CN104020152A - Sandwich-structural micron tube and preparation method and application thereof - Google Patents
Sandwich-structural micron tube and preparation method and application thereof Download PDFInfo
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- CN104020152A CN104020152A CN201410238144.0A CN201410238144A CN104020152A CN 104020152 A CN104020152 A CN 104020152A CN 201410238144 A CN201410238144 A CN 201410238144A CN 104020152 A CN104020152 A CN 104020152A
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Abstract
The invention belongs to the technical field of micro nano devices, and in particular relates to a sandwich-structural micron tube and a preparation method and application thereof. The sandwich-structural micron tube is prepared by the following steps: preparing a substrate, preparing a graphical sacrificial layer template on the substrate; depositing a double-layer oxide film with internal stress on the substrate and a sacrificial layer; selectively removing portion of the sacrificial layer between the oxide film and the substrate, releasing the oxide film, curling the oxide film into the micron tube; coating the inner wall and the outer wall of the micron tube with a polymer film. The sandwich-structural micron tube can be used as a humidity sensor for measurement. The details are as follows: the sandwich-structural micron tube is placed in sealed environment with adjustable humidity, when the environment humidity increases, the polymer absorbs water to swell, and the micron tube wall thickness increases. By measurement of changes in the resonant wavelength of the sandwich-structural micron tube, the environment humidity can be detected.
Description
Technical field
The invention belongs to micro-nano device technical field, be specifically related to a kind of sandwich structure micron tube and its preparation method and application.
Background technology
The light that " whispering gallery modes " in optical field (whispering gallery mode, WGM) refers to certain wavelength in the medium of higher refractive index around the process of its interface circulating propagation.The optical resonator with " Whispering-gallery-mode " is because it is to the susceptibility of surrounding environment medium, self surface topography and adsorbate thereof and demonstrate sizable potentiality in the detection of biology, environment, nano particle etc.For example, at biological field, by measuring the variation of optical resonator resonance wavelength, can detect its residing biotic component environment or its surface and whether adsorb and have virus, protein molecule etc.; In particle detection field, can pass through the swarming phenomenon of resonant optical mode, the single nanoparticle on detection resonator cavity and the position on resonator cavity thereof.In addition, optical resonator also can be used for medicament transport, the guidance quality growth of cell etc.Therefore, the optical resonator with " whispering gallery modes " can provide high precision, high-resolution detection information, and can extremely be widely used in every field.
Wherein, from the optical resonator of curling tubular structure because preparation technology is simple, size and arrange controlled, the multi-functional plurality of advantages such as integrated and being widely studied.G. the people such as S. Huang is in 2010 discoveries, utilize have " whispering gallery modes " from curling tubular structure, can detect its microfluidic environment of living in (such as acetone, alcohol, water etc.); J. the people such as Zhong found in 2013, and Water Molecular Adsorption can be divided into physisorption and two processes of chemisorption in the process from curling tubulose optical resonator, by suitable control, can make hydrone produce obviously impact to resonator cavity mode of resonance.These researchs show, what have resonant optical mode can be used as miniature hygrosensor from curling tubulose microtubule, detects ambient humidity of living in.
But, utilize oxide from curling microtubule, to survey the absorption of hydrone, mainly be subject to the restriction of two aspects: (1) different oxide materials are different to the adsorptive power of hydrone, so oxide is large to the detection sensitivity differences of hydrone from curling microtubule, can not sets up unified humidity and survey scale; (2) detection sensitivity of generally speaking, utilizing oxide to carry out humidity detection from curling microtubule is extremely low.On the other hand, much research shows, compares with oxide material, and high molecular polymer has the moisture sensitivity of height.The invention provides a kind of simple and easy and lower-cost preparation method and prepare polymkeric substance/oxide/polymeric tubular optical resonator.The method is the limitation of oxidated thing material hardly, can in a big way, change oxide kind and keeps its sensitivity that humidity is surveyed, thereby can be used as miniature hygrosensor and be widely used in all kinds of examples.
Summary of the invention
The object of the present invention is to provide a kind of sandwich structure micron tube and its preparation method and application.
