CN108333198A - A kind of method for observing block copolymer micelle pattern under high temperature of efficiently and accurately - Google Patents
A kind of method for observing block copolymer micelle pattern under high temperature of efficiently and accurately Download PDFInfo
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- CN108333198A CN108333198A CN201810213130.1A CN201810213130A CN108333198A CN 108333198 A CN108333198 A CN 108333198A CN 201810213130 A CN201810213130 A CN 201810213130A CN 108333198 A CN108333198 A CN 108333198A
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- block copolymer
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/02—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material
- G01N23/04—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and forming images of the material
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/03—Investigating materials by wave or particle radiation by transmission
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Abstract
The present invention relates to the methods of block copolymer micelle pattern under a kind of observation high temperature of efficiently and accurately, belong to the method for observation block copolymer micelle pattern.It is poly- using the triblock copolymer polystyrene of a concentration of 1.0mg/ml（4 vinylpyridines）Polyethylene oxide is laboratory sample, uses ethyl alcohol with tetrahydrofuran for solvent, and 10 ~ 14h of constant temperature in 60 ~ 90 DEG C of baking oven uses liquid nitrogen quick freezing micellar solution, solution is dropped in slow evaporation on 300 mesh copper mesh, observes its micella pattern later.The present invention can improve the accuracy of experiment, simplify experimental arrangement, it is easy to operate, it can be achieved that sample batch operation, improve work efficiency.
Description
Technical field
It is the present invention relates to the method for observation block copolymer micelle pattern, more particularly to embedding under different temperatures especially high temperature
The observation procedure of section copolymer micelle pattern.
Background technology
Block copolymer micelle pattern change can it is related with several factors, as block copolymer concentration, solvent ratios,
The factors such as rate of addition, block copolymer each section molecular size range, the rate of volatilization of solvent and the temperature of solvent are related.Room temperature
Under block copolymer micelle pattern be easy to observe by transmission electron microscope, but the micella pattern under high temperature is but difficult to catch
It catches.Because when solvent drops to room temperature by high temperature, Second Aggregation can occur for time longer micella, and micella pattern can also change, because
This is difficult the shape characteristic for observing micella under the condition of high temperature.
Invention content
The present invention provides a kind of method for observing block copolymer micelle pattern under high temperature of efficiently and accurately, to solve to be difficult
Observe block copolymer micelle at high operating temperatures pattern the problem of.
The technical solution adopted by the present invention is that including the following steps：
（1）Choose the triblock copolymer polystyrene-poly of a concentration of 1.0mg/ml（4-vinylpridine）Polyethylene oxide
1ml is laboratory sample in 20ml sample bottles, injects ethyl alcohol and tetrahydrofuran and is settled to 20ml, the ethyl alcohol and tetrahydrofuran volume
It is than 35：65；
（2）Sample bottle is put into 60 ~ 90 DEG C of baking oven, 10 ~ 14h of constant temperature；
（3）Sample bottle is taken out immediately, is placed in the container equipped with liquid nitrogen, is taken out after 2min；
（4）It is static to be dropped to solution on the copper mesh of 300 mesh to room temperature, it is to be measured；
（5）With the micella pattern of transmission electron microscope observing block copolymer, which is the micella pattern at 60 ~ 90 DEG C；
（6）Parallel to do one group of contrast test, remaining experimental condition is constant, room temperature is slowly dropped to after only being taken out from baking oven, so
The micella pattern of block copolymer is observed under transmission electron microscope afterwards.
Step of the present invention（1）In, ethyl alcohol used and tetrahydrofuran are top pure grade.
Step of the present invention（4）In, solution volatilizees naturally after dropping on copper mesh, and rate of volatilization is avoided to change to micella
The influence of pattern.
Step of the present invention（5）In, it chooses different location and observes micella pattern, ensure the accuracy of observation result.
The present invention, which is directed under the condition of high temperature, observes micella pattern, provides embedding under a kind of quick freezing condition of high temperature with liquid nitrogen
Section copolymer solution, the time of Second Aggregation occurs for block copolymer when substantially reducing cooling, slows down block in temperature-fall period
The structural relaxation rate of copolymer makes block copolymer solution only carry out the fine tuning on structure conformation, when not influencing its high temperature
Morphology observations, this method can improve the accuracy of experiment, simplify experimental arrangement, it is easy to operate, it can be achieved that sample batch
Amount operation, improves work efficiency.
