CN102408124A - Method for preparing zinc oxide nanometer sheet based on zinc oxide nanometer rod array - Google Patents
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Abstract
The invention relates to a method for preparing zinc oxide nanometer sheet based on zinc oxide nanometer rod array, which comprises the following steps of: preparing a vertically grown zinc oxide nanometer rod array layer on a clean plane substrate; configuring growth solution containing 0.025mol/L of zinc ions; mixing the following three solutions with molar concentration of 0.1mol/L: zinc salt solution, organic amine solution and solution of metal salt except for zinc salt in the volume ratio of 1 : 1 : 1 to 1 : 3 : 1, and placing in a high pressure reaction kettle; obliquely downwardly or vertically placing substrate with zinc oxide nanometer rod material in the growth solution; placing the high pressure reaction kettle in a constant temperature drying box, and reacting for 2-5h at 100-200 degrees centigrade; and taking out the substrate, repeatedly washing by de-ionized water, naturally drying, and heating at 200-600 degrees centigrade to obtain ultrathin zinc oxide nanometer sheet material with uniform shape, close arrangement, nanometer thickness and square micron area. The invention is simple to operate, environment-friendly, high-efficiency and high in crystallinity, and can prepare large area nanometer sheet and effectively improve photoelectric conversion efficiency.
Description
Technical field
The present invention relates to a kind of method for preparing Zinc oxide nano sheet based on nanometic zinc oxide rod array.Be used for technical fields such as photoelectricity, photochemical catalysis, self-cleaning, sensing.
Background technology
The nano zine oxide of yardstick between 1～100nm; It is a kind of novel high function fine inorganic material geared to the 21st century; Show many special nature; Like non-migrating property, fluorescence, piezoelectricity, absorption and scatters ultraviolet ability etc.; Utilize its marvellous performance, can make gas sensor, fluor, varistor, ultraviolet shielding material, image recording material, piezoelectric, voltage dependent resistor, effective catalyst, magneticsubstance and plastics film etc. at aspects such as light, electricity, magnetic, sensitivities.Zinc oxide is countries nowadays high-tech research and one of most important optoelectronic semiconductor material in exploitation field, forward position, and the countries in the world scientist has dropped into big quantity research with great enthusiasm in succession.
(patent No.: 200510122642.X) mention in [CN 100509998C 2009.7.8] application specification: compound concentration is the zinc nitrate hexahydrate of 0.1 mol and the dimethyamine borane precursor solution that concentration is 0.025～0.05 mol to the Chinese invention patent of announcing on May 30th, 2007 " having Zinc oxide nano sheet film materials of UV luminescent characteristics and preparation method thereof "; On silicon chip; Under 70～80 degrees celsius; Reacted 2～4 hours, and prepared a kind of Zinc oxide nano sheet.But in this invention process, require too strictness for substrate, need under the condition of the concentrated sulfuric acid, increase the danger of preparation process like this, simultaneously, in the required reagent, dimethyamine borane costs an arm and a leg, and scarcity of resources is difficult for promoting.Inhomogeneous through observing the Zinc oxide nano sheet size that this technological invention makes, arrange and disperse.
[Guo Yun such as Guo Yun; Xia Yiben, Min Jiahua is etc. the influence [J] to the growth of ZnO nanometer sheet of. polarity tourmalinite substrate. Journal of Inorganic Materials .2010 July; The 25th volume the 7th phase: 717-720.] be that the zinc nitrate of 0.1 mol is a presoma with concentration; Through being that substrate is cut into slices and surface finish is handled to the polarity tourmalinite, utilize the ultrasonic spray pyrolysis technology, prepare the Nano zinc oxide film of tabular crystal.But this technical process is numerous and diverse, and difficulty is bigger, and not easy to operate, cost is bigger, prepared nano structure of zinc oxide thickness big (100～200nm), arrange also more scrappy, undertighten.
Kang etc. [Colloids and Surfaces A:Physicochem.Eng.Aspects 369 (2010) 268-271] utilize the collosol and gel pyrogenic silica to prepare the ZnO nano belt; And studied the growth mechanism of ZnO through thermogravimetry; And with the rhodamine is the pollutent model, further studies the optical property of ZnO.The result shows, through simple collosol and gel pyrogenic silica, also can prepare the higher ZnO of degree of crystallization, and colloidal sol plays an important role in the ZnO forming process, and the ZnO rhodamine of under ultraviolet light conditions, degrading efficiently.But should technology also fail to obtain area and be square micron level, thickness and be nano level, evenly distributed nanometer sheet.
