CN103252251A - Preparation method of co-doped ZnO nano material - Google Patents
Preparation method of co-doped ZnO nano material Download PDFInfo
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- CN103252251A CN103252251A CN2013102095868A CN201310209586A CN103252251A CN 103252251 A CN103252251 A CN 103252251A CN 2013102095868 A CN2013102095868 A CN 2013102095868A CN 201310209586 A CN201310209586 A CN 201310209586A CN 103252251 A CN103252251 A CN 103252251A
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Abstract
The invention relates to the preparation of a semiconductor nano photo-catalytic material and particularly relates to a preparation method of a lanthanum-nitrogen co-doped ZnO nano material. The preparation method comprises the following steps of: firstly, obtaining a sediment by utilizing certain mol ratios of zinc nitrate hexahydrate (Zn(NO3)2*6H2O), lanthanum nitrate hexahydrate (La(NO3)3*6H2O) and sodium carbonate (Na2CO3) solutions by utilizing a co-precipitation method; then preparing lanthanum-doped ZnO by utilizing a heating treatment method; and finally, preparing the lanthanum-nitrogen co-doped ZnO nano material through a method for annealing in a pipe type furnace introduced with ammonia. The preparation method disclosed by the invention is simple in process, short in flow and stable in product quality; and production and application can be easily realized.
Description
Technical field
The present invention relates to the preparation method of semiconductor nano material, the preparation method of the nitrogen co-doped ZnO of especially a kind of lanthanum.
Background technology
In recent years, indoor used chemical industry article can cause room air pollution to release volatile organic matter in the air.From room air, detected hundreds of kind organic matter (for example formaldehyde etc.) at present.Formaldehyde is the important component part of adhesive, so every adhesive that relates to comprises that wood-based plate, coating, carpet, furniture all can contain formaldehyde.Formaldehyde is very harmful to human body, and a large amount of suctions also may cause death.The survey showed that, and some organic concentration is higher than outdoorly in room air, even is higher than the industrial area.In order to improve people's quality of life, the efficient catalysis material of removing indoor organic pollution of development has important practical significance, and has therefore all caused in academia and industrial circle and has studied interest and concern widely.
ZnO receives publicity owing to have the performance of cheap, nontoxic and good light degradation organic pollution.Yet its band gap width is big (3.2eV) too, therefore can not responding to visible light.In order effectively to utilize solar energy or room lighting light source, the photoresponse scope of ZnO is extended to visible light just has very important significance.The nitrogen doping techniques is a kind of effective ways that are used for researching and developing the visible light responsive photocatalytic material.But its N
3-Replace O
2-Can cause defective, and defective is usually as meeting the center and then can reducing photocatalytic activity.In this, the invention provides a kind of codope ZnO preparation of nanomaterials, ZnO and N, La are carried out doped and compounded, utilize the interface coupling effect, widen the spectral response range of photochemical catalyst, improve solar energy utilization rate; Also utilize simultaneously the high conductivity of ZnO particle, suppress the compound of photo-generated carrier, realize separating of hole and light induced electron better, improve the activity of photochemical catalyst.
Summary of the invention
[0003] the invention provides the preparation method of the nitrogen co-doped ZnO of lanthanum.
The present invention is accomplished by following technical solution:
(1) certain mol proportion example zinc nitrate hexahydrate (Zn (NO
3)
26H
2O) and lanthanum nitrate (La (NO
3)
36H
2O) adding the distilled water compound concentration is the solution of 0.5mol/L.
(2) be placed on magnetic force heating stirrer (40 ℃) upward and continue stirring, slowly adding concentration is the sodium carbonate (Na of 0.5mol/L simultaneously
2CO
3) solution.At Na
2CO
3After solution adds fully, stir 0.5h again.
(3) white precipitate with gained filters, and uses distilled water and alcohol flushing 4-6 time.Afterwards sediment is put into the dry 5h of baking oven (100 ℃).
(4) presoma of gained is calcined 2h down at 300 ℃, thereby obtain the ZnO that lanthanum mixes.
(5) ZnO powder of lanthanum doping (500 ℃) annealing 1h in the tube furnace that feeds ammonia.When furnace temperature is down to 380 ℃, substitute ammonia with nitrogen, sample is lowered the temperature naturally.
(6) powder that obtains lowers the temperature sample behind (400 ℃) calcining 2h in high temperature furnace naturally.Behind roasting in air atmosphere then (300 ℃) the sample 1h it is lowered the temperature naturally, obtained the nitrogen co-doped ZnO material of lanthanum.
