CN102995120B - Nanometer TiO2 monocrystalline material, preparation method and application thereof - Google Patents
Nanometer TiO2 monocrystalline material, preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a nanometer TiO2 monocrystalline material, a preparation method and an application thereof, and belongs to the field of inorganic nano-material preparation. Anatase type nanometer TiO2 monocrystalline particles having uniform particle size distribution and with the diameter of 30 nm are prepared by combination of precipitation-hydrothermal method at a relatively low temperature. The preparation method is simple in process and low in energy consumption; and the obtained titanium dioxide material has uniform morphology, high purity and excellent performance for photocatalytic degradation of organic materials.
Description
Technical field
The present invention relates to a kind of nano-TiO
2monocrystal material, Preparation Method And The Use, belong to field of inorganic nano-material preparation, particularly a kind of nano-TiO with highly homogeneous granularity
2monocrystal material and preparation method thereof, and it is in the purposes of photocatalysis field.
Background technology
TiO
2as a kind of important conductor oxidate, since the sixties in last century, the fields such as pigment, coating, ink, makeup, environmental pollution improvement are widely used in the physical and chemical performance of its excellence.Particularly the photochemical catalysis of its excellence and photoelectric properties, make TiO
2a large amount of application is also obtain in the new industry such as photochemical catalysis and solar cell.TiO
2these application have close contacting with himself pattern, size, crystalline structure etc.TiO
2common crystal formation has three kinds: brookite, anatase octahedrite and rutile, wherein anatase octahedrite TiO
2excellent performance is shown in photochemical catalysis and solar cell etc.The TiO that size is little
2have larger specific surface area, high-specific surface area contributes to the absorption and the specific refractory power that improve light, is conducive to the absorption of reactant on surface, makes TiO
2there is higher photocatalytic activity.For ensureing TiO
2stable performance in the research and apply continued, the TiO of synthesis
2material should have crystalline structure, and particle scale should keep homogeneous; Meanwhile, the nano-TiO that size-grade distribution is homogeneous
2in metering and field fo standardization, there is very important application.Therefore, the anatase crystal nano-TiO that prepared sizes are homogeneous
2material has great importance.
CN 101318128A discloses a kind of anatase structured highlight catalytic active nano TiO
2preparation method, comprise the following steps: the inorganic salt that (1) takes organo titanium compounds or titanium are dissolved in Glacial acetic acid and make mixed solution, are dissolved in by mixed solution in dehydrated alcohol, obtain solution 1; (2) choose two kinds or three kinds of template agent, be dissolved in dehydrated alcohol, obtain solution 2; (3) solution 1 and solution 2 are mixed, add distilled water, stir, obtain settled solution, leave standstill 2 ~ 5 days, form gel, dry; (4) template agent is removed in dry thing calcining, obtain anatase structured highlight catalytic active nano TiO
2, the anatase structured highlight catalytic active nano TiO prepared by the method for this invention
2its particle diameter is less than P-25, and specific surface area is greater than P-25, has the photocatalytic activity higher than P-25, can be widely used in the field such as photochemical catalysis, sensitization solar battery.
CN 1312223A relates to a kind of nano-TiO
2production method, select water soluble or organic solvent metallic salt to make it dissolve, mix with lewis' acid state, select a kind of suitable precipitation agent again or adopt the processes such as evaporation, crystallization, distillation, hydrolysis, by metal ion precipitation from homogeneous solution or crystallize out, then through dehydration or separate and decompose obtained powder.
At present, nano-TiO
2the preparation method of material has vapor phase process and liquid phase method.Wherein vapor phase process is because energy consumption is large, cost is high and the reason use range such as complex process is less, and liquid phase rule is due to energy consumption and advantage of lower cost, good uniformity and required equipment is simple etc. that advantage is widely used.That commonly uses in liquid phase method has chemical precipitation method, sol-gel method, the hot method of water/alcohol and microemulsion method etc., and wherein, chemical precipitation method is a kind of common method.But, the TiO that the precipitator method are prepared
2be unformed, hardly there is photocatalytic activity.For obtaining crystal TiO
2material, needs to carry out high-temperature heat treatment.Along with the raising of thermal treatment temp, nano-TiO
2will there is hard aggregation in particle, and specific surface area declines to a great extent.Therefore, low-temperature growth nano-TiO
2crystalline material is significant.The present invention utilizes chemical precipitation to combine with hydrothermal synthesis method, under cryogenic homogeneous, the anatase type nano TiO of prepared sizes distribution
2material.