Description of the drawings
Fig. 1 is the micella shape appearance figure with the transmission electron microscope observing block copolymer at 90 DEG C of the embodiment of the present invention 1；
Fig. 2 is the observation micella shape appearance figure under transmission electron microscope of 1 contrast test of the embodiment of the present invention.
Specific implementation mode
Embodiment 1
Include the following steps：
（1）Choose the triblock copolymer polystyrene-poly of a concentration of 1.0mg/ml（4-vinylpridine）Polyethylene oxide
1ml is laboratory sample in 20ml sample bottles, injects ethyl alcohol and tetrahydrofuran and is settled to 20ml, the ethyl alcohol and tetrahydrofuran volume
It is than 35：65；
（2）Sample bottle is put into 90 DEG C of baking oven, constant temperature 12h；
（3）Sample bottle is taken out immediately, is placed in the container equipped with liquid nitrogen, is taken out after 2min；
（4）It is static to be dropped to solution on the copper mesh of 300 mesh to room temperature, it is to be measured；
（5）With the micella pattern of transmission electron microscope observing block copolymer, which is the micella pattern at 90 DEG C, referring to
Fig. 1；
（6）Parallel to do one group of contrast test, remaining experimental condition is constant, room temperature is slowly dropped to after only being taken out from baking oven, so
The micella pattern for observing block copolymer under transmission electron microscope afterwards, referring to Fig. 2；
The step（1）In, ethyl alcohol used and tetrahydrofuran are top pure grade；
The step（4）In, solution volatilizees naturally after dropping on copper mesh, and rate of volatilization is avoided to change the shadow to micella pattern
It rings；
The step（5）In, it chooses different location and observes micella pattern, ensure the accuracy of observation result.
Embodiment 2
Include the following steps：
（1）Choose the triblock copolymer polystyrene-poly of a concentration of 1.0mg/ml（4-vinylpridine）Polyethylene oxide
1ml is laboratory sample in 20ml sample bottles, injects ethyl alcohol and tetrahydrofuran and is settled to 20ml, the ethyl alcohol and tetrahydrofuran volume
It is than 35：65；
（2）Sample bottle is put into 60 DEG C of baking oven, constant temperature 14h；
（3）Sample bottle is taken out immediately, is placed in the container equipped with liquid nitrogen, is taken out after 2min；
（4）It is static to be dropped to solution on the copper mesh of 300 mesh to room temperature, it is to be measured；
（5）With the micella pattern of transmission electron microscope observing block copolymer, which is the micella pattern at 60 DEG C；
（6）Parallel to do one group of contrast test, remaining experimental condition is constant, room temperature is slowly dropped to after only being taken out from baking oven, so
The micella pattern of block copolymer is observed under transmission electron microscope afterwards；
The step（1）In, ethyl alcohol used and tetrahydrofuran are top pure grade；
The step（4）In, solution volatilizees naturally after dropping on copper mesh, and rate of volatilization is avoided to change the shadow to micella pattern
It rings；
The step（5）In, it chooses different location and observes micella pattern, ensure the accuracy of observation result.
Embodiment 3
Include the following steps：
（1）Choose the triblock copolymer polystyrene-poly of a concentration of 1.0mg/ml（4-vinylpridine）Polyethylene oxide
1ml is laboratory sample in 20ml sample bottles, injects ethyl alcohol and tetrahydrofuran and is settled to 20ml, the ethyl alcohol and tetrahydrofuran volume
It is than 35：65；
（2）Sample bottle is put into 75 DEG C of baking oven, constant temperature 10h；
（3）Sample bottle is taken out immediately, is placed in the container equipped with liquid nitrogen, is taken out after 2min；
（4）It is static to be dropped to solution on the copper mesh of 300 mesh to room temperature, it is to be measured；
（5）With the micella pattern of transmission electron microscope observing block copolymer, which is the micella pattern at 75 DEG C；
（6）Parallel to do one group of contrast test, remaining experimental condition is constant, room temperature is slowly dropped to after only being taken out from baking oven, so
The micella pattern of block copolymer is observed under transmission electron microscope afterwards；
Step of the present invention（1）In, ethyl alcohol used and tetrahydrofuran are top pure grade；
Step of the present invention（4）In, solution volatilizees naturally after dropping on copper mesh, and rate of volatilization is avoided to change to micella pattern
Influence；
Step of the present invention（5）In, it chooses different location and observes micella pattern, ensure the accuracy of observation result.
