CN107814413A - The preparation method of water nano titanium oxide sol - Google Patents
The preparation method of water nano titanium oxide sol Download PDFInfo
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- CN107814413A CN107814413A CN201711104311.2A CN201711104311A CN107814413A CN 107814413 A CN107814413 A CN 107814413A CN 201711104311 A CN201711104311 A CN 201711104311A CN 107814413 A CN107814413 A CN 107814413A
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- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
- C01G23/0532—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing sulfate-containing salts
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Abstract
The invention discloses the synthetic method of a kind of nanometer of titanium oxide sol, the described method comprises the following steps：(1) acidolysis；(2) titanium liquid purifies；(3) sulfate radical removes；(4) it is catalytically decomposed；(5) centrifuge.Preparation in accordance with the present invention uses cheap ilmenite as raw material, without obtaining positive metatitanic acid by alkali precipitation titanyl sulfate, this method is used as reactive material by the use of barium peroxide, directly sulfate ion is precipitated, peroxide root and titanium ion are formed into complex simultaneously and are dissolved in water, reaction condition is gentle, and step is easy；Meanwhile by introducing Fe3O4As Fenton catalyst, avoid the gelation of titanium peroxide and the heterogeneous nucleation process on barium sulfate surface, the titanium oxides product granule-morphology of preparation is uniform, can largely save the use of alkali and the discharge of waste water, and preparation in accordance with the present invention technique is simply adapted to large-scale industrial production.
Description
Technical field
The invention belongs to inorganic titanium oxide preparation field, more particularly to high-activity nano TiO2The preparation side of sol material
Method.
Background technology
Titanium dioxide is important Inorganic Chemicals, in works such as coating, ink, papermaking, plastics, rubber, synthetic fibers
It is used as Chinese white in industry；Meanwhile industrially also there is important application in enamel, ceramics, welding rod, electronics, metallurgy etc..
Typically there are two kinds of technique productions of sulfuric acid process and chloridising：Traditional sulfuric acid process industrial production titanium white powder flow path
Long, three waste discharge is more, and obtained product particle is big and uneven, is difficult to control；And chloridising is high to ingredient requirement, equipment corrosion
Seriously, preparation condition is harsh.
TiO 2 sol is with a wide range of applications as the uniform and stable dispersion of nano titanium oxide, can be with
For the synthesis of photocatalytic film coating or automatically cleaning high grade paint etc..At present, prepare TiO 2 sol and typically use titanium
Organic compound control hydrolysis or the method for Ti-inorganic salt hydrolysis.Two are prepared using the method for titanium organic compound control hydrolysis
TiOx nano colloidal sol, because titanium organic compound is expensive, greatly improve cost；Simultaneously as mixed using alcohol water
Heshui solution, obtained product are organic solution, limit it and are applied in hydrophilic base.Using Ti-inorganic salt hydrolysis, it is necessary to height
The additional steps such as warm water thermal crystallisation, not only need special installation and device, add cost, also limit production scale.
Compound anion method for preparing rutile type titanium dioxide method patent such as number of patent application 91101522.1 is also reported
The titanium sulfate solution obtained using sulfuric acid decomposition ilmenite is added composite anion and prepares rutile titanium dioxide, but it is needed
Follow-up 800-900 DEG C of high temperature crystallization process is wanted, this not only adds apparatus and process difficulty and improves cost, while also due to
High temperature sintering causes powder reuniting to increase particle diameter.Hiroaki Katsuki[Journal of the Ceramic Society
Of Japan 106 [3] 344~347 1998] report the positive metatitanic acid obtained using hydrogen peroxide dissolving by titanium tetrachloride hydrolysis
The method that precipitation prepares TiO 2 sol.It is high to equipment requirement because it uses corrosivity titanium tetrachloride as presoma, thus
Industrial production cost is too high.
The content of the invention
In view of the above-mentioned problems of the prior art, it is an object of the present invention to prepare Detitanium-ore-type in sulfuric acid process
On the basis of the conventional method of titanium dioxide, there is provided the synthetic method using ilmenite as the nanometer titanium oxide sol of raw material, it is real
Existing normal pressure, low temperature liquid phase synthesis nanometer titanium oxide, can significantly reduce reaction process and production cost.