Summary of the invention
The object of the present invention is to provide the anatase type nano TiO that a kind of size-grade distribution is homogeneous
2material and its production and use.
For reaching this object, the present invention by the following technical solutions:
An object of the present invention is to provide a kind of nano-TiO
2the preparation method of monocrystal material, said method comprising the steps of:
(1) by TiCl
4be added drop-wise in ammonia soln, the system that drops to, for neutral or weakly alkaline, obtains milk sap;
(2) the milk sap solid-liquid separation in step (1) is precipitated, then by washing of precipitate to neutral;
(3) precipitation in step (2) is dispersed in the mixed system of ethanol, water or ethanol and water, is placed in reaction kettle for reaction;
(4) after completion of the reaction, by the white emulsion solid-liquid separation obtained, washing is precipitated thing, and lyophilize, namely obtain the nano-TiO that size-grade distribution is homogeneous
2monocrystal material.
Step of the present invention (1) described TiCl
4concentration be 0.05 ~ 0.5mol/L.If concentration is too small, relatively less and drip time-consuming, concentration is excessive for the precipitation capacity that step (2) is obtained, and causes system pH change too fast and make precipitation uneven.TiCl of the present invention
4concentration can select 0.051 ~ 0.49mol/L, 0.08 ~ 0.4mol/L, 0.11 ~ 0.34mol/L, 0.16 ~ 0.3mol/L, 0.23 ~ 0.28mol/L etc., all can be used for implementing the present invention, preferably 0.1 ~ 0.2mol/L, further preferably 0.2mol/L.
The concentration of ammonia soln of the present invention is 0.12 ~ 0.8mol/L, such as 0.14 ~ 0.78mol/L, 0.3 ~ 0.6mol/L, 0.33 ~ 0.57mol/L, 0.37 ~ 0.51mol/L, 0.43mol/L etc., further preferably 0.2 ~ 0.5mol/L, most preferably 0.5mol/L.
By TiCl in step of the present invention (1)
4be added drop-wise in ammonia soln, the system that drops to is for neutral or weakly alkaline, and such as pH value is 7.02 ~ 9.5,7.4 ~ 9, and 8 ~ 8.5 etc., the pH value preferably dropping to system is 7.2 ~ 9.0, and further preferable ph is 8.0.
With deionized water, washing of precipitate is extremely neutral in step of the present invention (2).Washing of precipitate can also can be selected from prior art by those skilled in the art to neutral mode by other.
In step of the present invention (3), the volume ratio of ethanol and water is 10:0 ~ 0:10, and wherein 10:0 refers to be all ethanol, and 0:10 refers to be all water, all can be used for implementing the present invention.Described volume ratio is preferably 10:0 ~ 1:1, such as 9.9:0.1,9.2:0.8,8.5:1.5,7.6:2.4,7:3,6.2:3.8,5.5:4.5 etc., further preferred 9:1.
Reaction times in step of the present invention (3) is 2 ~ 18h.Reaction times is too short, can not get product; Long, then product particle is reunited, dispersed poor.Such as 2.01 ~ 17.8h, 3 ~ 15h, 3.8 ~ 14h, 5 ~ 12.3h, 7.5 ~ 11h, 9h etc., further preferably 3 ~ 15h, most preferably 7.5h.
Temperature of reaction in step of the present invention (3) is 110 ~ 180 DEG C.Temperature of reaction is too low, needs to extend the reaction times just can obtain product and the crystallinity of product is poor; Temperature of reaction is too high, and product is easily reunited, and power consumption is dangerous again.Such as 112 ~ 178 DEG C, 120 ~ 168 DEG C, 124 ~ 163 DEG C, 130 ~ 157 DEG C, 137 ~ 150 DEG C, 146 DEG C etc., preferably 120 ~ 150 DEG C further, most preferably 150 DEG C.
Step of the present invention (4) middle ethanol and deionized water washing sediment.
In step of the present invention (4), cryodesiccated temperature is-85 ~-40 DEG C, such as-84 ~-41 DEG C ,-81 ~-43 DEG C ,-75 ~-48 DEG C ,-67 ~-55 DEG C ,-62 ~-59 DEG C etc., preferred-75 ~-50 DEG C further, most preferably-60 DEG C.