Forefathers have made many work for the preparation nano structure of zinc oxide, though obtained bigger achievement, long between remaining in the preparation, energy consumption is big, and structure is inhomogeneous, and it is comparatively scattered to distribute, the not high defective of degree of crystallization.
Summary of the invention
The invention discloses and a kind ofly prepare the method for Zinc oxide nano sheet, on monocrystalline silicon piece, prepare the unidimensional zinc oxide nano rod earlier, place the growth solution that configures to zinc oxide nano rod then based on nanometic zinc oxide rod array; In the tetrafluoroethylene autoclave, carry out chemical liquid deposition, not only technology is simple for the prepared Zinc oxide nano sheet that goes out, and preparation time is short; Mild condition, power consumption is few, and is evenly distributed; Arrange closely, it is long effectively to overcome the existing preparation time of prior art for preparing Zinc oxide nano sheet, and energy consumption is big; The uneven homogenize of structure, it is comparatively scattered to distribute, the not high defective of degree of crystallization.
A kind ofly prepare the method for Zinc oxide nano sheet based on nanometic zinc oxide rod array, at first the planar substrate of cleaning as: on monocrystalline silicon piece or the sheet glass, prepare the nanometic zinc oxide rod array layer of one deck diameter nano level, vertical growth; Carry out according to following steps then:
A) configuration growth solution:
Volumetric molar concentration is three kinds of solution of 0.1mol/L: 1: 1: 1 to 1: 3: 1 by volume the mixed of metal salt solution beyond zinc solution, organic amine solution and the zinc salt; Configure the growth solution that zinc ion concentration is 0.025mol/L, and this solution is placed autoclave;
The substrate that has the nanometic zinc oxide rod array layer that B) will prepare is oblique down or vertically place growth solution;
C) again autoclave is placed thermostatic drying chamber, reaction is 2～5 hours under 100～200 ℃ of environment;
D) take out substrate, wash repeatedly with deionized water, 200-600 ℃ thermal treatment is passed through in seasoning at last, obtain pattern evenly, arrange closely, thickness is nano level, area is the ultra-thin zinc-oxide nano sheet material of square micron level.
Described zinc solution is a kind of in zinc acetate dihydrate or the zinc nitrate hexahydrate.
Described organic amine solution is a kind of in vulkacit H or the trolamine.
Metal salt solution beyond the described zinc salt is a kind of in nitrate trihydrate copper or the magnesium chloride.
Adopt the inventive method to prepare Zinc oxide nano sheet; Mild condition, weak point simple to operate, consuming time, low, the environment-friendly high-efficiency of energy consumption; And the Zinc oxide nano sheet uniform distribution that makes, arrange closely, percent crystallinity is high, can prepare the large-area nano sheet, and effectively improve electricity conversion.
Description of drawings
Fig. 1 is the preparation process synoptic diagram of zinc-oxide nano sheet material;
Fig. 2 is 200,000 times of scanning electron microscope images of zinc-oxide nano bar material;
Fig. 3 is the scanning electron microscope image of zinc-oxide nano sheet material:
(a) 10,000 times, (b) 5000 times, (c) 2000 times, (d) 500 times.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is specified.
At first utilize chemical deposition, chemical Vapor deposition process, thermal evaporation or template on the monocrystalline silicon piece substrate, to prepare the nanometic zinc oxide rod array layer of one deck diameter 50 nanometers, vertical growth, as shown in Figure 2; Observe through Fig. 2, zinc oxide nano rod is arranged closely, vertically growth, and the upper end becomes the hexagon shape.
Embodiment 1
As shown in Figure 1: three kinds of solution that volumetric molar concentration are 0.1mol/L: zinc nitrate hexahydrate Zn (NO
3)
26H
2O (0.1mol/L), vulkacit H C
6H
12N
4(0.1mol/L), nitrate trihydrate copper Cu (NO
3)
23H
21: 2: 1 by volume mixed of O (0.1mol/L) configures the growth solution that zinc ion concentration is 0.025mol/L, and the growth solution that configures is placed reaction ax.
Clamp the monocrystalline silicon piece that has zinc oxide nano rod with sheet glass then, be tilted to down a silicon chip that has zinc oxide nano rod and place growth solution, the position roughly is positioned at the solution middle part; Place thermostatic drying chamber to reaction kettle again, under 160 ℃ of conditions, reacted 4 hours.
