/Ti-OH is by increase, and anatase octahedrite crystallization phases increases gradually with the ratio of unformed phase;
Fig. 5 is the different colours mixed phase nano-TiO that thermal treatment obtains
2part ultraviolet-visible absorption spectroscopy.Collection of illustrative plates shows the nano-TiO that color is darker
2, have more visible absorption and larger band curvature.Thermal treatment temp is higher, the nano-TiO obtaining
2energy gap is larger, and visible absorption is less.Dotted line represents 400 DEG C of heat treated nano-TiOs
2the position of the interband energy level producing;
Fig. 6 is the different colours mixed phase nano-TiO that thermal treatment obtains
2part VB XPS collection of illustrative plates.Collection of illustrative plates shows to be subject to the impact of mixed phase structure, nano-TiO
2top of valence band position can there is blue shift, cause band curvature, energy gap is narrowed.In figure, mark the position of the magnetic tape trailer of top of valence band and band curvature formation;
Fig. 7 is the different colours mixed phase nano-TiO that thermal treatment obtains
2part energy band structure schematic diagram.White TiO before thermal treatment
2only has discrete energy level, the TiO after thermal treatment
2have band curvature and interband energy level in various degree, along with thermal treatment temp raises, the magnetic tape trailer that can be with is less, and energy gap is larger;
Fig. 8 a is the different colours mixed phase nano-TiO that thermal treatment obtains
2degradation curve at xenon lamp simulated solar irradiation to the acid fuchsine solution;
Fig. 8 b is the different colours mixed phase nano-TiO that thermal treatment obtains
2add the degradation curve to the acid fuchsine solution under spectral filter simulation visible light catalytic at xenon lamp simulated solar irradiation.
Collection of illustrative plates shows that the ratio regular meeting of anatase octahedrite and unformed phase is to nano-TiO
2photocatalytic activity impact, but be not monotone variation, 700 DEG C of mixed phase nano-TiOs that thermal treatment obtains
2under solar irradiation, there is the highest photocatalytic activity.And 600 DEG C of mixed phase nano-TiOs that thermal treatment obtains
2under visible ray shines, there is the highest photocatalytic activity, illustrate that amorphous phase is more conducive to nano-TiO
2visible light catalysis activity, and by adjust thermal treatment temp, can obtain our required desired light catalytic material.
Embodiment
Below in conjunction with embodiment, the present invention is elaborated.
embodiment 1
Under ice-water bath condition, toward the 8.0g/100mL titanium sulfate solution and the 4mol/L ammoniacal liquor that add respectively 12mL and 20mL to prepare in 100mL deionized water, reaction system magnetic agitation 2h; By centrifugal the colloidal sol after stirring, solid precipitation deionized water supersound washing; Get the colloidal sol after 100mL washing, the dry white nano-TiO obtaining before thermal treatment at 80 DEG C
2solid (Fig. 1).This nano-TiO
2belong to unformed shape (Fig. 2), do not form crystalline structure (a part of Fig. 3), microtexture is TiO
6octahedral aggregate, according to quantum size effect, this TiO
2only have discrete energy level, do not possess quasi-continuous energy band structure, therefore very large (Fig. 7) of energy gap.Its specific surface area size is up to 328.55m
2/ g, therefore has very strong adsorption to the organism in solution, but because crystallinity is very poor, energy gap is large, almost there is no photocatalytic activity.Be applicable to doing sorbent material instead of photocatalyst.
embodiment 2
Under ice-water bath condition, toward the 8.0g/100mL titanium sulfate solution and the 4mol/L ammoniacal liquor that add respectively 12mL and 20mL to prepare in 100mL deionized water, reaction system magnetic agitation 2h; By centrifugal the colloidal sol after stirring, solid precipitation deionized water supersound washing; Get the colloidal sol after 100mL washing, at 80 DEG C, be dried and obtain white nano-TiO
2solid, then processes 3h by its constant temp. heating at 200 DEG C, obtains brown mixed phase nano-TiO
2(Fig. 1).This nano-TiO
2major part belongs to unformed shape (Fig. 2), and Anatase crystal starts forming core, the b part of median size 1.44nm(Fig. 3 simultaneously), specific surface area size reaches 281.88m
2/ g.This TiO
2there is high and the most continuous visible absorption (Fig. 5), therefore have maximum band curvature, cause its energy gap the narrowest (Fig. 7).This product also has certain adsorptive power, but because degree of crystallinity is also very poor, photocatalytic activity is not high, is not very desirable to the degraded of organic solution.