Step of the present invention (2) and solid-liquid separation described in step (4) comprise filter, centrifugation, precipitation, gravity settling or centrifugal settling; Preferred centrifugation.Those skilled in the art can be known and select the mode of solid-liquid separation from prior art, can realize the solid-state of corresponding system and Liquid segregation and not change its inherent nature.
A kind of nano-TiO
2the preparation method of monocrystal material, described method, through optimizing, comprises the following steps:
(1) by the TiCl of 0.1 ~ 0.2mol/L
4be added drop-wise in the ammonia soln of 0.2 ~ 0.5mol/L, dropping to system pH is 8.0, obtains white " milky " liquid;
(2) the milk sap centrifugation in step (1) is precipitated, then with deionized water, washing of precipitate is extremely neutral;
(3) precipitation in step (2) is dispersed in the mixed system of ethanol, water or ethanol and water, is placed in reactor, at 120 ~ 150 DEG C, react 3 ~ 15h;
(4) after completion of the reaction, by the white emulsion centrifugation obtained, the throw out obtained with ethanol and deionized water wash lyophilize at-75 ~-50 DEG C, namely obtain the nano-TiO that size-grade distribution is homogeneous
2monocrystal material.
Two of object of the present invention is to provide a kind of nano-TiO obtained by method described above
2monocrystal material, described material particle size distribution is homogeneous, and median size is about 30nm, and relative standard deviation is less than 9%.Described median size can be 29nm, 30nm, 32nm etc.Those skilled in the art can know the particle size range of nano material of the present invention according to relative standard deviation.Specific surface area is 70 ~ 80m
2/ g.
Three of object of the present invention is to provide a kind of described nano-TiO
2the purposes of monocrystal material, by nano-TiO
2monocrystal material is as photocatalyst.
Compared with prior art scheme, the present invention has following beneficial effect:
Adopt the TiO that method of the present invention obtains
2granule-morphology rule, better crystallinity degree, size are even, good dispersity, product purity are high, and have higher photocatalytic activity, and preparation method is simple to operate, environmental friendliness, and reaction conditions is gentle, energy consumption is low, is easy to promote the use of.
Accompanying drawing explanation
Fig. 1 is the TiO that the present invention obtains
2the transmission electron microscope picture of monocrystal material;
Fig. 2 is the TiO that the present invention obtains
2the scanning electron microscope (SEM) photograph of monocrystal material;
Fig. 3 is the TiO that the present invention obtains
2the XRD figure of monocrystal material;
Fig. 4 is the TiO that the present invention obtains
2monocrystal material is with business nano-TiO
2material degradation methylene blue photocatalysis effect comparison diagram.
The present invention is described in more detail below.But following example is only simple and easy example of the present invention, and do not represent or limit the scope of the present invention, protection scope of the present invention is as the criterion with claims.
Embodiment
For better the present invention being described, be convenient to understand technical scheme of the present invention, typical but non-limiting embodiment of the present invention is as follows:
Embodiment 1
(1) by the TiCl of 0.2mol/L
4being added drop-wise in the ammonia soln of 100mL 0.5mol/L, is 8.0 to system pH value, obtains white " milky " liquid;
(2) white precipitate is obtained by centrifugal for the white " milky " liquid in step (1), then with deionized water, washing of precipitate is extremely neutral;
(3) precipitation in step (2) is dispersed in the ethanol (namely the volume ratio of ethanol and water is 10:0) of 50mL, is placed in reactor, at 150 DEG C, reacts 5h;
(4) after completion of the reaction, by the white emulsion centrifugation obtained, washing precipitate lyophilize at-65 DEG C, namely obtain the anatase type nano TiO that size-grade distribution is homogeneous
2monocrystal material.
TiO obtained by the present embodiment
2monocrystal material comprises the nano particle of a large amount of pattern rule, size uniform, good dispersity, and the particle diameter of particle is 32nm, and specific surface area is 72m
2/ g, relative standard deviation is 8%.
