CN106064827A - A kind of preparation method of nanometer Zinc oxide powder - Google Patents
A kind of preparation method of nanometer Zinc oxide powder Download PDFInfo
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- CN106064827A CN106064827A CN201610606609.2A CN201610606609A CN106064827A CN 106064827 A CN106064827 A CN 106064827A CN 201610606609 A CN201610606609 A CN 201610606609A CN 106064827 A CN106064827 A CN 106064827A
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- zinc
- zinc oxide
- oxide powder
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention relates to the preparation of zinc oxide, the preparation method of a kind of nanometer Zinc oxide powder, it includes adding zinc nitrate solution stirring reaction in ammonia spirit；Drip ammonium bicarbonate solution reaction, ageing again；Then filter pressing, obtains presoma；Then presoma is dried, calcines, obtain nanometer Zinc oxide powder.The present invention, after zinc nitrate and ammonia react a period of time, generates substantial amounts of zinc hydroxide nucleus and thin crystalline substance, adds ammonium bicarbonate solution and react, and obtains zinc hydroxide nucleus and the composite precursor of thin brilliant outer cladding basic zinc carbonate；When calcining, zinc hydroxide first decomposes, rapid dehydration, and its steam generated can make cladding shell crush so that basic zinc carbonate decomposes, thus prepares nano-scale oxidized zinc powder.
Description
Technical field
The present invention relates to the preparation of Zinc oxide powder, the preparation method of a kind of nanometer Zinc oxide powder.
Background technology
Zinc oxide is a kind of new and high technology material of discovered in recent years, and being that only a few is several can realize quantum size effect
Oxide semiconductor material.Traditional zinc oxide material is widely used in pottery, piezoelectric transducer, catalyst and luminous organ
The fields such as part.Along with the further investigation of nano zine oxide preparation technology, the super-refinement of zinc oxide particles so that it is present tradition oxygen
Change property not available for zinc, such as nontoxic and non-migratory, fluorescence, piezoelectricity, absorption and scatters ultraviolet ability etc.,
Thus have broad application prospects.
For the application of nano-powder, its dispersibility and stability are most important.But owing to nano particle diameter is little,
Specific surface area is big, and interface atoms number is many, there is a large amount of unsaturated bond and dangling bond, and chemism is high, adds intergranular model moral
Hua Li, electrostatic force and surface tension etc., easily make nano-particle form larger-size aggregate.Nano powder after reunion
Body, has excellent specific property by the many losing himself so that it is usefulness cannot give full play to, and also will have a strong impact on nano-powder
Use value and application prospect.At present, the method that the technology of preparing of Zinc oxide powder uses is more, but oxygen prepared by existing method
Change zinc diameter of particle relatively big, be difficult to meet the demand of nano material.
Summary of the invention
For above-mentioned technical problem, the present invention provides the preparation method of the simple nanometer Zinc oxide powder of a kind of technique.
The technical solution used in the present invention is: the preparation method of a kind of nanometer Zinc oxide powder, and it comprises the following steps:
(1) zinc nitrate solution is added stirring reaction in ammonia spirit；
(2) ammonium bicarbonate solution reaction, ageing are dripped again；
(3) then filter pressing, obtains presoma；
(4) then presoma is dried, calcines, obtain nanometer Zinc oxide powder.
As preferably, zinc nitrate is 1:(1 1.2 with the ratio of the amount of the material of ammonia), zinc nitrate and ammonium hydrogencarbonate material
The ratio of amount be 1:(1.2 1.4).
As preferably, nitric acid zinc concentration is 1.5 2.5mol/L, and the concentration of ammonia spirit is 8 10mol/L, carbonic acid
Hydrogen ammonia solution concentration is 1 1.5mol/L.
As preferably, zinc nitrate solution adds stirring reaction 4 6min in ammonia spirit.
As preferably, ammonium bicarbonate solution is added dropwise to complete in 2 4min.
As preferably, digestion time is 20 30min.
As preferably, temperature when presoma is dried is 70 90 DEG C.
As preferably, temperature during calcining is 300 350 DEG C, and the time is 50 70min.
As can be known from the above technical solutions, the present invention, after zinc nitrate and ammonia react a period of time, generates substantial amounts of hydrogen-oxygen
Change zinc nucleus and thin crystalline substance, add ammonium bicarbonate solution and react, obtain zinc hydroxide nucleus and thin brilliant outer cladding alkali formula carbon
The composite precursor of acid zinc；When calcining, zinc hydroxide first decomposes, rapid dehydration, and its steam generated can make cladding shell break
Broken so that basic zinc carbonate decomposes, thus prepare nano-scale oxidized zinc powder.