embodiment 3
Under ice-water bath condition, toward the 8.0g/100mL titanium sulfate solution and the 4mol/L ammoniacal liquor that add respectively 12mL and 20mL to prepare in 100mL deionized water, reaction system magnetic agitation 2h; By centrifugal the colloidal sol after stirring, solid precipitation deionized water supersound washing; Get the colloidal sol after 100mL washing, at 80 DEG C, be dried and obtain white nano-TiO
2solid, then processes 3h by its constant temp. heating at 400 DEG C, obtains Yellow nanometer TiO
2(Fig. 1).This nano-TiO
2belong to anatase octahedrite and unformed shape mixed phase (Fig. 2), Anatase crystal is grown up gradually, and median size increases to the c part of 8.90nm(Fig. 3), specific surface area size is 161.18m
2/ g.This TiO
2in visible absorption spectrum, occurring a boss (Fig. 5), represent that it has an interband energy level (Fig. 7), is also the major cause that its energy gap narrows.The adsorptive power of this product is not high, but has suitable degree of crystallinity and energy gap, therefore has higher sunlight and visible light catalysis activity (Fig. 8 a, b) simultaneously.
embodiment 4
Under ice-water bath condition, toward the 8.0g/100mL titanium sulfate solution and the 4mol/L ammoniacal liquor that add respectively 12mL and 20mL to prepare in 100mL deionized water, reaction system magnetic agitation 2h; By centrifugal the colloidal sol after stirring, solid precipitation deionized water supersound washing; Get the colloidal sol after 100mL washing, at 80 DEG C, be dried and obtain white nano-TiO
2solid, then processes 3h by its constant temp. heating at 500 DEG C, obtains faint yellow nano-TiO
2(Fig. 1).This nano-TiO
2belong to anatase octahedrite and unformed shape mixed phase (Fig. 2), Anatase crystal continues to grow up, and median size increases to 12.68nm.The energy band structure of this product and 400 DEG C of heat treated TiO
2similar, and its degree of crystallinity is higher than the latter, therefore its under solar irradiation to the degradation rate of fuchsin solution higher than 400 DEG C of heat treated nano-TiOs
2, and at visible ray according to next contrary (Fig. 8 a, b).
embodiment 5
Under ice-water bath condition, toward the 8.0g/100mL titanium sulfate solution and the 4mol/L ammoniacal liquor that add respectively 12mL and 20mL to prepare in 100mL deionized water, reaction system magnetic agitation 2h; By centrifugal the colloidal sol after stirring, solid precipitation deionized water supersound washing; Get the colloidal sol after 100mL washing, at 80 DEG C, be dried and obtain white nano-TiO
2solid, then processes 3h by its constant temp. heating at 600 DEG C, obtains yellow-white nano-TiO
2(Fig. 1).This nano-TiO
2belong to anatase octahedrite and unformed shape mixed phase (Fig. 2) because its degree of crystallinity is higher, median size 15.11nm, under solar irradiation to the degradation rate of fuchsin solution higher than 500 DEG C of heat treated nano-TiOs
2(Fig. 8 a); Simultaneously because it also has certain band curvature (Fig. 7), in structure, unformed and ratio anatase octahedrite is conducive to visible light catalytic most, the therefore TiO after all thermal treatment
2in there is the highest visible light catalysis activity (Fig. 8 b).
embodiment 6
Under ice-water bath condition, toward the 8.0g/100mL titanium sulfate solution and the 4mol/L ammoniacal liquor that add respectively 12mL and 20mL to prepare in 100mL deionized water, reaction system magnetic agitation 2h; By centrifugal the colloidal sol after stirring, solid precipitation deionized water supersound washing; Get the colloidal sol after 100mL washing, at 80 DEG C, be dried and obtain white nano-TiO
2solid, then processes 3h by its constant temp. heating at 700 DEG C, obtains white nano-TiO
2(Fig. 1).This nano-TiO
2belong to anatase octahedrite and unformed shape mixed phase, the brilliant median size 16.43nm of anatase-phase nano, illustrates highly crystalline of this product.Because the degree of crystallinity that it is high, still have a small amount of unformed shape to exist simultaneously, in its structure, unformed and ratio anatase octahedrite is conducive to sunlight catalytic most, therefore under solar irradiation to fuchsin solution the nano-TiO after all thermal treatment
2in have the highest degradation rate (Fig. 8 a), but visible ray according under catalyzed degradation activity lower (Fig. 8 b).