The synthetic method of nanometer titanium oxide sol according to the present invention comprises the following steps：
(1) acidolysis
The concentrated sulfuric acid for being more than 80wt% with weight percent concentration dissolves by heating ilmenite, the ilmenite and the concentrated sulfuric acid
Mass ratio be 1:0.5 to 1:6, react fierce rapid, typically completed in 5~30min, reaction maximum temperature obtains up to 250 DEG C
To solid precipitation thing obtain titanium liquid with the water extraction of 5-10 times of volume；
(2) titanium liquid purifies
The titanium liquid of step (1) is carried out to be filtered to remove insoluble slag, frozen recrystallization obtains to be filtered to remove ferrous sulfate
To the precursor solution of titaniferous；
(3) sulfate radical removes
The precursor solution in step 2) is diluted with water to sulfur acid oxygen titanium (TiOSO4) mass percent is
5wt% to 20wt% solution, by BaO2It is 5wt% to 20wt% to be dispersed in water and to form mass percent concentration, is preferably
10wt% BaO2Suspension, then according to Ti:Ba mol ratios are 1:0.2 to 1:8 ratio is by BaO2Suspension is added to dilution
In the precursor solution of titaniferous afterwards, orange-yellow emulsion is obtained；
(4) it is catalytically decomposed
Fe is added in the orange-yellow emulsion obtained into step 3)3O4Powder is to Fe3O4Molar concentration for 0.005 to
0.1mol/l, 90-100 DEG C of backflow 30min, obtain light yellow emulsion.
(5) centrifuge
The light yellow emulsion obtained in step 4) is utilized into centrifuge precipitation and separation and supernatant, resulting is orange-yellow
Clear is titanium oxides product colloidal sol.
Preferably, in step 1), the mass ratio of the ilmenite and the concentrated sulfuric acid is 1:0.5 to 1:4, more preferably 1:1 to
1:3, most preferably 1:2.
Preferably, in step 1), the obtained solid precipitation thing obtains titanium liquid with the water extraction of 6-8 times of volume, more excellent
Elect the water of 7.5 times of volumes as.
Preferably, in step 3), the Ti:Ba mol ratios are 1:0.5 to 1:4, more preferably 1:0.6 to 1:2, most preferably
For 1:1 to 1:1.2.
Preferably, in step 3), the precursor solution in step 2) is diluted with water to sulfur acid oxygen titanium
(TiOSO4) mass percent be 5wt% to 15wt% solution, more preferably 10wt%.
Preferably, in step 4), Fe is added in the orange-yellow emulsion obtained into step 3)3O4Powder is to Fe3O4Rub
Your concentration is 0.005 to 0.06mol/l, more preferably 0.005 to 0.02mol/l, most preferably 0.01mol/l.
Preferably, preparation method according to the present invention is carried out as follows：
1) concentrated sulfuric acid that mass percent concentration is more than 80wt% is dissolved by heating into ilmenite, wherein ilmenite and sulfuric acid
Mass ratio be 1:2, obtained solid precipitation thing obtains titanium liquid with the water extraction of 7.5 times of volumes, is then filtered to remove insoluble
Slag；
2) the titanium liquid frozen recrystallization in step 1) is obtained into the precursor solution of titaniferous to be filtered to remove ferrous sulfate；
3) precursor solution in step 2) is diluted to sulfur acid oxygen titanium (TiOSO4) mass percent is
10wt% solution；It is that 10wt% titanyl sulfate solutions addition 250g mass percents are to take mass percent described in 200g
10wt% BaO2Suspension, wherein Ti:Ba mol ratio is about 1:1.2；
4) 1g Fe is added in the mixture obtained into step 3)3O4Powder, the 30min that flowed back at 100 DEG C obtain yellow
Colloidal sol；
5) yellow sol obtained in step 4) is centrifugally separating to obtain clear titanyl with centrifuge 5000rpm
Compound product colloidal sol.
It is another object of the present invention to provide a kind of titanium oxides product aerosol product, the titanium oxides product are molten
Glue product is prepared by preparation method according to the present invention.
