CN102140037B - Method for realizing self-assembly of zinc oxide nanometer wires - Google Patents
Method for realizing self-assembly of zinc oxide nanometer wires Download PDFInfo
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- CN102140037B CN102140037B CN2011100719162A CN201110071916A CN102140037B CN 102140037 B CN102140037 B CN 102140037B CN 2011100719162 A CN2011100719162 A CN 2011100719162A CN 201110071916 A CN201110071916 A CN 201110071916A CN 102140037 B CN102140037 B CN 102140037B
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000001338 self-assembly Methods 0.000 title claims abstract description 21
- 239000011787 zinc oxide Substances 0.000 title abstract description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 72
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 72
- 239000010703 silicon Substances 0.000 claims abstract description 72
- 238000005576 amination reaction Methods 0.000 claims abstract description 13
- 230000033444 hydroxylation Effects 0.000 claims abstract description 8
- 238000005805 hydroxylation reaction Methods 0.000 claims abstract description 8
- 239000006185 dispersion Substances 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims abstract description 3
- 230000004048 modification Effects 0.000 claims abstract description 3
- 238000012986 modification Methods 0.000 claims abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 45
- 239000008367 deionised water Substances 0.000 claims description 44
- 229910021641 deionized water Inorganic materials 0.000 claims description 44
- 229910052757 nitrogen Inorganic materials 0.000 claims description 26
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 15
- 239000004141 Sodium laurylsulphate Substances 0.000 claims description 15
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 15
- OKHIGGWUISQLMG-UHFFFAOYSA-N 3-diethoxysilylpropan-1-amine Chemical compound CCO[SiH](OCC)CCCN OKHIGGWUISQLMG-UHFFFAOYSA-N 0.000 claims description 11
- 239000002070 nanowire Substances 0.000 claims description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 238000000137 annealing Methods 0.000 claims description 10
- 238000009835 boiling Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 150000003376 silicon Chemical class 0.000 claims description 6
- 230000005611 electricity Effects 0.000 claims description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 239000001117 sulphuric acid Substances 0.000 claims description 2
- 235000011149 sulphuric acid Nutrition 0.000 claims description 2
- 235000012431 wafers Nutrition 0.000 abstract 2
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 abstract 1
- 239000012528 membrane Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- 239000010408 film Substances 0.000 description 12
- 238000004506 ultrasonic cleaning Methods 0.000 description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- 239000006228 supernatant Substances 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 5
- 150000002978 peroxides Chemical class 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- 125000000524 functional group Chemical group 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000009827 uniform distribution Methods 0.000 description 2
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229920000307 polymer substrate Polymers 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The invention relates to a method for realizing the self-assembly of zinc oxide nanometer wires in the field of nanometer processing, which comprises the following steps of: performing hydroxylation and amination on the surfaces of silicon wafers sequentially, and immersing the silicon wafers in dispersion liquid of the zinc oxide nanometer wires, which is subjected to surface modification by lauryl sodium sulfate, to realize the self-assembly. The method is simple, convenient and efficient, and the prepared zinc oxide nanometer wire membranes are suitable for preparing high-quality devices.
Description
Technical field
What the present invention relates to is the method in a kind of nano processing technology field, specifically is a kind of method that realizes the zinc oxide nanowire self-assembly.
Background technology
Zinc oxide nanowire has remarkable characteristic of semiconductor, optical characteristics, piezoelectric property, has received widely paying close attention to, and has obtained further investigation.Zinc oxide nanowire can be used to prepare field-effect transistor, ultraviolet light detector, gas sensor, solar cell, nano generator and feds etc.The prerequisite of preparation zinc oxide nanowire thin-film device is to obtain the good film of nano wire uniform distribution property.And for zinc oxide nanowire, also lacking effectively, method prepares nano wire film.Prepare one deck gold nano grain film as catalyzer at silicon chip surface; Can make nano wire film; But because the existence of catalyzer can influence the thin-film device performance, even can't come fabricate devices with this film, so the suitable device of making of nano wire film that makes with this method.