The preparation method of sandwich structure micron tube provided by the invention, comprises following step:
(1) prepare a substrate, on substrate, have patterned sacrifice layer template;
(2) at substrate and above sacrifice layer, deposit the double-deck sull with internal stress; Described internal stress comes from the different heat expansion coefficient of double-deck sull;
(3) optionally remove the partial sacrifice layer between sull and substrate, discharge sull, thus the curling oxide micron tube that becomes;
(4) coated polymer film on oxide micron tube inside and outside wall.
In the present invention, the described oxide bilayer film with internal stress that deposits on sacrifice layer of step (2), the twice corresponding film of deposition in front and back in processes of physical vapor deposition, by changing deposition parameter in deposition process, such as deposit thickness (5-100 nm), rate of sedimentation (0.2-20/s), underlayer temperature (25-300
oc) and deposition pressure (10
-3-10
-4pa) etc., the corresponding film of twice of front and back deposition, to form the internal stress due to thermal expansivity different between different materials.Wherein, the method for physical vapour deposition (PVD) comprises sputter, thermal evaporation, or electron beam evaporation etc.
In the present invention, described oxide material is yttria, zirconia, aluminium oxide, titanium dioxide, silicon monoxide or silicon dioxide one-component, or the multilevel oxide structure of several formations in these oxides.
In the present invention, the described polymeric material of step (4) is polypropylene, polyetherimide, polyvinyl alcohol (PVA) one-component, or the multiple layer polymer of several formations in these polymkeric substance
In the present invention, the geometric parameter of gained sandwich structure micron tube, microtubule diameter for example, the thickness of coated polymer layer etc. can be determined as requested.
Sandwich structure micron tube provided by the invention can be used as humidity and surveys, specific as follows:
Sandwich structure micron tube is placed in to the container of sealing, meanwhile, in container, adds saturated salt solution.By changing the kind of saturated salt solution, change sandwich structure micron tube humidity environment of living in.When humidity increases, the polymkeric substance imbibition on micron tube inside and outside wall, pipe thickness increases.Optical resonance wavelength by micro-Raman tester test sandwich structure micron tube based on " whispering gallery modes ".When the wall thickness of micron tube increases, the resonance wavelength of optical resonance ripple moves to long wavelength.Therefore, can utilize sandwich structure micron tube to carry out humidity detection.
Accompanying drawing explanation
The process of sandwich structure micron tube is prepared for the present invention in Fig. 1-5, wherein:
Fig. 1 is Si substrate;
Fig. 2 be on Si substrate patterned photoresist layer as sacrifice layer;
The method that Fig. 3 represents to adopt electron beam evaporation sull of inclined deposition different materials successively on sacrifice layer;
Fig. 4 represents to utilize acetone that sacrifice layer is removed, and makes the oxide film layer on sacrifice layer curling;
Fig. 5 is illustrated in the micro-tubular structure after coated polymer on curling oxide microtubule.
Fig. 6 represents by inclination substrate angle deposition oxide film, utilizes shadow effect to manufacture the removal opening of sacrifice layer, determines film curl direction.
Fig. 7 represents that microtubule is placed in sealing, the controlled environment of humidity, carries out the testing process of resonant optical mode.
When Fig. 8 represents that ambient humidity increases, polymeric layer absorbs and expands, and inside and outside wall thickness increases.
Number in the figure: 1. Si sinks to the bottom; 2. sacrifice layer; 3. internal layer sull; 4. outer oxide thing film; 5. polymkeric substance; 6. sandwich structure micron; 7. the angle that the normal direction of substrate and the incident direction of evaporation source become; 8. evaporation source; 9. airtight container; 10. regulate the saturated salt solution of humidity; 11. incoming laser beams.
Embodiment
Below by example, the present invention is further described.
Below in conjunction with accompanying drawing and instantiation, invention is prepared to sandwich structure micron tube and be described further.