Detailed description of the invention
The present invention is described more detail below, and illustrative examples and explanation in this present invention are used for explaining the present invention,
But it is not as a limitation of the invention.
A kind of preparation method of nanometer Zinc oxide powder, it comprises the following steps:
First, zinc nitrate solution is added stirring reaction, response time about 4 6min in ammonia spirit, thus can generate a large amount of
Zinc hydroxide nucleus and thin brilliant；Drip ammonium bicarbonate solution reaction, ageing again；Wherein the amount of the material of zinc nitrate and ammonia it
Than being 1:(1 1.2), zinc nitrate is 1:(1.2 1.4 with the ratio of the amount of ammonium hydrogencarbonate material), and nitric acid zinc concentration is
1.5 2.5mol/L, the concentration of ammonia spirit is 8 10mol/L, and ammonium bicarbonate solution concentration is 1 1.5mol/L；In employing
Stating concentration and proportioning, the solute degree of supersaturation concentration that zinc nitrate can be made to be formed after adding ammonia spirit is big so that substantial amounts of hydrogen-oxygen
Change zinc crystal seed to separate out rapidly, cause solute concentration to reduce rapidly, thus obtain the most tiny granule；In implementation process, carbon
Acid hydrogen ammonia solution should be added dropwise to complete in 2 4min, and basic zinc carbonate so can be promoted to separate out zinc hydroxide nucleus with thin
It is coated with rapidly deposition on crystalline substance, thus shortens the response time, it is to avoid interparticle coagulation is grown up.
In the present invention, when zinc nitrate reacts with ammonia and ammonium hydrogencarbonate, protective layer can be produced at particle surface, and be aged and have
Helping formation and the reinforcing of protective layer, general digestion time is 20 30min；After ageing, carry out filter pressing, obtain compound precursor
Body；Finally being dried by presoma, calcine, obtain nanometer Zinc oxide powder, temperature when presoma is dried is 70 90 DEG C, calcining
Time temperature be 300 350 DEG C, the time is 50 70min.Being dried to make the particle diameter of product become less, and calcining can make alkali formula
Zinc carbonate decomposes, and reaches the Zinc oxide particles of relatively small particle.
Embodiment 1
The zinc nitrate solution of 1.5mol/L is added stirring reaction about 4 in the ammonia spirit of 8mol/L, then drips the carbon of 1mol/L
Acid hydrogen ammonia solution reacts, and ammonium bicarbonate solution is added dropwise to complete in 2min, and the ratio of zinc nitrate and the amount of the material of ammonia
For 1:1, zinc nitrate is 1:1.2 with the ratio of the amount of ammonium hydrogencarbonate material, is then aged 20min, then filter pressing, obtains compound precursor
Body；Then composite precursor is dried at a temperature of 70 DEG C, finally with the temperature calcination 50min of 300 DEG C, obtains oxide powder and zinc
Body.The particle diameter recording Zinc oxide powder is 46.3nm.
Embodiment 2
The zinc nitrate solution of 2mol/L is added stirring in the ammonia spirit of 9mol/L and reacts about 5min, then drip 1.2mol/L's
Ammonium bicarbonate solution reacts, and ammonium bicarbonate solution is added dropwise to complete in 3min, and the amount of the material of zinc nitrate and ammonia it
Ratio is 1:1.1, and zinc nitrate and the ratio of the amount of ammonium hydrogencarbonate material are 1:1.3, are then aged 250min, then filter pressing, are combined
Presoma；Then composite precursor is dried at a temperature of 80 DEG C, finally with the temperature calcination 60min of 320 DEG C, is aoxidized
Zinc powder body.The particle diameter recording Zinc oxide powder is 33.5nm.
Embodiment 3
The zinc nitrate solution of 2.5mol/L is added stirring in the ammonia spirit of 10mol/L and reacts about 6min, then drip 1.5mol/
The ammonium bicarbonate solution of L reacts, and ammonium bicarbonate solution is added dropwise to complete in 4min, and the amount of the material of zinc nitrate and ammonia
Ratio be 1:1.2, zinc nitrate is 1:1.4 with the ratio of the amount of ammonium hydrogencarbonate material, is then aged 30min, then filter pressing, is combined
Presoma；Then composite precursor is dried at a temperature of 90 DEG C, finally with the temperature calcination 70min of 350 DEG C, is aoxidized
Zinc powder body.The particle diameter recording Zinc oxide powder is 38.7nm.