Beneficial effect
Preparation in accordance with the present invention uses cheap ilmenite as raw material, avoids using expensive organic metatitanic acid
Ester type compound, while without by alkali precipitation titanyl sulfate obtain positive metatitanic acid, then multiple washing remove sulfate ion,
Alkaline precipitating agent, pure positive metatitanic acid is obtained, then nano-titanium oxide is prepared with hydrogen peroxide dissolving.This method peroxidating
Barium directly precipitates sulfate ion as reactive material, while peroxide root and titanium ion are formed into complex and are dissolved in water, reacts
Mild condition, step are easy；Meanwhile by introducing Fe3O4As Fenton catalyst, avoid titanium peroxide gelation and
The heterogeneous nucleation process on barium sulfate surface, the titanium oxides product granule-morphology of preparation is uniform, can largely save alkali use and
The discharge of waste water, preparation in accordance with the present invention technique are simply adapted to large-scale industrial production.
Brief description of the drawings
Fig. 1 is the TEM figures of product prepared by embodiment 1；
Fig. 2 is product XRD spectra prepared by embodiment 1；
Fig. 3 is that the methylene blue of product prepared by embodiment 1 decomposes ultraviolet spectrogram.
Embodiment
Hereinafter, it will be described in detail the present invention.Before doing so, it should be appreciated that in this specification and appended
Claims in the term that uses should not be construed as being limited to general sense and dictionary meanings, and inventor should allowed
On the basis of appropriate definition term is to carry out the principle of best interpretations, according to implication corresponding with the technical elements of the present invention and generally
Thought explains.Therefore, description presented herein is not intended to limitation originally merely for the sake of the preferred embodiment for illustrating purpose
The scope of invention, it will thus be appreciated that without departing from the spirit and scope of the present invention, it can be obtained by it
His equivalents or improved procedure.
General synthetic method by sulfuric acid process acidolysis obtain titanyl sulfate be used as precursor synthesis nano-titanium oxide, it is necessary to
Alkali precipitation obtains positive metatitanic acid, then removes sulfate ion, alkaline precipitating agent in multiple washing, obtains pure positive metatitanic acid, then
Nano-titanium oxide is prepared with hydrogen peroxide dissolving.This method is directly by the use of barium peroxide as reactive material, directly by sulfuric acid
Radical ion is precipitated, while peroxide root and titanium ion are formed into complex and are dissolved in water, can realize sulfuric acid by simple centrifugally operated
Barium separates to be prepared with titanium peroxide presoma.Simultaneously as there is serious polycondensation reaction, above-mentioned barium sulfate peroxidating in titanium peroxide
Operation, which is directly centrifuged, in titanium system can result in gel；And above-mentioned barium sulfate titanium peroxide system directly heats reaction
Titanium oxide precipitate can be made can not to obtain high-purity titanium oxide sol in barium sulfate precipitate superficial growth.The present invention is by titanium oxide
The mechanism regulation of liquid growth, realize normal pressure, the method for low temperature liquid phase synthesis related system oxide material.The pass of the present invention
Key point is using barium peroxide while produced by precipitating removing sulfate ion；And introduce peroxide and form titanium mistake with ion
Oxygen complex, while obtain titanium oxide using Fe fenton principles catalysis fast decoupled peroxide root.By introducing Fe3O4Make
For catalyst, decomposed based on Fenton mechanism quick catalysis titanium peroxide, form stable titanium oxide sol system and barium sulfate
Suspension system, realize that separation barium sulfate precipitate obtains high-purity titanium oxide sol by centrifuging.The present invention can be used for being directly realized by
Normal pressure, low temperature liquid phase synthesis nanometer titanium oxide, can significantly reduce reaction process and production cost.
The synthetic method of nanometer titanium oxide sol according to the present invention comprises the following steps：
(1) acidolysis
The concentrated sulfuric acid for being more than 80wt% with weight percent concentration dissolves by heating ilmenite, the ilmenite and the concentrated sulfuric acid
Mass ratio be 1:0.5 to 1:6, react fierce rapid, typically completed in 5~30min, reaction maximum temperature obtains up to 250 DEG C
To solid precipitation thing obtain titanium liquid with the water extraction of 5-10 times of volume；
(2) titanium liquid purifies
The titanium liquid of step (1) is carried out to be filtered to remove insoluble slag, frozen recrystallization obtains to be filtered to remove ferrous sulfate
To the precursor solution of titaniferous；
(3) sulfate radical removes
The precursor solution in step 2) is diluted with water to sulfur acid oxygen titanium (TiOSO4) mass percent is
5wt% to 20wt% solution, by BaO2It is 5wt% to 20wt% to be dispersed in water and to form mass percent concentration, is preferably
10wt% BaO2Suspension, then according to Ti:Ba mol ratios are 1:0.2 to 1:8 ratio is by BaO2Suspension is added to dilution
In the precursor solution of titaniferous afterwards, orange-yellow emulsion is obtained；
(4) it is catalytically decomposed
Fe is added in the orange-yellow emulsion obtained into step 3)3O4Powder is to Fe3O4Molar concentration for 0.005 to
0.1mol/l, 90-100 DEG C of backflow 30min, obtain light yellow emulsion.