The process of sandwich structure micron tube is prepared for the present invention in Fig. 1-6, and wherein: Fig. 1 is Si substrate, on Si substrate, spin coating photoresist, as sacrifice layer, and carries out photoetching, obtains patterned structures as shown in Figure 2.The method of deposited by electron beam evaporation, on sacrifice layer, first deposit thickness is the outer wall film that 12 nm, material are yttria, rate of sedimentation is 3/s; Deposit thickness is that 24 nm, material are zirconic inner wall membrane again, and rate of sedimentation is 0.5/s, as shown in Figure 3.In deposition process, the normal direction of substrate is become to 60 degree angles (7) with the incident direction of evaporation source, as shown in Figure 6, because inclination substrate angle deposit film exists shadow effect, manufacture by this method the removal opening of sacrifice layer, thereby determine film curl direction.The stress of sacrifice layer is removed and the curly course of film is to complete by supercritical drying instrument, and film is as shown in Figure 4 curling.The diameter of scanning electron microscope oxide microtubule is 7.2 μ m.Finally, oxide microtubule is infiltrated respectively polymer poly acrylic acid/polyetherimide (PAA/PEI) 15 minutes, make coated polymer on the inside and outside wall of microtubule, the original depth of polymer covering layer is about 33 nm.The sandwich structure micron tube obtaining through above-mentioned steps as shown in Figure 5.
Fig. 7 is the schematic diagram that sandwich structure micron tube is carried out humidity detection.Micron tube is placed in to the double dish (9) of sealing, in double dish, places saturated salt solution the humidity environment shown in micron tube is regulated and controled simultaneously.In this example, saturated salt solution used is LiClH
2o, MgCl
26H
2o, Mg (NO
3)
26H
2o, NaCl, KCl and K
2sO
4, corresponding humidity is respectively 12%, 33%, 52%, 75%, 97%.In addition, place silica gel (silica gel) in double dish, can represent the environment of relatively dry, its humidity is 5%.Under the regulation and control of each saturated salt solution or silica gel, utilize the resonant optical mode of micro-Raman tester test sandwich structure micron tube, obtain its resonance wavelength.When the residing humidity of micron tube increases, the polymkeric substance imbibition on tube wall, wall thickness increases, as shown in Figure 8.Now, the optical resonance wavelength of micron tube moves to long wavelength's direction.Experimental result shows, for above-mentioned diameter, is 7.2 μ m, and polymkeric substance original depth is the sandwich structure micron tube of 33 nm, and when humidity is increased to 97% from 5%, its resonance wavelength has moved 11.2 nm (TE mode of resonance, pattern count is 43).Therefore, sandwich structure micron tube can be carried out highly sensitive humidity detection.
Claims (7)
1. a preparation method for sandwich structure micron tube, is characterized in that concrete steps are:
(1) prepare a substrate, on substrate, have patterned sacrifice layer template;
(2) at substrate and above sacrifice layer, deposit the double-deck sull with internal stress; Described internal stress comes from the different heat expansion coefficient of double-deck sull;
(3) optionally remove the partial sacrifice layer between sull and substrate, discharge sull, thus the curling oxide micron tube that becomes;
(4) coated polymer film on the inside and outside wall of oxide micron tube;
The described oxide bilayer film with internal stress that deposits on sacrifice layer of step (2) is the twice corresponding film of deposition in front and back in processes of physical vapor deposition, to form the internal stress due to different heat expansion coefficient between different materials.
2. preparation method according to claim 1, its feature is Si substrate at described substrate, described sacrifice layer is photoresist layer.
3. preparation method according to claim 1 and 2, it is characterized in that utilizing physical vaporous deposition to deposit two-layer sull in patterned photoresist template in step (2), by controlling deposition parameter: the thickness of deposition materials, rate of sedimentation, underlayer temperature or deposition pressure, the double layer planar film that obtains having internal stress, described internal stress comes from double-layer films different heat expansion coefficient; Wherein, control deposit thickness is: 5-100 nm, and rate of sedimentation is 0.2-20/s, underlayer temperature is 25-300
oc, deposition pressure is 10
-3-10
-4pa.
4. preparation method according to claim 1 and 2, it is characterized in that described oxide material is yttria, zirconia, aluminium oxide, titanium dioxide, monox or silicon dioxide one-component, or the multilevel oxide structure of several formations in these oxides.
5. according to the preparation method one of claim 1-4 Suo Shu, it is characterized in that described polymeric material is polypropylene, polyetherimide, polyvinyl alcohol (PVA) one-component, or the multilayer polymer structure of several formations in these polymkeric substance.
6. the sandwich structure micron tube preparing according to the preparation method described in claim 1-5.