Claims (4)
1. the method for block copolymer micelle pattern under a kind of observation high temperature of efficiently and accurately, which is characterized in that including following step
Suddenly：
（1）Choose the triblock copolymer polystyrene-poly of a concentration of 1.0mg/ml（4-vinylpridine）Polyethylene oxide
1ml is laboratory sample in 20ml sample bottles, injects ethyl alcohol and tetrahydrofuran and is settled to 20ml, the ethyl alcohol and tetrahydrofuran volume
It is than 35：65；
（2）Sample bottle is put into 60 ~ 90 DEG C of baking oven, 10 ~ 14h of constant temperature；
（3）Sample bottle is taken out immediately, is placed in the container equipped with liquid nitrogen, is taken out after 2min；
（4）It is static to be dropped to solution on the copper mesh of 300 mesh to room temperature, it is to be measured；
（5）With the micella pattern of transmission electron microscope observing block copolymer, which is the micella pattern at 60 ~ 90 DEG C；
（6）Parallel to do one group of contrast test, remaining experimental condition is constant, room temperature is slowly dropped to after only being taken out from baking oven, so
The micella pattern of block copolymer is observed under transmission electron microscope afterwards.
2. the method for block copolymer micelle pattern under a kind of observation high temperature of efficiently and accurately according to claim 1,
It is characterized in that, the step（1）In, ethyl alcohol used and tetrahydrofuran are top pure grade.
3. the method for block copolymer micelle pattern under a kind of observation high temperature of efficiently and accurately according to claim 1,
It is characterized in that, the step（4）In, solution volatilizees naturally after dropping on copper mesh, and rate of volatilization is avoided to change to micella pattern
Influence.
4. the method for block copolymer micelle pattern under a kind of observation high temperature of efficiently and accurately according to claim 1,
It is characterized in that, the step（5）In, it chooses different location and observes micella pattern, ensure the accuracy of observation result.
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| CN201810213130.1A CN108333198A (en) | 2018-03-15 | 2018-03-15 | A kind of method for observing block copolymer micelle pattern under high temperature of efficiently and accurately |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101632834A (en) * | 2009-07-29 | 2010-01-27 | 吉林大学 | Magnetic nano-carrier with targeted hydrophobic drug delivery to tumor and preparation method thereof |
| CN102295772A (en) * | 2011-05-20 | 2011-12-28 | 西北工业大学 | Monomethoxy polyethylene glycol-poly(L-tryptophan) amphipathic segmented copolymer, preparation method thereof and preparation method of drug loaded miceller solution thereof |
| CN103120644A (en) * | 2011-11-17 | 2013-05-29 | 山东绿叶制药有限公司 | Amphiphilic segmented copolymer micelle of macromolecules of biologically functional protein and preparation and application thereof |
| CN104725581A (en) * | 2015-02-02 | 2015-06-24 | 北京科技大学 | Method for preparing and applying light/temperature sensitive amphiphilic block polymer micelle |
| CN105044133A (en) * | 2015-06-01 | 2015-11-11 | 国家纳米科学中心 | Transmission electron microscope simple detection method directed at polymer nano-material |
| CN105646918A (en) * | 2016-02-03 | 2016-06-08 | 北京大学 | Preparing, regulating and control method for stable nanometer pattern based on cross-linkable high polymer material |
-
2018
- 2018-03-15 CN CN201810213130.1A patent/CN108333198A/en not_active Withdrawn
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101632834A (en) * | 2009-07-29 | 2010-01-27 | 吉林大学 | Magnetic nano-carrier with targeted hydrophobic drug delivery to tumor and preparation method thereof |
| CN102295772A (en) * | 2011-05-20 | 2011-12-28 | 西北工业大学 | Monomethoxy polyethylene glycol-poly(L-tryptophan) amphipathic segmented copolymer, preparation method thereof and preparation method of drug loaded miceller solution thereof |
| CN103120644A (en) * | 2011-11-17 | 2013-05-29 | 山东绿叶制药有限公司 | Amphiphilic segmented copolymer micelle of macromolecules of biologically functional protein and preparation and application thereof |
| CN104725581A (en) * | 2015-02-02 | 2015-06-24 | 北京科技大学 | Method for preparing and applying light/temperature sensitive amphiphilic block polymer micelle |
| CN105044133A (en) * | 2015-06-01 | 2015-11-11 | 国家纳米科学中心 | Transmission electron microscope simple detection method directed at polymer nano-material |
| CN105646918A (en) * | 2016-02-03 | 2016-06-08 | 北京大学 | Preparing, regulating and control method for stable nanometer pattern based on cross-linkable high polymer material |
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