Ko S H, et al.ZnO nanowire network transistor fabrication on a polymer substrate by low-temperature are found in retrieval through to prior art; All-inorganic nanoparticle solution process.APPLIED PHYSICS LETTERS, 2008,92:154102 (Gao Chenghuan; Deng. utilizing low temperature full-inorganic nanoparticle prepared is the zinc oxide nanowire network of transistors of substrate with the polymkeric substance, Applied Physics wall bulletin, 2008; Put down in writing 92:154102): utilize hydrothermal method;, as seed it is immersed in the aqueous solution that contains zinc nitrate and vulkacit H with Zinc oxide nanoparticle, also can makes the zinc oxide nanowire film; But the nano wire in this film is not to be tiled in the substrate; But tiltedly standing, therefore with this nano wire film fabricate devices, channel current can be smaller.Therefore, be necessary to develop a kind of technology simple, with low cost, easy to operate, prepare the method for high-quality zinc oxide nano wire film efficiently, this will be a key of making the nano wire film device.
Summary of the invention
The present invention is directed to the above-mentioned deficiency that prior art exists, a kind of method that realizes the zinc oxide nanowire self-assembly is provided, this method is simple, convenient, efficient, the suitable preparation of the zinc oxide nanowire film for preparing high quality device.
The present invention realizes that through following technical scheme the present invention is soaked in the zinc oxide nanowire dispersion liquid after sodium lauryl sulphate is carried out finishing through after silicon chip surface being carried out successively hydroxylation and amination processing, realizes self-assembly.
Described hydroxylation is meant: the mixing solutions of the hydrogen peroxide solution of compound concentration 30wt% sulphuric acid soln and concentration 98wt%; Its volume ratio is 2.5: 1, and cleaned silicon chip is put into this solution, under 90 ℃, boils 2～3 hours; After having boiled silicon chip is taken out and clean repeatedly with deionized water; At last silicon chip is put into deionized water, after boiling 20～30 minutes under 80 ℃ of conditions, taking-up dries up with nitrogen.
Described amination is meant: in deionized water, add 3-aminopropyl diethoxy silane; And carried out supersound process 10 minutes; Afterwards hydroxylated silicon chip is put into and wherein left standstill 10～15 hours; Leave standstill and finish post-heating to 80 ℃ and kept 1～2 hour, then take out silicon chip and clean, at last with the silicon chip vacuum annealing.
The consumption of described 3-aminopropyl diethoxy silane is to add 1～4 milliliter 3-aminopropyl diethoxy silane in per 100 ml deionized water.
The temperature of described vacuum annealing is 120～180 ℃, and annealing time is 10～20 hours.
Described finishing is meant: zinc oxide nanowire is put into deionized water; In deionized water, add sodium lauryl sulphate simultaneously; And carry out supersound process, make zinc oxide nanowire homodisperse in solution, and make nano wire wear negative electricity in the modification following table of sodium lauryl sulphate.
The consumption of described zinc oxide nanowire is that per 100 ml deionized water add 1～3 milligram.
The consumption of described sodium lauryl sulphate is to add 0.01～0.10 gram sodium lauryl sulphate in per 100 ml deionized water.
The time of described supersound process is 2～4 hours.
Principle of work of the present invention is: zinc oxide nanowire is with negative electricity in the surface after sodium lauryl sulphate is modified.Silicon chip surface is after 3-aminopropyl diethoxy silane is handled, and there is amino functional group in the surface, and amino functional group becomes positively charged in water.Therefore, in deionized water, the electrostatic attraction that electronegative zinc oxide nanowire receives silicon chip surface positively charged amino functional group has realized the self-assembly of zinc oxide nanowire at silicon chip surface.
The invention has the beneficial effects as follows: utilize self-assembly to realize the uniform distribution of zinc oxide nanowire at silicon chip surface, equally distributed nano wire can be used for preparing high-quality thin-film device.
Description of drawings
Fig. 1 is the ESEM picture of the zinc oxide nanowire self-assembly of the embodiment of the invention 1.