7. according to the sandwich structure micron tube described in claim 1-6, as humidity sensor, the humidity in environment is changed the application detecting.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104569064A (en) * | 2015-02-06 | 2015-04-29 | 北京邮电大学 | Graphene gas sensor and preparation method thereof |
| CN104555899A (en) * | 2014-12-18 | 2015-04-29 | 北京邮电大学 | Method for reducing diameter of self-crimping micron tube by virtue of metal nanoparticles |
| CN104591079A (en) * | 2014-12-04 | 2015-05-06 | 复旦大学 | Processing method for micrometer pipe |
| CN109153961A (en) * | 2016-05-24 | 2019-01-04 | 日本电信电话株式会社 | The three-dimension film structural body and its manufacturing method of interior packet molecule |
| CN113008841A (en) * | 2021-02-26 | 2021-06-22 | 复旦大学 | Hydrogen sensor based on palladium-whispering gallery mode optical resonant cavity and preparation and application thereof |
| CN115172521A (en) * | 2022-07-12 | 2022-10-11 | 复旦大学 | Preparation method of curled tubular photoelectric detector |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102305256A (en) * | 2011-09-06 | 2012-01-04 | 复旦大学 | Metal micrometer/nanometer spring as well as preparation method and application thereof |
| CN102431966A (en) * | 2011-12-27 | 2012-05-02 | 复旦大学 | Tubular multi-pore micron motor and preparation method and application thereof |
| CN103774088A (en) * | 2014-02-13 | 2014-05-07 | 复旦大学 | SERS (Surface Enhanced Raman Scattering) probe molecule self-collecting micropipe as well as preparation method and application thereof |
-
2014
- 2014-06-02 CN CN201410238144.0A patent/CN104020152B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102305256A (en) * | 2011-09-06 | 2012-01-04 | 复旦大学 | Metal micrometer/nanometer spring as well as preparation method and application thereof |
| CN102431966A (en) * | 2011-12-27 | 2012-05-02 | 复旦大学 | Tubular multi-pore micron motor and preparation method and application thereof |
| CN103774088A (en) * | 2014-02-13 | 2014-05-07 | 复旦大学 | SERS (Surface Enhanced Raman Scattering) probe molecule self-collecting micropipe as well as preparation method and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| JIAN ZHONG等: "Effect of physisorption and chemisorption of water on resonant modes of rolled-up tubular microcavities", 《NANOSCALE RESEARCH LETTERS》 * |
| JIAO WANG等: "Tubular oxide microcavity with high-index-contrast walls:Mie scattering theory and 3D confinement of resonant modes", 《OPTICS EXPRESS》 * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104591079A (en) * | 2014-12-04 | 2015-05-06 | 复旦大学 | Processing method for micrometer pipe |
| CN104591079B (en) * | 2014-12-04 | 2019-11-12 | 复旦大学 | A kind of processing method of micron of pipeline |
| CN104555899A (en) * | 2014-12-18 | 2015-04-29 | 北京邮电大学 | Method for reducing diameter of self-crimping micron tube by virtue of metal nanoparticles |
| CN104569064A (en) * | 2015-02-06 | 2015-04-29 | 北京邮电大学 | Graphene gas sensor and preparation method thereof |
| CN109153961A (en) * | 2016-05-24 | 2019-01-04 | 日本电信电话株式会社 | The three-dimension film structural body and its manufacturing method of interior packet molecule |
| CN109153961B (en) * | 2016-05-24 | 2022-07-12 | 日本电信电话株式会社 | Three-dimensional film structure containing fine particles and method for producing same |
| CN113008841A (en) * | 2021-02-26 | 2021-06-22 | 复旦大学 | Hydrogen sensor based on palladium-whispering gallery mode optical resonant cavity and preparation and application thereof |
| CN113008841B (en) * | 2021-02-26 | 2022-08-23 | 复旦大学 | Hydrogen sensor based on palladium-whispering gallery mode optical resonant cavity and preparation and application thereof |
| CN115172521A (en) * | 2022-07-12 | 2022-10-11 | 复旦大学 | Preparation method of curled tubular photoelectric detector |
| CN115172521B (en) * | 2022-07-12 | 2024-03-19 | 复旦大学 | Preparation method of coiled tubular photoelectric detector |
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