(5) centrifuge
The light yellow emulsion obtained in step 4) is utilized into centrifuge precipitation and separation and supernatant, resulting is orange-yellow
Clear is titanium oxides product colloidal sol.
Wherein in step 1), the mass ratio of the ilmenite and the concentrated sulfuric acid is 1:0.5 to 1:4, more preferably 1:1 to 1:3,
Most preferably 1:2.When the mass ratio of ilmenite and the concentrated sulfuric acid is more than 1:When 1, i.e. the amount of ilmenite is superfluous, then can not give birth to completely
Into TiOSO4, contain a large amount of ilmenite raw materials in titanium liquid, turn into impurity, cause in second step to be difficult to by frozen recrystallization mistake
Filter out ferrous sulfate；When the mass ratio of ilmenite and the concentrated sulfuric acid is less than 1:When 3, i.e. excess sulfuric acid then not only generates
TiOSO4, but also generate Ti (SO4)2, the waste of titanium source is caused, while the content of titanium in titanium liquid is difficult to control, and then be difficult to control
Later stage BaO processed2With the ratio of titanium.
Preferably, in step 1), the obtained solid precipitation thing obtains titanium liquid with the water extraction of 6-8 times of volume, more excellent
Elect the water of 7.5 times of volumes as.If the water used is less than 6 times of volumes, leaching is incomplete；And if greater than 8 times of volumes, then titanium
Liquid concentration is too low, the problems such as causing late phase reaction speed degradation.
Preparation in accordance with the present invention, Ti:Ba mol ratio is one of key, it is preferable that in step 3), the Ti:
Ba mol ratios are 1:0.5 to 1:4, more preferably 1:0.6 to 1:2, most preferably 1:1 to 1:1.2.Work as Ti:Ba mol ratios are more than
1:0.6, i.e. ti excess, then titanium peroxide polycondensation reaction easily occurs, with barium sulfate formed gel flocculation, it is difficult to centrifuge；
Work as Ti:Ba mol ratios are less than 1:2, i.e. barium is excessive, then equally easily causes titanium peroxide and polycondensation reaction occurs.
Preferably, in step 4), Fe is added in the orange-yellow emulsion obtained into step 3)3O4Powder is to Fe3O4Rub
Your concentration is 0.005 to 0.06mol/l, more preferably 0.005 to 0.02mol/l, most preferably 0.01mol/l.Work as Fe3O4's
When molar concentration is less than 0.005mol/l, then it can not decompose titanium peroxide complete, it is impossible to form stable titanium oxide sol body
System and barium sulfate suspension system；When more than 0.02mol/l, then titanium peroxide decomposition rate is too fast, is difficult to control, causes oxygen
Change titanium colloidal sol to flocculate with barium sulfate particle.
Following examples are enumerated only as the example of embodiment of the present invention, do not form any limit to the present invention
System, it will be appreciated by those skilled in the art that the modification in the range of without departing from the essence of the present invention and design each falls within the present invention
Protection domain.Unless stated otherwise, the reagent and instrument used in following examples is commercially available product.
Embodiment 1
1) concentrated sulfuric acid that mass percent concentration is 85wt% is dissolved by heating to the matter of ilmenite, wherein ilmenite and sulfuric acid
Amount is than being 1:2, obtained solid precipitation thing obtains titanium liquid with the water extraction of 7.5 times of volumes, is then filtered to remove insoluble slag；
2) the titanium liquid frozen recrystallization in step 1) is obtained into the precursor solution of titaniferous to be filtered to remove ferrous sulfate；
3) precursor solution in step 2) is diluted to sulfur acid oxygen titanium (TiOSO4) mass percent is
10wt% solution；It is that 10wt% titanyl sulfate solutions addition 250g mass percents are to take mass percent described in 200g
10wt% BaO2Suspension, wherein Ti:Ba mol ratio is about 1:1.2；
4) 1g Fe is added in the mixture obtained into step 3)3O4Powder, the 30min that flowed back at 100 DEG C obtain yellow
Colloidal sol；
5) yellow sol obtained in step 4) is centrifugally separating to obtain clear titanyl with centrifuge 5000rpm
Compound product colloidal sol.