Embodiment 2
(1) by the TiCl of 0.2mol/L
4being added drop-wise in the ammonia soln of 100mL 0.5mol/L, is 8.0 to system pH, obtains white " milky " liquid;
(2) white precipitate is obtained by centrifugal for the white " milky " liquid in step (1), then with deionized water, washing of precipitate is extremely neutral;
(3) precipitation in step (2) is dispersed in 50mL ethanol and water volume ratio is in the system of 9:1, is placed in reactor, at 150 DEG C, reacts 5h;
(4) after completion of the reaction, by the white emulsion centrifugation obtained, washing precipitate lyophilize at-75 DEG C, namely obtain the anatase type nano TiO that size-grade distribution is homogeneous
2monocrystal material.
TiO obtained by the present embodiment
2monocrystal material comprises the nano particle of a large amount of pattern rule, size uniform, good dispersity, and the particle diameter of particle is 30nm, and specific surface area is 76m
2/ g, relative standard deviation is 7%.
Embodiment 3
(1) by the TiCl of 0.2mol/L
4being added drop-wise in the ammonia soln of 100mL 0.5mol/L, is 8.0 to system pH, obtains white " milky " liquid;
(2) white precipitate is obtained by centrifugal for the white " milky " liquid in step (1), then with deionized water, washing of precipitate is extremely neutral;
(3) precipitation in step (2) is dispersed in 50mL ethanol (namely the volume ratio of ethanol and water is 10:0), is placed in reactor, at 150 DEG C, reaction 15h;
(4) after completion of the reaction, by the white emulsion centrifugation obtained, washing precipitate lyophilize at-50 DEG C, namely obtain the anatase type nano TiO that size-grade distribution is homogeneous
2monocrystal material.
TiO obtained by the present embodiment
2monocrystal material comprises the nano particle of a large amount of pattern rule, size uniform, good dispersity, and the particle diameter of particle is 32nm, and specific surface area is 71m
2/ g, relative standard deviation is 9%.
Embodiment 4
(1) by the TiCl of 0.2mol/L
4being added drop-wise in the ammonia soln of 100mL 0.2mol/L, is 8.0 to system pH, obtains white " milky " liquid;
(2) white precipitate is obtained by centrifugal for the white " milky " liquid in step (1), then with deionized water, washing of precipitate is extremely neutral;
(3) precipitation in step (2) is dispersed in 50mL ethanol (namely the volume ratio of ethanol and water is 10:0), is placed in reactor, at 120 DEG C, reacts 7.5h;
(4) after completion of the reaction, by the white emulsion centrifugation obtained, washing precipitate lyophilize at-65 DEG C, namely obtain the anatase type nano TiO that size-grade distribution is homogeneous
2monocrystal material.
TiO obtained by the present embodiment
2monocrystal material comprises the nano particle of a large amount of pattern rule, size uniform, good dispersity, and the particle diameter of particle is 30nm, and specific surface area is 75m
2/ g, relative standard deviation is 7%.
Embodiment 5
(1) by the TiCl of 0.1mol/L
4being added drop-wise in the ammonia soln of 100mL 0.2mol/L, is 8.0 to system pH, obtains white " milky " liquid;
(2) white precipitate is obtained by centrifugal for the white " milky " liquid in step (1), then with deionized water, washing of precipitate is extremely neutral;
(3) precipitation in step (2) is dispersed in 50mL ethanol (namely the volume ratio of ethanol and water is 10:0), is placed in reactor, at 150 DEG C, reacts 7.5h;
(4) after completion of the reaction, by the white emulsion centrifugation obtained, washing precipitate lyophilize at-60 DEG C, namely obtain the anatase type nano TiO that size-grade distribution is homogeneous
2monocrystal material.
TiO obtained by the present embodiment
2monocrystal material comprises the nano particle of a large amount of pattern rule, size uniform, good dispersity, and the particle diameter of particle is 29nm, and specific surface area is 78m
2/ g, relative standard deviation is 8%.
Embodiment 6
(1) by the TiCl of 0.05mol/L
4being added drop-wise in the ammonia soln of 100mL 0.8mol/L, is 9.5 to system pH, obtains white " milky " liquid;
(2) white precipitate is obtained by centrifugal for the white " milky " liquid in step (1), then with deionized water, washing of precipitate is extremely neutral;
(3) precipitation in step (2) is dispersed in 50mL ethanol and water volume ratio is in the system of 1:1, be placed in reactor, at 120 DEG C, react 5h;
(4) after completion of the reaction, by the white emulsion centrifugation obtained, with ethanol and deionized water washing sediment and lyophilize at-68 DEG C, the anatase type nano TiO that size-grade distribution is homogeneous is namely obtained
2monocrystal material.