Reaction process is as follows:
(CH
2)
6N
4+6H
2O?→6HCHO+4NH
3
2OH
-+Zn
2+→Zn(OH)
2
Zn(OH)
2→ZnO
(s)+H
2O
When the chemical solution of configuration when being heated, the vulkacit H in the solution decomposes and generates formaldehyde and ammonia, and ammonia is water-soluble and discharge OH
-, the zinc nitrate hexahydrate dissolving provides reaction required Zn
2+, both chemical combination generate zinc hydroxide, and zinc hydroxide oxidation under heating condition generates zinc oxide.
At last, take out sample, clean repeatedly with deionized water, seasoning after 450 ℃ thermal treatment, obtains the zinc-oxide nano sheet material.Scanning electron microscope image is as shown in Figure 3; As can be seen from Figure 3, nanometer sheet is evenly distributed, compact, area becomes square micron level, thickness to become nano level.
Embodiment 2
Utilize the substrate of conductive glass sheet as zinc oxide nano rod, the configuration zinc ion concentration is the growth solution of 0.025mol/L.Volumetric molar concentration is three kinds of solution of 0.1mol/L: zinc nitrate hexahydrate Zn (NO
3)
26H
2O (0.1mol/L), vulkacit H C
6H
12N
4(0.1mol/L), nitrate trihydrate copper Cu (NO
3)
23H
21: 1: 1 by volume mixed of O (0.1mol/L) places reaction kettle; Clamp the conductive glass sheet that has the zinc-oxide nano bar material with sheet glass then, be tilted to down a silicon chip that has zinc oxide nano rod and place growth solution, the position roughly is positioned at the solution middle part.Place thermostatic drying chamber to reaction kettle then, under 160 ℃ of conditions, reacted 4 hours.Take out sample, clean repeatedly with deionized water, seasoning after 450 ℃ thermal treatment, obtains the zinc-oxide nano sheet material.
Embodiment 3
With the substrate of simple glass sheet as zinc oxide nano rod, the configuration zinc ion concentration is the growth solution of 0.025mol/L.Volumetric molar concentration is three kinds of solution of 0.1mol/L: zinc nitrate hexahydrate Zn (NO
3)
26H
2O (0.1mol/L), vulkacit H C
6H
12N
4(0.1mol/L), magnesium chloride Mg Cl
2(0.1mol/L) 1: 3: 1 by volume mixed places reaction kettle; Vertically place growth solution to the simple glass sheet that has zinc oxide nano rod then, the position roughly is positioned at the solution middle part.Place thermostatic drying chamber to reaction kettle then, under 160 ℃ of conditions, reacted 4 hours.Take out sample, clean repeatedly with deionized water, seasoning after 450 ℃ thermal treatment, obtains the zinc-oxide nano sheet material.
The configuration zinc ion concentration is the growth solution of 0.025mol/L.Volumetric molar concentration is three kinds of solution of 0.1mol/L: zinc nitrate hexahydrate Zn (NO
3)
26H
2O (0.1mol/L), vulkacit H C
6H
12N
4(0.1mol/L), nitrate trihydrate copper Cu (NO
3)
23H
21: 2: 1 by volume mixed of O (0.1mol/L) places reaction kettle; Clamp the monocrystalline silicon piece that has the zinc-oxide nano bar material with sheet glass then, be tilted to down a silicon chip that has zinc oxide nano rod and place growth solution, the position roughly is positioned at the solution middle part.Place thermostatic drying chamber to reaction kettle then, under 100 ℃ of conditions, reacted 4 hours.Take out sample, clean repeatedly with deionized water, seasoning after 450 ℃ thermal treatment, obtains the zinc-oxide nano sheet material.
Embodiment 5
The configuration zinc ion concentration is the growth solution of 0.025mol/L.Volumetric molar concentration is three kinds of solution of 0.1mol/L: zinc nitrate hexahydrate Zn (NO
3)
26H
2O (0.1mol/L), vulkacit H C
6H
12N
4(0.1mol/L), nitrate trihydrate copper Cu (NO
3)
23H
21: 2: 1 by volume mixed of O (0.1mol/L) places reaction kettle; Clamp the monocrystalline silicon piece that has the zinc-oxide nano bar material with sheet glass then, be tilted to down a silicon chip with zinc oxide nano rod and place growth solution, the position roughly is positioned at the solution middle part.Place thermostatic drying chamber to reaction kettle then, under 200 degrees celsius, reacted 4 hours.Take out sample, clean repeatedly with deionized water, seasoning after 450 degrees centigrade thermal treatment, obtains the zinc-oxide nano sheet material.