The nitrogen co-doped ZnO of lanthanum of the present invention adopts two-step method synthetic.At first the co-precipitation after-baking method that adopts realizes La
3+Doping ZnO, and then adopt the method doping N that in the tube furnace that feeds ammonia, anneals
3-Ion.Obtained the nitrogen co-doped ZnO of lanthanum.Method of the present invention is made simpler, and good quality of product is easy to realize industrialization.
Description of drawings
Fig. 1 is the ultraviolet-visible absorption spectroscopy of invention compound.
The specific embodiment
The specific embodiment one: 11.934g Zn (NO
3)
26H
2It is the solution of 0.5mol/L that O adds distilled water configuration 80mL concentration, stirs 0.5h under the normal temperature, is placed on magnetic force heating stirrer (40 ℃) more upward and continues and stir.Add the Na by 3.326g simultaneously
2CO
3The 80mL concentration that is made into is the solution of 0.5mol/L, add stirred 0.5h again in 8 minutes after, add (the NO by 0.0346g La again
3)
36H
2The solution that O is made into stirred 20 minutes.With the sedimentation and filtration of gained, use distilled water flushing twice then, and with alcohol flushing four times.Afterwards sediment is placed on dry 5h in the baking oven (100 ℃).The presoma of gained is calcined 2h down at 300 ℃, thereby obtain the ZnO that lanthanum mixes.The ZnO powder that lanthanum mixes is (500 ℃) annealing 1h in the tube furnace that feeds ammonia.When furnace temperature is down to 380 ℃, substitute ammonia with nitrogen, sample is lowered the temperature naturally.The powder that obtains lowers the temperature sample calcine 2h in high temperature furnace (400 ℃) after naturally.Behind roasting in air atmosphere then (300 ℃) the sample 1h it is lowered the temperature naturally, obtain the nitrogen co-doped ZnO material of lanthanum, be labeled as ZnO-N-0.2%La.
The specific embodiment two: one preparation method is similar to the specific embodiment, the difference is that Zn (NO
3)
26H
2The quality of O is 11.890g, La (NO
3)
36H
2The quality of O is 0.077g.Finally obtain the nitrogen co-doped ZnO material of lanthanum, be labeled as ZnO-N-0.5%La.
The specific embodiment three: one preparation method is similar to the specific embodiment, the difference is that Zn (NO
3)
26H
2The quality of O is 11.862g, La (NO
3)
36H
2The quality of O is 0.1384g.Finally obtain the nitrogen co-doped ZnO material of lanthanum, be labeled as ZnO-N-0.8%La.
The specific embodiment four: one preparation method is similar to the specific embodiment, the difference is that Zn (NO
3)
26H
2The quality of O is 11.412g, La (NO
3)
36H
2The quality of O is 0.865g.Finally obtain the nitrogen co-doped ZnO material of lanthanum, be labeled as ZnO-N-5%La.
Claims (6)
1. nitrogen co-doped ZnO preparation of nanomaterials of lanthanum.It is characterized in that preparation may further comprise the steps: (1) zinc nitrate hexahydrate (Zn (NO
3)
26H
2O) and lanthanum nitrate hexahydrate (La (NO
3)
36H
2O) adding distilled water preparation 80mL concentration according to the certain molar ratio example is the solution of 0.5mol/L.(2) be placed on magnetic force heating stirrer (40 ℃) upward and continue stirring, slowly adding 80mL concentration is the sodium carbonate (Na of 0.5mol/L simultaneously
2CO
3) solution.At Na
2CO
3After solution adds fully, stir 0.5h again.(3) white precipitate with gained filters, and uses distilled water and alcohol flushing 4-6 time.Afterwards sediment is put into the dry 5h of baking oven (100 ℃).(4) presoma of gained is calcined 2h down at 300 ℃, thereby obtain the ZnO that lanthanum mixes.(5) ZnO powder of lanthanum doping (500 ℃) annealing 1h in the tube furnace that feeds ammonia.When furnace temperature is down to 380 ℃, substitute ammonia with nitrogen, sample is lowered the temperature naturally.(6) powder that obtains lowers the temperature sample behind (400 ℃) calcining 2h in high temperature furnace naturally.Behind roasting in air atmosphere then (300 ℃) the sample 1h it is lowered the temperature naturally, obtained the nitrogen co-doped ZnO material of lanthanum.
2. the method for claim 1 is characterized in that used reactant is Na
2CO
3, Zn (NO
3)
26H
2O and La (NO
3)
36H
2O.
3. the method for claim 1, the temperature that it is characterized in that co-precipitation is 40 ℃.Stir 0.5～2h.
4. the method for claim 1 is characterized in that the sediment of gained is calcined 2h down at 300 ℃, thereby obtains the ZnO that lanthanum mixes.
