CN101393092B - Method for making scanning electron microscope example for assembling nanometer line array in aluminum oxide template - Google Patents
Method for making scanning electron microscope example for assembling nanometer line array in aluminum oxide template Download PDFInfo
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- CN101393092B CN101393092B CN200810156883XA CN200810156883A CN101393092B CN 101393092 B CN101393092 B CN 101393092B CN 200810156883X A CN200810156883X A CN 200810156883XA CN 200810156883 A CN200810156883 A CN 200810156883A CN 101393092 B CN101393092 B CN 101393092B
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Abstract
The invention discloses a method for manufacturing a scanning electron microscope sample for an assembled nanometer line array in an aluminum oxide template, which is characterized by comprising the following steps: eroding the template by an alkali liquor the concentration of which is between 0.05 and 5 M, soaking the template continuously in the alkali liquor with lower concentration of between0.001 and 0.0001 M for three to five minutes, then washing the template by water for a few times, and airing the template for the observation under the scanning electron microscope, wherein the alkali liquor is NaOH or KOH solution. The scanning electron microscope sample for the assembled nanometer line array in the aluminum oxide template manufactured by the method can avoid the effect caused by Al(OH)3 deposition attached on the surface of the sample on the observation of the scanning electron microscope.
Description
Technical field
The invention belongs to the manufacture technology field of scanning electron microscope example, be specifically related to the method for making of the scanning electron microscope example of assembling nanometer line array in the alumina formwork.
Background technology
According to the U.S. " physical chemistry magazine B " (J.Phys.Chem.B, 2004, the 106th volume, the 1844th page) and Holland " crystal growth magazine " (J.Cryst.Growth, 2005, the 285th volume, the 527th page) report, the nano-wire array of assembling in the existing alumina formwork, the making of its scanning electron microscope example all is after adopting alkali lye (NaOH solution) corrosion template, directly water cleans several times, promptly observes under scanning electron microscope after drying.Because aluminium oxide and alkali reaction produce meta-aluminate, the easy hydrolysis of meta-aluminate generated Al (OH) when directly water cleaned
3Precipitation, these precipitations tend to attached to sample surfaces, thereby influence the observation of scanning electron microscope example.For a long time, be engaged in the scientific research of alumina formwork and assembly system thereof and experimenter in a large number, fail to propose a kind of simple and effective solution always in the face of the fuzzy result of this stereoscan photograph.
Summary of the invention
The present invention proposes the method for making of the scanning electron microscope example of assembling nanometer line array in a kind of alumina formwork, to avoid sample surfaces by Al (OH)
3Precipitation is adhered to and is influenced the observation of scanning electron microscope.
The method for making of the scanning electron microscope example of assembling nanometer line array in the alumina formwork of the present invention, after it is characterized in that template concentration is the alkali liquid corrosion of 0.05～5M, continuation was soaked in the alkali lye of 0.001 lower～0.0001M of concentration 5～30 minutes, and then water cleaning template several times, can arrive under the scanning electron microscope after drying and observe; Described alkali lye is NaOH or KOH solution.
The concentration range of selected NaOH or KOH solution should be controlled between 0.05～5M and be advisable in the inventive method, because when the concentration of alkali lye is lower than 0.05M, corrosion speed is too slow, and the consumption of alkali lye is too big; And corrosion speed is too fast when the concentration of alkali lye is higher than 5M, and the meta-aluminate concentration that reaction generates is too high, and hydrolysis easily is unfavorable for ensuing immersion and cleaning process.
After the alkali liquid corrosion template with 0.05～5M in the inventive method, continue the dipping by lye of 0.001～0.0001M of employing lower concentration, this moment solution pH value between 10～11, so the meta-aluminate that aluminium oxide and alkali reaction generate can hydrolysis generation Al (OH)
3Precipitation; And because after soaking a period of time, the concentration of the meta-aluminate at template surface place has reduced greatly, this moment, water cleaned again, the Al (OH) that hydrolysis generates on alumina surface
3Precipitation will be very little, can not produce significantly influence to the surface topography of sample, thereby can not influence the observation of scanning electron microscope.Soak time should be controlled at 5～30 minutes proper because the time less than 5 minutes, near the meta-aluminate the template surface just can not be diffused in the solution fully uniformly; And when soak time during greater than 30 minutes, this rarer alkali lye will continue to corrode template, thereby increases the concentration of meta-aluminate in the solution.