Embodiment
Elaborate in the face of embodiments of the invention down, present embodiment provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment being to implement under the prerequisite with technical scheme of the present invention.
Embodiment 1
The first step, silicon chip cleans.At first, the silicon chip that will have silicon dioxide insulating layer is put into 50 milliliters of ethanol, carries out ultrasonic cleaning 10 minutes, takes out to dry up with nitrogen; Then, silicon chip is put into 50 milliliters of acetone, carried out ultrasonic cleaning 10 minutes, taking-up dries up with nitrogen; At last silicon chip is put into 100 ml deionized water, carried out ultrasonic cleaning 10 minutes, taking-up dries up with nitrogen.
Second step, the hydroxylation of silicon chip surface.Preparation sulfuric acid (concentration 98%) and ydrogen peroxide 50 (concentration 30%) volume ratio are 2.5: 1 solution, and cleaned silicon chip is put into this solution, under 90 ℃ of conditions, boil 2.5 hours, after having boiled silicon chip are taken out and clean repeatedly with deionized water.At last, silicon chip is put into deionized water, after boiling 20 minutes under 80 ℃, taking-up dries up with nitrogen.
The 3rd step, the amination of silicon chip surface.In 50 ml deionized water, add 1 milliliter of 3-aminopropyl diethoxy silane, and carried out supersound process 10 minutes, hydroxylated silicon chip is put into wherein left standstill 10 hours afterwards.Leave standstill and finish post-heating to 80 ℃ and kept 1 hour, then take out silicon chip and it is cleaned repeatedly, dry up with nitrogen with ethanol; At last, silicon chip under 150 ℃ of hot conditionss, was carried out vacuum annealing 10 hours.
The 4th step, the finishing of zinc oxide nanowire.5 milligrams of zinc oxide nanowires are put into 250 ml deionized water, in deionized water, add 100 milligrams of sodium lauryl sulphate simultaneously, carried out supersound process afterwards 3 hours, make zinc oxide nanowire homodisperse in solution.
The 5th step, the self-assembly of zinc oxide nanowire.After the aqueous solution of above-mentioned zinc oxide nanowire leaves standstill 40 minutes, get 180 milliliters of its supernatants.The silicon chip of surface amination is put into this supernatant, leave standstill under 20 ℃ after 10 hours and take out, and, dry up with nitrogen at last with deionized water cleaning silicon chip repeatedly.Figure one is the ESEM picture of zinc oxide nanowire in the silicon chip surface self-assembly.
Embodiment 2
The first step, silicon chip cleans.At first, the silicon chip that will have silicon dioxide insulating layer is put into 50 milliliters of ethanol, carries out ultrasonic cleaning 10 minutes, takes out to dry up with nitrogen; Then, silicon chip is put into 50 milliliters of acetone, carried out ultrasonic cleaning 10 minutes, taking-up dries up with nitrogen; At last silicon chip is put into 100 ml deionized water, carried out ultrasonic cleaning 10 minutes, taking-up dries up with nitrogen.
Second step, the hydroxylation of silicon chip surface.Preparation sulfuric acid (concentration 98%) and ydrogen peroxide 50 (concentration 30%) volume ratio are 2.5: 1 solution, and cleaned silicon chip is put into this solution, under 90 ℃ of conditions, boil 2 hours, after having boiled silicon chip are taken out and clean repeatedly with deionized water.At last, the silicon chip that cleans is put into deionized water, after boiling 25 minutes under 80 ℃ of conditions, taking-up dries up with nitrogen.
The 3rd step, the amination of silicon chip surface.In 50 ml deionized water, add 0.5 milliliter of 3-aminopropyl diethoxy silane, and carried out supersound process 10 minutes, hydroxylated silicon chip is put into wherein left standstill 12 hours afterwards.Leave standstill and finish post-heating to 80 ℃ and kept 1.5 hours, then take out silicon chip and it is cleaned repeatedly, dry up with nitrogen with deionized water; At last, silicon chip under 180 ℃ of hot conditionss, was carried out vacuum annealing 12 hours.