5. the method for claim 1 is characterized in that the method that nitrogen doping employing is annealed in the tube furnace that feeds ammonia.500 ℃ of temperature, annealing 1h.
6. the method for claim 1 is characterized in that powder temperature is 300 ℃ to the heat treatment 1h in air of the sample behind the nitrogen treatment.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105727963A (en) * | 2016-04-18 | 2016-07-06 | 盐城工学院 | Fe and Cu co-doped nano-sized ZnO photocatalyst and preparation method thereof |
| CN106673640A (en) * | 2016-12-15 | 2017-05-17 | 陕西科技大学 | Barium ferrite / zinc oxide composite wave-absorbing material and preparation method thereof |
| CN107597093A (en) * | 2017-07-31 | 2018-01-19 | 吉林师范大学 | A kind of nano-particles self assemble Chinese herbaceous peony shape La3+Adulterate ZnO and its preparation method and application |
| CN108067283A (en) * | 2018-01-30 | 2018-05-25 | 清华大学深圳研究生院 | Nitrogen co-doped Zinc oxide-base catalysis material of niobium and its preparation method and application |
| CN110052272A (en) * | 2019-04-23 | 2019-07-26 | 北京化工大学 | The preparation method and applications of Co doping zinc oxide nanometer floral material |
| CN110227437A (en) * | 2019-06-24 | 2019-09-13 | 塔里木大学 | A kind of La doping ZnO catalyst and the preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1779913A (en) * | 2004-11-25 | 2006-05-31 | 中国科学院半导体研究所 | Preparation of P-type zinc oxide semiconductor film materials by strain modification dosing process |
| JP2011173102A (en) * | 2010-02-25 | 2011-09-08 | Mitsubishi Chemicals Corp | Photocatalyst for water photolysis reaction and method for producing the same |
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2013
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Patent Citations (2)
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|---|---|---|---|---|
| CN1779913A (en) * | 2004-11-25 | 2006-05-31 | 中国科学院半导体研究所 | Preparation of P-type zinc oxide semiconductor film materials by strain modification dosing process |
| JP2011173102A (en) * | 2010-02-25 | 2011-09-08 | Mitsubishi Chemicals Corp | Photocatalyst for water photolysis reaction and method for producing the same |
Non-Patent Citations (2)
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|---|
| ZONGBAO YU ET AL.: "Crystallinity-dependent substitutional nitrogen doping in ZnO and its improved visible light photocatalytic activity", 《JOURNAL OF COLLOID AND INTERFACE SCIENCE》 * |
| 牛新书等: "掺杂La3+纳米ZnO的制备及其光催化性能", 《化工环保》 * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105727963A (en) * | 2016-04-18 | 2016-07-06 | 盐城工学院 | Fe and Cu co-doped nano-sized ZnO photocatalyst and preparation method thereof |
| CN105727963B (en) * | 2016-04-18 | 2018-05-18 | 盐城工学院 | A kind of Fe, Cu co-doped nano ZnO photocatalyst and preparation method thereof |
| CN106673640A (en) * | 2016-12-15 | 2017-05-17 | 陕西科技大学 | Barium ferrite / zinc oxide composite wave-absorbing material and preparation method thereof |
| CN107597093A (en) * | 2017-07-31 | 2018-01-19 | 吉林师范大学 | A kind of nano-particles self assemble Chinese herbaceous peony shape La3+Adulterate ZnO and its preparation method and application |
| CN107597093B (en) * | 2017-07-31 | 2019-08-02 | 吉林师范大学 | A kind of nano-particles self assemble Chinese herbaceous peony shape La3+Adulterate ZnO and its preparation method and application |
| CN108067283A (en) * | 2018-01-30 | 2018-05-25 | 清华大学深圳研究生院 | Nitrogen co-doped Zinc oxide-base catalysis material of niobium and its preparation method and application |
| CN108067283B (en) * | 2018-01-30 | 2020-10-09 | 清华大学深圳研究生院 | Niobium-nitrogen co-doped zinc oxide-based photocatalytic material and preparation method and application thereof |
| CN110052272A (en) * | 2019-04-23 | 2019-07-26 | 北京化工大学 | The preparation method and applications of Co doping zinc oxide nanometer floral material |
| CN110227437A (en) * | 2019-06-24 | 2019-09-13 | 塔里木大学 | A kind of La doping ZnO catalyst and the preparation method and application thereof |
| CN110227437B (en) * | 2019-06-24 | 2021-11-23 | 塔里木大学 | La-doped ZnO catalyst and preparation method and application thereof |
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Application publication date: 20130821 |