With after the existing employing alkali liquid corrosion template directly the water method of cleaning compare, the effect that the method for making of the scanning electron microscope example of assembling nanometer line array has a marked improvement in the alumina formwork of the present invention is embodied in:
Because after the present invention adopts concentration to be the alkali liquid corrosion template of 0.05～5M, continue in the alkali lye of 0.001 lower～0.0001M of concentration, to soak 5～30 minutes, and then the method for water cleaning, thereby avoided generating Al (OH) at the alumina formwork surface hydrolysis
3Precipitation, thus the observation of scanning electron microscope example can not be influenced.
Description of drawings
Fig. 1 is the stereoscan photograph that adopts the Te nano-wire array of the present invention's processing.
Fig. 2 is the stereoscan photograph that adopts the Te nano-wire array of prior art processing.
Fig. 3 is the Ag that adopts the present invention to handle
2The stereoscan photograph of Te nano-wire array.
Fig. 4 is the Ag that adopts the present invention to handle
7Te
4The stereoscan photograph of nano-wire array.
Embodiment
Below pass through embodiment, and the invention will be further described in conjunction with the accompanying drawings.
Embodiment 1: the making of the scanning electron microscope example of Te nano-wire array in the alumina formwork
1, adopt the inventive method to make the scanning electron microscope example of Te nano-wire array in the alumina formwork
Get the alumina formwork that a slice is assembled with the Te nano-wire array, be placed on beaker bottom, getting 0.1mL concentration with dropper is that the NaOH drips of solution of 1M is in the middle of template, after 5 minutes, injecting 100mL concentration is the NaOH solution of 0.0001M, soaks after 15 minutes, take out sample, clean repeatedly several times with big water gaging, dry the back and under scanning electron microscope, observe, obtain stereoscan photograph Fig. 1 of the Te nano-wire array after the inventive method is handled.As can be seen, sample surfaces is smooth clear from this stereoscan photograph Fig. 1, and the hole of template can both see too clearly, and does not find that other material adheres to.
2, make comparisons with the scanning electron microscope example that adopts existing method to make
Get the alumina formwork that a slice is assembled with the Te nano-wire array, be placed on beaker bottom, getting 0.1mL concentration with dropper is that the NaOH drips of solution of 1M is in the middle of template, after 5 minutes, directly clean sample repeatedly several times with big water gaging, dry the back and under scanning electron microscope, observe, obtain stereoscan photograph Fig. 2 of Te nano-wire array.As can be seen, adhered to layer of substance at template surface from this stereoscan photograph Fig. 2, they have covered the pattern details of sample surfaces, have had a strong impact on the observation of sample.
Embodiment 2: Ag in the alumina formwork
2The making of the scanning electron microscope example of Te nano-wire array
Get a slice and be assembled with Ag
2The alumina formwork of Te nano-wire array, be placed on beaker bottom, getting 0.1mL concentration with dropper is that the KOH drips of solution of 0.05M is in the middle of template, after 15 minutes, injecting 20mL concentration is the KOH solution of 0.0005M, soaks after 15 minutes, take out sample, clean repeatedly several times with big water gaging, dry the back and under scanning electron microscope, observe, obtain the Ag after the inventive method is handled
2Stereoscan photograph Fig. 3 of Te nano-wire array.As can be seen, sample surfaces is smooth clear from this stereoscan photograph Fig. 3, and the pattern details of sample surfaces is not covered, and does not find that also other material adheres to.