The 4th step, the finishing of zinc oxide nanowire.2 milligrams of zinc oxide nanowires are put into 200 ml deionized water, in deionized water, add 20 milligrams of sodium lauryl sulphate simultaneously, carried out supersound process afterwards 2 hours, make zinc oxide nanowire homodisperse in solution.
The 5th step, the self-assembly of zinc oxide nanowire.After the aqueous solution of above-mentioned zinc oxide nanowire leaves standstill 35 minutes, get 150 milliliters of its supernatants.The silicon chip of surface amination is put into this supernatant, take out silicon chip after leaving standstill 24 hours, and spend Virahol and clean repeatedly, dry up with nitrogen at last at 45 ℃.
Embodiment 3
The first step, silicon chip cleans.At first, the silicon chip that will have silicon dioxide insulating layer is put into 50 milliliters of ethanol, carries out ultrasonic cleaning 10 minutes, takes out to dry up with nitrogen; Then, silicon chip is put into 50 milliliters of acetone, carried out ultrasonic cleaning 10 minutes, taking-up dries up with nitrogen; At last silicon chip is put into 100 ml deionized water, carried out ultrasonic cleaning 10 minutes, taking-up dries up with nitrogen.
Second step, the hydroxylation of silicon chip surface.Preparation sulfuric acid (concentration 98%) and ydrogen peroxide 50 (concentration 30%) volume ratio are 2.5: 1 solution, and cleaned silicon chip is put into this solution, under 90 ℃ of conditions, boil 3 hours, after having boiled silicon chip are taken out and clean repeatedly with deionized water.At last, the silicon chip that cleans is put into deionized water, after boiling 30 minutes under 80 ℃ of conditions, taking-up dries up with nitrogen.
The 3rd step, the amination of silicon chip surface.In 50 ml deionized water, add 2 milliliters of 3-aminopropyl diethoxy silanes, and carried out supersound process 10 minutes, hydroxylated silicon chip is put into wherein left standstill 15 hours afterwards.Leave standstill and finish post-heating to 80 ℃ and kept 2 hours, then take out silicon chip and it is cleaned repeatedly, dry up with nitrogen with acetone; At last, silicon chip under 120 ℃ of hot conditionss, was carried out vacuum annealing 20 hours.
The 4th step, the finishing of zinc oxide nanowire.6 milligrams of zinc oxide nanowires are put into 200 ml deionized water, in deionized water, add 200 milligrams of sodium lauryl sulphate simultaneously, carried out supersound process afterwards 4 hours, make zinc oxide nanowire homodisperse in solution.
The 5th step, the self-assembly of zinc oxide nanowire.After the aqueous solution of above-mentioned zinc oxide nanowire leaves standstill 50 minutes, get 150 milliliters of its supernatants.The silicon chip of surface amination is put into this supernatant, take out silicon chip after leaving standstill 30 minutes, and spend ethanol and clean repeatedly, dry up with nitrogen at last at 70 ℃.
Embodiment 4
The first step, silicon chip cleans.At first, the silicon chip that will have silicon dioxide insulating layer is put into 50 milliliters of ethanol, carries out ultrasonic cleaning 10 minutes, takes out to dry up with nitrogen; Then, silicon chip is put into 50 milliliters of acetone, carried out ultrasonic cleaning 10 minutes, taking-up dries up with nitrogen; At last silicon chip is put into 100 ml deionized water, carried out ultrasonic cleaning 10 minutes, taking-up dries up with nitrogen.
Second step, the hydroxylation of silicon chip surface.Preparation sulfuric acid (concentration 98%) and ydrogen peroxide 50 (concentration 30%) volume ratio are 2.5: 1 solution, and cleaned silicon chip is put into this solution, under 90 ℃ of conditions, boil 2.5 hours, after having boiled silicon chip are taken out and clean repeatedly with deionized water.At last, the silicon chip that cleans is put into deionized water, after boiling 30 minutes under 80 ℃ of conditions, taking-up dries up with nitrogen.