TiO obtained by the present embodiment
2monocrystal material comprises the nano particle of a large amount of pattern rule, size uniform, good dispersity, and the particle diameter of particle is 31nm, and specific surface area is 74m
2/ g, relative standard deviation is 7%.
Embodiment 7
(1) by the TiCl of 0.5mol/L
4being added drop-wise in the ammonia soln of 100mL 0.12mol/L, is 9.0 to system pH, obtains white " milky " liquid;
(2) the white " milky " liquid centrifuging in step (1) is obtained white precipitate, then with deionized water, washing of precipitate is extremely neutral;
(3) precipitation in step (2) is dispersed in 50mL water (namely the volume ratio of ethanol and water is 0:10), is placed in reactor, at 180 DEG C, reacts 2h;
(4) after completion of the reaction, by the white emulsion centrifuging obtained, washing precipitate lyophilize at-40 DEG C, namely obtain the anatase type nano TiO that size-grade distribution is homogeneous
2monocrystal material.
TiO obtained by the present embodiment
2monocrystal material comprises the nano particle of a large amount of pattern rule, size uniform, good dispersity, and the particle diameter of particle is 30nm, and specific surface area is 75m
2/ g, relative standard deviation is 8%.
Embodiment 8
(1) by the TiCl of 0.15mol/L
4being added drop-wise in the ammonia soln of 100mL 0.3mol/L, is 7.2 to system pH, obtains white " milky " liquid;
(2) the white " milky " liquid gravity settling in step (1) is obtained white precipitate, then with deionized water, washing of precipitate is extremely neutral;
(3) volume ratio precipitation in step (2) being dispersed in 50mL ethanol and water is in the system of 7:3, is placed in reactor, at 110 DEG C, reacts 18h;
(4) after completion of the reaction, the white emulsion gravity settling obtained is precipitated thing, with ethanol and deionized water washing sediment and lyophilize at-85 DEG C, namely obtains the anatase type nano TiO that size-grade distribution is homogeneous
2monocrystal material.
TiO obtained by the present embodiment
2monocrystal material comprises the nano particle of a large amount of pattern rule, size uniform, good dispersity, and the particle diameter of particle is 28nm, and specific surface area is 80m
2/ g, relative standard deviation is 5%.
Embodiment 9
The TiO that embodiment 6 is prepared for the present invention
2monocrystal material (A) is 30nm TiO as catalyzer and business median size
2(B) the photocatalysis effect contrast of catalyzer when degradation of dye methylene blue.0.01g catalyzer is added to 100mL to be contained in the methylene blue solution of 10mg/L, stirs 1h under lucifuge condition, makes to arrive adsorption-desorption balance between catalyzer and dyestuff.Be that the high pressure xenon lamp of 365nm is from external irradiation reactor with emission wavelength.In During Illumination, every 15min sampling, the centrifugal 5min of 8000r/min, gets supernatant liquid and tests in ultraviolet-visible pectrophotometer.The concentration of methylene blue solution corresponds to the absorbancy at 665nm place.Result shows, the TiO prepared with the present invention
2the specific activity business TiO of material catalyzes degradation of methylene blue
2the activity of catalyzer is high.
Applicant states, the present invention illustrates preparation method of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned steps, does not namely mean that the present invention must rely on above-mentioned steps and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of ancillary component, the concrete way choice etc. of raw material selected by the present invention, all drops within protection scope of the present invention and open scope.
Claims (15)
1. a nano-TiO
2the preparation method of monocrystal material, is characterized in that, said method comprising the steps of:
(1) by TiCl
4be added drop-wise in ammonia soln, the system that drops to, for neutral or weakly alkaline, obtains milk sap;
(2) the milk sap solid-liquid separation in step (1) is precipitated, then by washing of precipitate to neutral;
(3) precipitation in step (2) is dispersed in the mixed system of ethanol, water or ethanol and water, is placed in reaction kettle for reaction;
(4) after completion of the reaction, by the white emulsion solid-liquid separation obtained, washing is precipitated thing, and lyophilize, namely obtain the nano-TiO that size-grade distribution is homogeneous
2monocrystal material;
Step (1) described TiCl
4concentration be 0.05 ~ 0.5mol/L, the concentration of described ammonia soln is 0.12 ~ 0.8mol/L;
Reaction times in described step (3) is 2 ~ 18h, and temperature of reaction is 110 ~ 180 DEG C.
