CN1217734C - Method for preparing nano titanium oxynitrides by plasma process - Google Patents
Method for preparing nano titanium oxynitrides by plasma process Download PDFInfo
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- CN1217734C CN1217734C CN 03119056 CN03119056A CN1217734C CN 1217734 C CN1217734 C CN 1217734C CN 03119056 CN03119056 CN 03119056 CN 03119056 A CN03119056 A CN 03119056A CN 1217734 C CN1217734 C CN 1217734C
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- titanium oxide
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- titanium dioxide
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Abstract
The present invention relates to a method using a plasma method to prepare nanometer nitrogen heterocyclic titanium oxide. The method is characterized in that nanometer titanium dioxide is placed in a microwave plasma generator; after vacuum is pumped, nitrogen is filled into the microwave plasma generator to generate nitrogen plasma so as to process the nanometer titanium dioxide; the nanometer nitrogen heterocyclic titanium oxide is prepared. The photocatalytic performance of the prepared nanometer nitrogen heterocyclic titanium oxide is better than that of nanometer titanium dioxide. The method has the characteristics of short reaction time, low reaction temperature and no need of catalysts.
Description
Technical field
The present invention relates to modified Nano material field, particularly a kind of method for preparing nanometer aza-titanium oxide with plasma method.
Background technology
Nanometer anatase titania can decompose toxic chemical, smog residue, stench chemicals, foul, stimulus, bacterium or the like through UV-irradiation and be nontoxic, free of contamination material, (electronics the during irradiation of wavelength＜388nm) in its valence band is excited and forms electronegative high activity electronics when ultraviolet light, produce the valence band hole of positively charged simultaneously, electronics separates with the hole, moves to the diverse location of particle surface.Hole and electronics produce the hydroxyl radical free radical and the superoxide ion free radical of high reaction activity respectively with the water on surface and oxygen reaction, these free radicals can decompose toxic chemical effectively.Therefore, cause people's very big interest, wish to utilize this photocatalysis characteristic to solve the earth environment pollution problem that increasingly sharpens.
Nanometer anatase titania only just has catalysis under UV-irradiation, and the content of natural daylight medium ultraviolet light very little, only account for the 4-6% of the solar radiation total amount that reaches ground, and along with the time changes obviously, artificial produce ultraviolet light power consumption greatly, also need drop into the higher device expense, the expense of large-area ultraviolet irradiation is higher even be difficult to realize.Utilize scope if can expand the spectrum of photochemical catalyst, with sunshine as light source, equipment investment and operating cost are reduced greatly, make that decontamination etc. becomes possibility in natural environment, also create condition as the immobilized material of nano-photocatalyst material for macromolecular material.In order to realize this grand target, a lot of scholars have carried out the research work in this field.
Wang C M, Choi, Anpo etc. attempt adopting transient metal doped TiO
2The preparation catalysis material has obviously improved ultraviolet catalytic efficient, but does not realize the visible light catalytic function.
Asahi (Science, 2001,293 (5528): the 269) N of employing 30%
2/ Ar mist is handled nanometer anatase titania TiO
2Film or adopt 67% NH
3/ Ar mist is handled anatase titanium dioxide TiO
2Nano powder 4 hours has prepared aza-titanium oxide TiO respectively
2-xN
xNano thin-film and nano powder.This nano material is to make acetaldehyde etc. be decomposed into carbon dioxide and water under the illumination of wavelength＜500nm is penetrated at visible light.But this method reaction time is long, and needs argon gas, thereby cost is too high.
Plasma is meant the mixture of being made up of electronics, cation and neutral particle, is called the 4th kind of state of material usually again.The energy of various spikes that is in plasma state is quite high, when molecule is exposed in the environment of plasma, this energy is enough to cause the fracture of chemical bond, the using plasma technology can prepare the material that usual method is difficult to prepare, for example, can carry out the nitrogenize of the synthetic and metal ion of titanium nitride TiN by nitrogen plasma.