The 3rd step, the amination of silicon chip surface.In 50 ml deionized water, add 1.5 milliliters of 3-aminopropyl diethoxy silanes, and carried out supersound process 10 minutes, hydroxylated silicon chip is put into wherein left standstill 15 hours afterwards.Leave standstill and finish post-heating to 80 ℃ and kept 2 hours, then take out silicon chip and it is cleaned repeatedly, dry up with nitrogen with Virahol; At last, silicon chip under 160 ℃ of hot conditionss, was carried out vacuum annealing 13 hours.
The 4th step, the finishing of zinc oxide nanowire.4 milligrams of zinc oxide nanowires are put into 200 ml deionized water, in deionized water, add 160 milligrams of sodium lauryl sulphate simultaneously, carried out supersound process afterwards 4 hours, make zinc oxide nanowire homodisperse in solution.
The 5th step, the self-assembly of zinc oxide nanowire.After the aqueous solution of above-mentioned zinc oxide nanowire leaves standstill 40 minutes, get 150 milliliters of its supernatants.The silicon chip of surface amination is put into this supernatant, take out silicon chip at 60 ℃ after leaving standstill 6 hours, and clean repeatedly, dry up with nitrogen at last with deionized water.
Claims (5)
1. a method that realizes the zinc oxide nanowire self-assembly is characterized in that, through after silicon chip surface being carried out successively carboxylated and amination and handling, is soaked in the zinc oxide nanowire dispersion liquid after sodium lauryl sulphate is carried out finishing, realizes self-assembly;
Described hydroxylation is meant: the mixing solutions of the hydrogen peroxide solution of compound concentration 30wt% sulphuric acid soln and concentration 98wt%; Its volume ratio is 2.5:1, and cleaned silicon chip is put into this solution, under 90 ℃, boils 2～3 hours; After having boiled silicon chip is taken out and clean repeatedly with deionized water; At last silicon chip is put into deionized water, after boiling 20～30 minutes under 80 ℃ of conditions, taking-up dries up with nitrogen;
Described amination is meant: in deionized water, add 3-aminopropyl diethoxy silane; And carried out supersound process 10 minutes; Afterwards hydroxylated silicon chip is put into and wherein left standstill 10～15 hours; Leave standstill and finish post-heating to 80 ℃ and kept 1～2 hour, then take out silicon chip and clean, at last with the silicon chip vacuum annealing;
Described finishing is meant: zinc oxide nanowire is put into deionized water; In deionized water, add sodium lauryl sulphate simultaneously; And carry out supersound process, make zinc oxide nanowire homodisperse in solution, and make nano wire wear negative electricity in the modification following table of sodium lauryl sulphate.
2. the method for realization zinc oxide nanowire according to claim 1 self-assembly is characterized in that, the consumption of described 3-aminopropyl diethoxy silane is to add 1～4 milliliter 3-aminopropyl diethoxy silane in per 100 ml deionized water.
3. the method for realization zinc oxide nanowire according to claim 1 self-assembly is characterized in that, the temperature of described vacuum annealing is 120～180 ℃, and annealing time is 10～20 hours.
4. the method for realization zinc oxide nanowire according to claim 1 self-assembly is characterized in that, the consumption of described zinc oxide nanowire is that per 100 ml deionized water add 1～3 milligram.
5. the method for realization zinc oxide nanowire according to claim 1 self-assembly is characterized in that, the consumption of described sodium lauryl sulphate is to add 0.01～0.10 gram sodium lauryl sulphate in per 100 ml deionized water.
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| CN103147133B (en) * | 2013-02-25 | 2015-03-25 | 西南大学 | Three-dimensional carrier of microarray biochip and preparation method thereof |
| CN104034884B (en) * | 2014-07-01 | 2016-08-24 | 西南大学 | Preparation method of microarray antibody chip based on dendritic polymer and products thereof |
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| CN109301073B (en) * | 2018-10-23 | 2022-02-01 | 中国科学院重庆绿色智能技术研究院 | Zinc oxide nanowire/ferrocenyl polythiophene composite material, gold electrode and preparation method thereof |
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