The technical scheme provided the embodiment of the present invention above is described in detail, specific case used herein
Principle and embodiment to the embodiment of the present invention are set forth, and the explanation of above example is only applicable to help to understand this
The principle of inventive embodiments；Simultaneously for one of ordinary skill in the art, according to the embodiment of the present invention, in specific embodiment party
All will change in formula and range of application, in sum, this specification content should not be construed as limitation of the present invention.
Claims (8)
1. a preparation method for nanometer Zinc oxide powder, it comprises the following steps:
(1) zinc nitrate solution is added stirring reaction in ammonia spirit；
(2) ammonium bicarbonate solution reaction, ageing are dripped again；
(3) then filter pressing, obtains presoma；
(4) then presoma is dried, calcines, obtain nanometer Zinc oxide powder.
The preparation method of nanometer Zinc oxide powder the most according to claim 1, it is characterised in that: zinc nitrate and the material of ammonia
The ratio of amount be 1:(1 1.2), zinc nitrate is 1:(1.2 1.4 with the ratio of the amount of ammonium hydrogencarbonate material).
3. the preparation method of nanometer Zinc oxide powder as claimed in claim 1, it is characterised in that: nitric acid zinc concentration is 1.5
2.5mol/L, the concentration of ammonia spirit is 8 10mol/L, and ammonium bicarbonate solution concentration is 1 1.5mol/L.
4. the preparation method of nanometer Zinc oxide powder as claimed in claim 1, it is characterised in that: it is molten that zinc nitrate solution adds ammonia
Stirring reaction 4 6min in liquid.
5. the preparation method of nanometer Zinc oxide powder as claimed in claim 1, it is characterised in that: ammonium bicarbonate solution is 2
It is added dropwise to complete in 4min.
6. the preparation method of nanometer Zinc oxide powder as claimed in claim 1, it is characterised in that: digestion time is 20 30min.
7. the preparation method of nanometer Zinc oxide powder as claimed in claim 1, it is characterised in that: temperature when presoma is dried is
70—90℃。
8. the preparation method of nanometer Zinc oxide powder as claimed in claim 1, it is characterised in that: temperature during calcining is 300
350 DEG C, the time is 50 70min.
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| CN201610606609.2A CN106064827A (en) | 2016-07-29 | 2016-07-29 | A kind of preparation method of nanometer Zinc oxide powder |
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| CN201610606609.2A CN106064827A (en) | 2016-07-29 | 2016-07-29 | A kind of preparation method of nanometer Zinc oxide powder |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109850933A (en) * | 2019-01-08 | 2019-06-07 | 西南科技大学 | A kind of preparation method of the zinc oxide nano-particle for bio-imaging |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1296041A (en) * | 2000-11-30 | 2001-05-23 | 上海博纳科技发展有限公司 | Process for preparing nanometer zinc oxide |
| CN1396117A (en) * | 2002-06-13 | 2003-02-12 | 山东小鸭集团有限责任公司 | Process for preparing nano zinc oxide |
| CN101767813A (en) * | 2010-01-07 | 2010-07-07 | 西北稀有金属材料研究院 | Preparation method of flaky nanometer zinc oxide powder |
| CN102795659A (en) * | 2012-07-30 | 2012-11-28 | 西安理工大学 | Method for preparing rod-like zinc oxide nano-crystals |
-
2016
- 2016-07-29 CN CN201610606609.2A patent/CN106064827A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1296041A (en) * | 2000-11-30 | 2001-05-23 | 上海博纳科技发展有限公司 | Process for preparing nanometer zinc oxide |
| CN1396117A (en) * | 2002-06-13 | 2003-02-12 | 山东小鸭集团有限责任公司 | Process for preparing nano zinc oxide |
| CN101767813A (en) * | 2010-01-07 | 2010-07-07 | 西北稀有金属材料研究院 | Preparation method of flaky nanometer zinc oxide powder |
| CN102795659A (en) * | 2012-07-30 | 2012-11-28 | 西安理工大学 | Method for preparing rod-like zinc oxide nano-crystals |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109850933A (en) * | 2019-01-08 | 2019-06-07 | 西南科技大学 | A kind of preparation method of the zinc oxide nano-particle for bio-imaging |
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