Embodiment 3: Ag in the alumina formwork
7Te
4The making of the scanning electron microscope example of nano-wire array
Get a slice and be assembled with Ag
7Te
4The alumina formwork of nano-wire array, be placed on beaker bottom, getting 0.05mL concentration with dropper is that the NaOH drips of solution of 5M is in the middle of template, after 30 minutes, injecting 100mL concentration is the KOH solution of 0.0001M, soaks after 30 minutes, take out sample, clean repeatedly several times with big water gaging, dry the back and under scanning electron microscope, observe, obtain Ag
7Te
4Stereoscan photograph Fig. 4 of nano-wire array.As can be seen, sample surfaces is smooth clear from this stereoscan photograph Fig. 4, and the pattern details is not covered equally, does not find that also other material adheres to.
Conclusion:
As can be seen from the above embodiments, the scanning electron microscope example of assembling nanometer line array in the alumina formwork that employing the inventive method is made, because after adopting concentration to be the alkali liquid corrosion template of 0.05～5M, continuation was soaked in the alkali lye of 0.001 lower～0.0001M of concentration 5～30 minutes, and then the method for water cleaning, thereby can avoid sample surfaces because of Al (OH)
3Precipitation is adhered to and is influenced the observation of scanning electron microscope.
Claims (1)
1. the method for making of the scanning electron microscope example of assembling nanometer line array in the alumina formwork, after it is characterized in that template concentration is the alkali liquid corrosion of 0.05～5M, continuation was soaked in the alkali lye of 0.001 lower～0.0001M of concentration 5～30 minutes, and then water cleaning template several times, can arrive under the scanning electron microscope after drying and observe; Described alkali lye is NaOH or KOH solution.
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| CN200810156883XA CN101393092B (en) | 2008-09-28 | 2008-09-28 | Method for making scanning electron microscope example for assembling nanometer line array in aluminum oxide template |
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| CN200810156883XA CN101393092B (en) | 2008-09-28 | 2008-09-28 | Method for making scanning electron microscope example for assembling nanometer line array in aluminum oxide template |
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| CN101393092A CN101393092A (en) | 2009-03-25 |
| CN101393092B true CN101393092B (en) | 2010-08-11 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102732963B (en) * | 2011-04-15 | 2015-03-04 | 中国科学技术大学 | Preparation method of monocrystalline metal nanowire array based on alumina template |
| CN102494934A (en) * | 2011-12-16 | 2012-06-13 | 河北工业大学 | Alkaline corrosive agent for representing defects in GaN (Gallium Nitride) epitaxial layer and preparation method thereof |
| CN104928519A (en) * | 2015-07-07 | 2015-09-23 | 内蒙古科技大学 | Method for extracting second phase in Al-Mg-Si system aluminum alloy |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1998048456A1 (en) * | 1997-04-24 | 1998-10-29 | Massachusetts Institute Of Technology | Nanowire arrays |
| JP2006064693A (en) * | 2004-07-27 | 2006-03-09 | Horiba Ltd | Carbon nanotube analysis method and sample analysis method |
| US7267859B1 (en) * | 2001-11-26 | 2007-09-11 | Massachusetts Institute Of Technology | Thick porous anodic alumina films and nanowire arrays grown on a solid substrate |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1998048456A1 (en) * | 1997-04-24 | 1998-10-29 | Massachusetts Institute Of Technology | Nanowire arrays |
| US7267859B1 (en) * | 2001-11-26 | 2007-09-11 | Massachusetts Institute Of Technology | Thick porous anodic alumina films and nanowire arrays grown on a solid substrate |
| JP2006064693A (en) * | 2004-07-27 | 2006-03-09 | Horiba Ltd | Carbon nanotube analysis method and sample analysis method |
Non-Patent Citations (5)
| Title |
|---|
| Chong Jia etal.Single crystal Ag7Te4 nanowire arrays prepared by DC electrodeposition from aqueous solution.Journal of Crystal Growth.2005,285(4),527-533. * |
| 向娟 等.两步电沉积法制备单晶Au纳米线阵列.电化学.2004,10(1),9-13. |
| 向娟等.两步电沉积法制备单晶Au纳米线阵列.电化学.2004,10(1),9-13. * |
| 贾冲 等.Sb有序单晶纳米线阵列的制备.物理化学学报.2004,20(3),240-243. |
| 贾冲等.Sb有序单晶纳米线阵列的制备.物理化学学报.2004,20(3),240-243. * |
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