2. the method for claim 1, is characterized in that, step (1) described TiCl
4concentration be 0.1 ~ 0.2mol/L.
3. the method for claim 1, is characterized in that, the concentration of step (1) described ammonia soln is 0.2 ~ 0.5mol/L.
4. the method for claim 1, is characterized in that, drips TiCl in step (1)
4in ammonia soln to the pH value of system be 7.2 ~ 9.0.
5. the method as described in any one of claim 1-4, is characterized in that, with deionized water, washing of precipitate is extremely neutral in described step (2).
6. the method as described in one of claim 1-4, is characterized in that, in described step (3), the volume ratio of ethanol and water is 9.9:0.1 ~ 1:1.
7. the method as described in one of claim 1-4, is characterized in that, the reaction times in described step (3) is 3 ~ 15h.
8. the method as described in one of claim 1-4, is characterized in that, the temperature of reaction in described step (3) is 120 ~ 150 DEG C.
9. the method as described in one of claim 1-4, is characterized in that, described step (4) middle ethanol and deionized water washing sediment.
10. the method as described in one of claim 1-4, is characterized in that, in described step (4), cryodesiccated temperature is-85 ~-40 DEG C.
11. methods as described in one of claim 1-4, step (2) comprises centrifugation, precipitation or gravity settling with the solid-liquid separation described in step (4).
12. methods as claimed in claim 11, step (2) is centrifugal settling with the solid-liquid separation described in step (4).
13. methods as described in one of claim 1-4, is characterized in that, said method comprising the steps of:
(1) by the TiCl of 0.1 ~ 0.2mol/L
4be added drop-wise in the ammonia soln of 0.2 ~ 0.5mol/L, dropping to system pH is 8.0, obtains white " milky " liquid;
(2) the white " milky " liquid centrifugation in step (1) is precipitated, then with deionized water, washing of precipitate is extremely neutral;
(3) precipitation in step (2) is dispersed in the mixed system of ethanol, water or ethanol and water, is placed in reactor, at 120 ~ 150 DEG C, react 3 ~ 15h;
(4) after completion of the reaction, by the white emulsion centrifugation obtained, the throw out obtained with ethanol and deionized water wash lyophilize at-75 ~-50 DEG C, namely obtain the nano-TiO that size-grade distribution is homogeneous
2monocrystal material.
14. 1 kinds of nano-TiOs obtained by method as described in one of claim 1-13
2monocrystal material, is characterized in that, described material particle size distribution is homogeneous, median size 30nm, relative standard deviation≤9%.
15. 1 kinds of nano-TiOs as claimed in claim 14
2the purposes of monocrystal material, is characterized in that, by nano-TiO
2monocrystal material is as photocatalyst.
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| CN103877964B (en) * | 2014-03-12 | 2016-09-14 | 浙江大学 | A kind of preparation method of the hetero-junctions of Perovskite Phase lead titanate monocrystal nano line and anatase phase titanium dioxide |
| CN103964502B (en) * | 2014-05-26 | 2016-04-13 | 国家纳米科学中心 | A kind of nano-TiO 2monocrystal material and its preparation method and application |
| CN107324383B (en) * | 2017-07-20 | 2020-07-07 | 国家纳米科学中心 | Nano TiO (titanium dioxide)2Aqueous dispersion, method for producing same and use thereof |
| CN108675345A (en) * | 2018-05-29 | 2018-10-19 | 东北大学 | A kind of titanium dioxide nano hollow ball and preparation method thereof |
| CN111519251B (en) * | 2019-02-01 | 2021-09-21 | 中国科学院福建物质结构研究所 | Titanium dioxide single crystal material and growth method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1237654A (en) * | 1998-06-02 | 1999-12-08 | 南京大学 | Preparation method of monocrystal titanium dioxide nanometer filament |
| CN102140687A (en) * | 2011-03-08 | 2011-08-03 | 华东理工大学 | Preparation method of single-crystal titanium dioxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1237654A (en) * | 1998-06-02 | 1999-12-08 | 南京大学 | Preparation method of monocrystal titanium dioxide nanometer filament |
| CN102140687A (en) * | 2011-03-08 | 2011-08-03 | 华东理工大学 | Preparation method of single-crystal titanium dioxide |
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