Product result is characterized as nano particle through TEM, sees accompanying drawing 1.Obtained titanium oxides product colloidal sol is done by vacuum
Nano-titanium dioxide powder is obtained after dry, XRD spectra measurement result is confirmed that it is anatase titanium dioxide crystal, sees accompanying drawing 2.
Embodiment 2
Except the mass ratio of ilmenite and the concentrated sulfuric acid is 1:Beyond 3, titanium oxide is prepared according to the identical mode of embodiment 1
Product colloidal sol.
Embodiment 3
Except Ti in step 3):Ba mol ratio is adjusted to 1:Beyond 0.6, titanium is prepared according to the identical mode of embodiment 1
Oxide products colloidal sol.
Embodiment 4
Except Fe in step 4)3O4Molar concentration be adjusted to beyond 0.02mol/l, according to the identical mode system of embodiment 1
Standby titanium oxides product colloidal sol.
Comparative example 1
Except Ti in step 3):Ba mol ratio is adjusted to 1:Beyond 4, titanyl is prepared according to the identical mode of embodiment 1
Compound product colloidal sol, but can not effectively obtain titanium oxides product colloidal sol.
Comparative example 2
Except Fe in step 4)3O4Molar concentration be adjusted to beyond 0.06mol/l, according to the identical mode system of embodiment 1
Standby titanium oxides product colloidal sol, but titanium peroxide decomposition rate is too fast, and titanium oxide mutually flocculates with barium sulfate particle, produces a large amount of
Precipitation, can not obtain titanium oxides product colloidal sol.
Comparative example 3
Except Ti in step 3):Ba mol ratio is adjusted to 1:Beyond 0.5, titanium is prepared according to the identical mode of embodiment 1
Oxide products colloidal sol, but can not effectively obtain titanium oxides product colloidal sol.
Comparative example 4
Except Fe in step 4)3O4Molar concentration be adjusted to beyond 0.005mol/l, according to the identical mode of embodiment 1
Prepare titanium oxides product colloidal sol, it is impossible to form stable titanium oxide sol system and barium sulfate suspension system.
EXPERIMENTAL EXAMPLE 1
By the titanium oxides product colloidal sol prepared in embodiment 1 to 4 by czochralski method in glass surface film forming, interception 1*
2cm width is immersed in the 1mmol methylene blue solutions that 20ml after 24 hours, is immersed in 2mmol methylene blue solutions, in 365nm
It is determined under ultraviolet irradiation condition to methylene blue degradation effect.The discomposing effect of embodiment 1 is shown in accompanying drawing 3, methylene blue degraded
Light requirement shines 62 minutes when rate is 50%；The product light requirement of embodiment 2 shines 61 minutes when methylene blue degradation rate is 50%；Methylene
The product light requirement of embodiment 2 shines 63 minutes when blue degradation rate is 50%；The product of embodiment 4 when methylene blue degradation rate is 50%
Light requirement shines 64 minutes.Organic matter etc. can be effectively realized according to the titanium oxides product colloidal sol of the preparation of the present invention as can be seen here
Degraded, have broad application prospects.
Claims (8)
1. the synthetic method of a kind of nanometer of titanium oxide sol comprises the following steps：
(1) acidolysis
The concentrated sulfuric acid for being more than 80wt% with weight percent concentration dissolves by heating ilmenite, the matter of the ilmenite and the concentrated sulfuric acid
Amount is than being 1:0.5 to 1:6, react fierce rapid, typically completed in 5~30min, reaction maximum temperature obtains up to 250 DEG C
Solid precipitation thing obtains titanium liquid with the water extraction of 5-10 times of volume；
(2) titanium liquid purifies
The titanium liquid of step (1) is carried out to be filtered to remove insoluble slag, frozen recrystallization is contained to be filtered to remove ferrous sulfate
The precursor solution of titanium；
(3) sulfate radical removes
The precursor solution in step 2) is diluted with water to sulfur acid oxygen titanium (TiOSO4) mass percent be 5wt% extremely
20wt% solution, by BaO2It is 5wt% to 20wt% to be dispersed in water and to form mass percent concentration, preferably 10wt%'s
BaO2Suspension, then according to Ti:Ba mol ratios are 1:0.2 to 1:8 ratio is by BaO2Suspension is added to the titaniferous after dilution
Precursor solution in, obtain orange-yellow emulsion；
(4) it is catalytically decomposed
Fe is added in the orange-yellow emulsion obtained into step 3)3O4Powder is to Fe3O4Molar concentration for 0.005 to
0.1mol/l, 90-100 DEG C of backflow 30min, obtain light yellow emulsion.