Embodiment 6
The configuration zinc ion concentration is the growth solution of 0.025mol/L.Volumetric molar concentration is three kinds of solution of 0.1mol/L: zinc nitrate hexahydrate Zn (NO
3)
26H
2O (0.1mol/L), vulkacit H C
6H
12N
4(0.1mol/L), nitrate trihydrate copper Cu (NO
3)
23H
21: 2: 1 by volume mixed of O (0.1mol/L) places reaction kettle; Clamp the monocrystalline silicon piece that has the zinc-oxide nano bar material with sheet glass then, be tilted to down a silicon chip that has zinc oxide nano rod and place growth solution, the position roughly is positioned at the solution middle part.Place thermostatic drying chamber to reaction kettle then, under 160 degrees celsius, reacted 2 hours.Take out sample, clean repeatedly with deionized water, seasoning after 450 degrees centigrade thermal treatment, obtains the zinc-oxide nano sheet material.
Embodiment 7
The configuration zinc ion concentration is the growth solution of 0.025mol/L.Volumetric molar concentration is three kinds of solution of 0.1mol/L: zinc nitrate hexahydrate Zn (NO
3)
26H
2O (0.1mol/L), vulkacit H C
6H
12N
4(0.1mol/L), nitrate trihydrate copper Cu (NO
3)
23H
21: 2: 1 by volume mixed of O (0.1mol/L) places reaction kettle; Clamp the monocrystalline silicon piece that has the zinc-oxide nano bar material with sheet glass then, be tilted to down a silicon chip with zinc oxide nano rod and place growth solution, the position roughly is positioned at the solution middle part.Place thermostatic drying chamber to reaction kettle then, under 160 degrees celsius, reacted 5 hours.Take out sample, clean repeatedly with deionized water, seasoning after 450 degrees centigrade thermal treatment, obtains the zinc-oxide nano sheet material.
Embodiment 8
The configuration zinc ion concentration is the growth solution of 0.025mol/L.Volumetric molar concentration is three kinds of solution of 0.1mol/L: zinc nitrate hexahydrate Zn (NO
3)
26H
2O (0.1mol/L), vulkacit H C
6H
12N
4(0.1mol/L), nitrate trihydrate copper Cu (NO
3)
23H
21: 2: 1 by volume mixed of O (0.1mol/L) places reaction kettle; Clamp the monocrystalline silicon piece that has the zinc-oxide nano bar material with sheet glass then, be tilted to down a silicon chip that has zinc oxide nano rod and place growth solution, the position roughly is positioned at the solution middle part.Place thermostatic drying chamber to reaction kettle then, under 160 degrees celsius, reacted 3 hours.Take out sample, clean repeatedly with deionized water, seasoning after 200 degrees centigrade thermal treatment, obtains the zinc-oxide nano sheet material.
Embodiment 9
The configuration zinc ion concentration is the growth solution of 0.025mol/L.Volumetric molar concentration is three kinds of solution of 0.1mol/L: zinc nitrate hexahydrate Zn (NO
3)
26H
2O (0.1mol/L), vulkacit H C
6H
12N
4(0.1mol/L), nitrate trihydrate copper Cu (NO
3)
23H
21: 2: 1 by volume mixed of O (0.1mol/L) places reaction kettle; Clamp the monocrystalline silicon piece that has the zinc-oxide nano bar material with sheet glass then, be tilted to down a silicon chip that has zinc oxide nano rod and place growth solution, the position roughly is positioned at the solution middle part.Place thermostatic drying chamber to reaction kettle then, under 160 degrees celsius, reacted 3 hours.Take out sample, clean repeatedly with deionized water, seasoning after 500 degrees centigrade thermal treatment, obtains the zinc-oxide nano sheet material.
The configuration zinc ion concentration is the growth solution of 0.025mol/L.Volumetric molar concentration is three kinds of solution of 0.1mol/L: zinc nitrate hexahydrate Zn (NO
3)
26H
2O (0.1mol/L), trolamine C
6H
15NO
3(0.1mol/L), nitrate trihydrate copper Cu (NO
3)
23H
21: 2: 1 by volume mixed of O (0.1mol/L) places reaction kettle; Clamp the monocrystalline silicon piece that has the zinc-oxide nano bar material with sheet glass then, be tilted to down a silicon chip that has zinc oxide nano rod and place growth solution, the position roughly is positioned at the solution middle part.Place thermostatic drying chamber to reaction kettle then, under 200 degrees celsius, reacted 5 hours.Take out sample, clean repeatedly with deionized water, seasoning after 450 degrees centigrade thermal treatment, obtains the zinc-oxide nano sheet material.