embodiment 7
Under ice-water bath condition, toward the 8.0g/100mL titanium sulfate solution and the 4mol/L ammoniacal liquor that add respectively 12mL and 20mL to prepare in 100mL deionized water, reaction system magnetic agitation 2h; By centrifugal the colloidal sol after stirring, solid precipitation deionized water supersound washing; Get the colloidal sol after 100mL washing, at 80 DEG C, be dried and obtain white nano-TiO
2solid, then processes 3h by its constant temp. heating at 800 DEG C, obtains white nano-TiO
2(Fig. 1).This nano-TiO
2the overwhelming majority belongs to the anatase octahedrite (Fig. 2) of highly crystalline, also has a small amount of unformed shape, and Anatase crystal median size has been grown up to 31.05nm(Fig. 3), specific surface area size reduces to 19.35m
2/ g.Although this product has maximum degree of crystallinity, there is not band curvature, energy gap wider (Fig. 7), therefore not high (Fig. 8 a, b) of sunlight and visible light photocatalysis active.
embodiment 8
Under ice-water bath condition, toward the 8.0g/100mL titanium sulfate solution and the 4mol/L ammoniacal liquor that add respectively 12mL and 20mL to prepare in 100mL deionized water, reaction system magnetic agitation 2h; By centrifugal the colloidal sol after stirring, solid precipitation deionized water supersound washing; Get the colloidal sol after 100mL washing, at 80 DEG C, be dried and obtain white nano-TiO
2solid, then processes 3h by its constant temp. heating at 1000 DEG C, obtains khaki color nano-TiO
2.This nano-TiO
2belong to the rutile (Fig. 2) of highly crystalline.
Claims (10)
1. the mixed phase nano-TiO of a series of different colours
2, it is characterized in that, they are by the white armorphous nano TiO to after water one-step synthesis
2carry out obtaining after the thermal treatment of differing temps, described mixed phase is amorphous and anatase octahedrite mixed phase, and thermal treatment temp is higher, and unformed phase proportion is lower.
2. the mixed phase nano-TiO of different colours according to claim 1
2, it is characterized in that, described water one-step synthesis is titanium sulfate solution and ammoniacal liquor single step reaction in water.
3. the mixed phase nano-TiO of different colours according to claim 1
2, it is characterized in that, described thermal treatment temp is 200-800 DEG C, processes the pressed powder that obtains comprising palm fibre, Huang, ash, white colour under differing temps.
4. the mixed phase nano-TiO of different colours according to claim 1
2, it is characterized in that, when described thermal treatment temp is 700 DEG C, the mixed phase nano-TiO obtaining
2under solar irradiation, there is the highest photocatalytic activity.
5. the mixed phase nano-TiO of different colours according to claim 1
2, it is characterized in that, when described thermal treatment temp is 600 DEG C, the mixed phase nano-TiO obtaining
2under shining, visible ray there is the highest photocatalytic activity.
6. the mixed phase nano-TiO of different colours according to claim 1
2, it is characterized in that, the energy gap of nano TiO 2 raises and increases with thermal treatment temp, and specific surface area raises and reduces with thermal treatment temp.
7. the mixed phase nano-TiO of different colours according to claim 1
2preparation method, it is characterized in that, concrete steps are:
1) under ice-water bath condition, titanium sulfate solution and ammoniacal liquor are joined in deionized water, this single step reaction, through being uniformly mixed 2h, obtains TiO
2the colloidal sol of unformed hydrate;
2) colloidal sol centrifugation step 1) being obtained, solid precipitation deionized water wash;
3) by step 2) in washing after colloidal sol evaporate to dryness at low temperatures, obtain white armorphous nano TiO
2solid, passes through respectively heat treatments at different, obtains the mixed phase nano-TiO of different colours
2.
8. the mixed phase nano-TiO of a kind of different colours according to claim 7
2preparation method, it is characterized in that, in step 1), the concentration of titanium sulfate solution is 8.0g/100mL, the concentration of ammoniacal liquor is 4mol/L, the pH of reaction system maintains 9-10.
9. the mixed phase nano-TiO of a kind of different colours according to claim 7
2preparation method, it is characterized in that step 2) at least 5500rpm of centrifugation rate, more than washing time 20min.
10. the mixed phase nano-TiO of a kind of different colours according to claim 7
2preparation method, it is characterized in that, low temperature evaporate to dryness described in step 3) is 60-80 DEG C of constant temperature evaporate to dryness in air dry oven, then the solid of evaporate to dryness is put into retort furnace, respectively at 200 DEG C, 300 DEG C, 400 DEG C, 500 DEG C, 600 DEG C, 700 DEG C and 800 DEG C of thermal treatment 3h, 10 DEG C/min of temperature rise rate, obtains the mixed phase nano-TiO of different colours
2.
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