(5) centrifuge
The light yellow emulsion obtained in step 4) is utilized into centrifuge precipitation and separation and supernatant, resulting orange-yellow clarification
Transparent is titanium oxides product colloidal sol.
2. the synthetic method of according to claim 1 nanometer of titanium oxide sol, it is characterised in that described in step 1)
The mass ratio of ilmenite and the concentrated sulfuric acid is 1:0.5 to 1:4, more preferably 1:1 to 1:3, most preferably 1:2.
3. the synthetic method of according to claim 1 nanometer of titanium oxide sol, it is characterised in that described in step 1)
Obtained solid precipitation thing obtains titanium liquid, the water of more preferably 7.5 times volumes with the water extraction of 6-8 times of volume.
4. the synthetic method of according to claim 1 nanometer of titanium oxide sol, it is characterised in that described in step 3)
Ti:Ba mol ratios are 1:0.5 to 1:4, more preferably 1:0.6 to 1:2, most preferably 1:1 to 1:1.2.
5. the synthetic method of according to claim 1 nanometer of titanium oxide sol, it is characterised in that in step 3), will walk
It is rapid 2) in the precursor solution be diluted with water to sulfur acid oxygen titanium (TiOSO4) mass percent be 5wt% to 15wt%'s
Solution, more preferably 10wt%.
6. the synthetic method of according to claim 1 nanometer of titanium oxide sol, it is characterised in that in step 4), Xiang Bu
It is rapid 3) in add Fe in obtained orange-yellow emulsion3O4Powder is to Fe3O4Molar concentration be 0.005 to 0.06mol/l, more
Preferably 0.005 to 0.02mol/l, most preferably 0.01mol/l.
7. the synthetic method of according to claim 1 nanometer of titanium oxide sol, it is characterised in that the preparation method is such as
Lower progress：
1) concentrated sulfuric acid that mass percent concentration is more than 80wt% is dissolved by heating to the matter of ilmenite, wherein ilmenite and sulfuric acid
Amount is than being 1:2, obtained solid precipitation thing obtains titanium liquid with the water extraction of 7.5 times of volumes, is then filtered to remove insoluble slag；
2) the titanium liquid frozen recrystallization in step 1) is obtained into the precursor solution of titaniferous to be filtered to remove ferrous sulfate；
3) precursor solution in step 2) is diluted to sulfur acid oxygen titanium (TiOSO4) mass percent be 10wt% it is molten
Liquid；It is the BaO that 10wt% titanyl sulfate solutions add that 250g mass percents are 10wt% to take mass percent described in 200g2It is outstanding
Turbid, wherein Ti:Ba mol ratio is about 1:1.2；
4) 1g Fe is added in the mixture obtained into step 3)3O4Powder, it is molten that the 30min that flowed back at 100 DEG C obtains yellow
Glue；
5) yellow sol obtained in step 4) is centrifugally separating to obtain clear titanium oxide with centrifuge 5000rpm
Product colloidal sol.
8. a kind of titanium oxides product aerosol product, the titanium oxides product aerosol product according in claim 1 to 7 by appointing
One preparation method of meaning is prepared.
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| CN101786656A (en) * | 2010-03-26 | 2010-07-28 | 湘潭大学 | Preparation method of Barium Titanate nano-powder |
| CN103449510A (en) * | 2013-04-09 | 2013-12-18 | 深圳信息职业技术学院 | Submicron barium titanate crystal and preparation method thereof |
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| CN1654335A (en) * | 2004-12-24 | 2005-08-17 | 广东省生态环境与土壤研究所 | Preparation method of visible light photoactivated octahedrite type titanium oxide colloidal sols |
| CN1935669A (en) * | 2005-09-22 | 2007-03-28 | 中国科学院理化技术研究所 | Low temperature crystallized nano titanium dioxide powder and sol synthesizing method |
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