Summary of the invention
The objective of the invention is the deficiency that reaction time is long and manufacturing cost is high, utilize the advantage of plasma technique, and a kind of method for preparing nanometer aza-titanium oxide with plasma method is provided at the existence of prior art.The characteristics of this method are: 1. the reaction time lacked, less than 1 hour; 2. reaction temperature is low, less than 500 ℃; 3. need not catalyst; 4. Zhi Bei nanometer aza-titanium oxide has the better photocatalysis performance of ratio nano titanium dioxide.
The objective of the invention is to adopt following technical measures to realize:
Nano titanium oxide is put into microwave plasma generation device, be evacuated to vacuum less than 50 millimetress of mercury after, logical nitrogen is to microwave plasma generation device, regulate nitrogen flow rate 1-60 cubic centimetre/minute, microwave power 300-1000W, temperature 200-500 ℃, radiation treatment 1-60 minute, promptly get nanometer aza-titanium oxide.
Prepare with plasma method that nano titanium oxide can be nano-titanium dioxide powder, nano-titanium dioxide film or TiO 2 porous material described in the method for nanometer aza-titanium oxide.
The present invention has following advantage: (1) reaction time was short, less than 1 hour; (2) reaction temperature is low, less than 500 ℃; (3) need not catalyst; (4) Zhi Bei nanometer aza-titanium oxide has good photocatalytic, contains 10 milliliter 1% methyl orange solution of 0.5 gram nanometer aza-titanium oxide, 30-50min under solar light irradiation, and its color retreats to colourless.
The experiment of chromate photocatalytic degradation rate shows, adopt the aza-titanium oxide of the present invention's preparation to have good photocatalytic (seeing the following form) than unmodified titanium dioxide, absorbance is more little, and chromate concentration is few more in the system, the chromate that is degraded is many more, and photocatalysis performance is good more.Take by weighing the 0.5g aza-titanium oxide in the 50mL beaker, drip 1.6mLCr
2O
7 2-Behind the solution (Cr (VI) content 0.08g/L), fluorescent high voltage mercury lamp radiation 8min, also cooling is taken out in the back, adds water 15mL then and shakes up, and centrifugal sedimentation is got the 10mL supernatant liquor and is changed the 25mL colorimetric cylinder over to, adds 0.3mL H
2SO
4(1: 1) and 2mLH
3PO
4, shake up and leave standstill, add 0.5mL diphenylcarbazide (DCPI) again, rapidly water is rare to 25mL, shakes up immediately, puts into 721 type spectrophotometers after leaving standstill 5min, in wavelength 540nm place mensuration solution absorbency; Unmodified titanium dioxide adopts above method to carry out same experiment to make comparisons.Its absorbance data row are as following table.
Aza-titanium oxide and unmodified optically catalytic TiO 2 experimental data
| Sample type | Absorbance A |
| The unmodified titanium dioxide of the unmodified titanium dioxide of aza-titanium oxide (20nm) aza-titanium oxide (10nm) (20nm) (10nm) | 0.28 0.08 1.05 0.92 |
Embodiment 1
With granularity is that the titanium dioxide powder of 20 nanometers is put into the microwave plasma chemical gaseous phase deposition device, after being evacuated to vacuum 45 millimetress of mercury, regulating nitrogen flow is 50 cc/min, 500 ℃ of temperature, microwave power is 450W, reacts promptly to get product in 30 minutes.It is faint yellow that product is, and shows with elementary analysis, and nitrogen element content is 0.35%, takes by weighing this powder 0.2 and restrain in 10 milliliter 1% methyl orange solution, and with 30min under the solar light irradiation, its color retreats to colourless.
Embodiment 2
The titanium deoxid film of thickness 80 nanometers is put into the microwave plasma chemical gaseous phase deposition device, after being evacuated to vacuum 45 millimetress of mercury, regulating nitrogen flow is 1 cc/min, 200 ℃ of temperature, microwave power is 1000W, reacts promptly to get product in 60 minutes.It is faint yellow that product is, and shows with elementary analysis, and nitrogen element content is 0.10%, takes by weighing this film 0.2 and restrain in 10 milliliter 1% methyl orange solution, uses solar light irradiation 50min, and its color retreats to colourless.