Embodiment 11
The configuration zinc ion concentration is the growth solution of 0.025mol/L.Volumetric molar concentration is three kinds of solution of 0.1mol/L: zinc acetate dihydrate Zn (CH
3COO)
22H
2O (0.1mol/L), vulkacit H C
6H
12N
4(0.1mol/L), nitrate trihydrate copper Cu (NO
3)
23H
21: 2: 1 by volume mixed of O (0.1mol/L) places reaction kettle; Clamp the monocrystalline silicon piece that has the zinc-oxide nano bar material with sheet glass then, place growth solution to a silicon chip that has zinc oxide nano rod under oblique, the position roughly is positioned at the solution middle part.Place thermostatic drying chamber to reaction kettle then, under 200 degrees celsius, reacted 3 hours.Take out sample, clean repeatedly with deionized water, seasoning after 300 degrees centigrade thermal treatment, obtains the zinc-oxide nano sheet material.
Through the enforcement to above embodiment, synthesis result draws to draw a conclusion:
1, the Zinc oxide nano sheet of embodiment 1 preparation has obtained optimum oxidation zinc nanometer sheet pattern, and area becomes micron order, and thickness is about 10nm;
2, embodiment 2, through changing the configuration proportion of growth solution, are substrate with the conductive glass, and resulting Zinc oxide nano sheet area shape is less, and it is comparatively sparse to distribute;
3, embodiment 3, are substrate with the simple glass, and vertically place substrate, and it is big that the growth solution ratio becomes, and when having magnesium chloride, Zinc oxide nano sheet thickness thickening is about 30nm;
4, embodiment 4 and 5, when temperature of reaction obtained changing, it is comparatively scattered that (like embodiment 4) lesser temps also can make Zinc oxide nano sheet distribute, and comparatively high temps (like embodiment 5) can make the Zinc oxide nano sheet edge that spination is arranged;
5, embodiment 6 and 7, when the reaction times obtained changing, short reaction times (like embodiment 6) resulting Zinc oxide nano sheet was comparatively scattered, and the Zinc oxide nano sheet that the long reaction times (like embodiment 7) obtains is similar with embodiment 1;
6, embodiment 8 and 9 compares with embodiment 1, and the appearance of gained Zinc oxide nano sheet is similar, but degree of crystallization is lower;
7, embodiment 10, and trolamine does not have considerable influence for the pattern of Zinc oxide nano sheet, similar embodiment 1;
8, embodiment 11, and zinc acetate dihydrate has certain influence for the pattern of Zinc oxide nano sheet, and resulting Zinc oxide nano sheet is less.
Claims (4)
1. one kind prepares the method for Zinc oxide nano sheet based on nanometic zinc oxide rod array, it is characterized in that: at first the planar substrate of cleaning as: on monocrystalline silicon piece or the sheet glass, prepare the nanometic zinc oxide rod array layer of one deck vertical growth; Carry out according to following steps then:
A) configuration growth solution:
Volumetric molar concentration is three kinds of solution of 0.1mol/L: 1: 1: 1 to 1: 3: 1 by volume the mixed of metal salt solution beyond zinc solution, organic amine solution and the zinc salt; Configure the growth solution that zinc ion concentration is 0.025mol/L, and this solution is placed autoclave;
The substrate tilting that has the nanometic zinc oxide rod array layer that B) will prepare places growth solution downwards or vertically;
C) again autoclave is placed thermostatic drying chamber, reaction is 2～5 hours under 100～200 ℃ of environment;
D) take out substrate, wash repeatedly with deionized water, 200-600 ℃ thermal treatment is passed through in seasoning at last, obtain pattern evenly, arrange closely, thickness is nano level, area is the ultra-thin zinc-oxide nano sheet material of square micron level.
2. according to claim 1ly a kind ofly prepare the method for Zinc oxide nano sheet based on nanometic zinc oxide rod array, it is characterized in that: described zinc solution is a kind of in zinc acetate dihydrate or the zinc nitrate hexahydrate.
3. according to claim 1ly a kind ofly prepare the method for Zinc oxide nano sheet based on nanometic zinc oxide rod array, it is characterized in that: described organic amine solution is a kind of in vulkacit H or the trolamine.
4. according to claim 1ly a kind ofly prepare the method for Zinc oxide nano sheet based on nanometic zinc oxide rod array, it is characterized in that: the metal salt solution beyond the described zinc salt is a kind of in nitrate trihydrate copper or the magnesium chloride.
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| CN116425190B (en) * | 2023-04-04 | 2024-04-12 | 华东师范大学 | Method for in-situ growth of zinc oxide nanorods based on microfluidic chip |
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Application publication date: 20120411 |