Embodiment 3
Poriferous titanium dioxide is put into the microwave plasma chemical gaseous phase deposition device, be evacuated to vacuum 45 millimetress of mercury after, regulating nitrogen flow is 30 cc/min, 300 ℃ of temperature, microwave power is 300W, reacts promptly to get product in 20 minutes.It is faint yellow that product is, and shows with elementary analysis, and nitrogen element content is 0.10%, takes by weighing this product 0.2 and restrain in 10 milliliter 1% methyl orange solution, uses solar light irradiation 50min, and its color retreats to colourless.
Claims (2)
1, a kind of method for preparing nanometer aza-titanium oxide with plasma method, it is characterized in that: nano titanium oxide is put into microwave plasma generation device, be evacuated to vacuum less than 50 millimetress of mercury after, logical nitrogen is to microwave plasma generation device, regulate nitrogen flow rate 1-60 cubic centimetre/minute, microwave power 300-1000W, temperature 200-500 ℃, radiation treatment 1-60 minute, promptly get nanometer aza-titanium oxide.
2, the method for preparing nanometer aza-titanium oxide according to claim 1 is characterized in that nano titanium oxide is nano-titanium dioxide powder, nano-titanium dioxide film or TiO 2 porous material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03119056 CN1217734C (en) | 2003-05-13 | 2003-05-13 | Method for preparing nano titanium oxynitrides by plasma process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03119056 CN1217734C (en) | 2003-05-13 | 2003-05-13 | Method for preparing nano titanium oxynitrides by plasma process |
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| Publication Number | Publication Date |
|---|---|
| CN1451474A CN1451474A (en) | 2003-10-29 |
| CN1217734C true CN1217734C (en) | 2005-09-07 |
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| CN 03119056 Expired - Fee Related CN1217734C (en) | 2003-05-13 | 2003-05-13 | Method for preparing nano titanium oxynitrides by plasma process |
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1304114C (en) * | 2004-02-06 | 2007-03-14 | 华东理工大学 | Method for preparing nanometer TiO(2-x)N(x) photocatalyst and fluidized bed reactor |
| CN100360425C (en) * | 2005-11-15 | 2008-01-09 | 武汉化工学院 | Method for preparing nanometer aza-titanium oxide by using micro-wave radiation |
| US7967891B2 (en) * | 2006-06-01 | 2011-06-28 | Inco Limited | Method producing metal nanopowders by decompositon of metal carbonyl using an induction plasma torch |
| CN100463861C (en) * | 2007-01-18 | 2009-02-25 | 武汉工程大学 | Method of preparing ordered porous titanium oxide doped with nitrogen |
| CN100441289C (en) * | 2007-04-24 | 2008-12-10 | 武汉工程大学 | Method for preparing aza-titanium oxide/fluorine-containing polymer kernel-hull composite ordered porous microspheres |
| CN102974378A (en) * | 2012-10-22 | 2013-03-20 | 复旦大学 | Preparation method for high-efficiency nitrogen-doped strontium titanate photocatalyst |
| CN104174391A (en) * | 2014-08-21 | 2014-12-03 | 华中科技大学 | Nanometer titania photocatalyst for degrading VOC and preparation method of nanometer titania photocatalyst for degrading VOC |
| CN108371954A (en) * | 2018-03-30 | 2018-08-07 | 华南农业大学 | A kind of support type Ag-TiO2/Ti(NO2) film catalyst and its fruit storage in application |
| CN108355470A (en) * | 2018-03-30 | 2018-08-03 | 华南农业大学 | A kind of Ag-TiO2/Ti(NO2)/ITO optoelectronic poles, electrical enhanced photocatalysis reaction unit and its application |
| CN112582626B (en) * | 2020-12-22 | 2022-03-25 | 北京理工大学深圳汽车研究院(电动车辆国家工程实验室深圳研究院) | Method for improving electrocatalytic activity of perovskite oxide and substance thereof |
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2003
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Granted publication date: 20050907 Termination date: 20100513 |