CN104390878A - Real-time and in-situ quantitative determination method of mass of solution in thin polymer film and viscoelasticity of thin polymer film - Google Patents
Real-time and in-situ quantitative determination method of mass of solution in thin polymer film and viscoelasticity of thin polymer film Download PDFInfo
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- CN104390878A CN104390878A CN201410609737.3A CN201410609737A CN104390878A CN 104390878 A CN104390878 A CN 104390878A CN 201410609737 A CN201410609737 A CN 201410609737A CN 104390878 A CN104390878 A CN 104390878A
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- 229920006254 polymer film Polymers 0.000 title claims abstract description 48
- 238000011065 in-situ storage Methods 0.000 title description 3
- 238000004445 quantitative analysis Methods 0.000 title 1
- 238000003380 quartz crystal microbalance Methods 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 24
- 238000012417 linear regression Methods 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims description 45
- 229940059939 kayexalate Drugs 0.000 claims description 13
- 229920001467 poly(styrenesulfonates) Polymers 0.000 claims description 13
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 8
- 150000003839 salts Chemical class 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 230000010355 oscillation Effects 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000013078 crystal Substances 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000010453 quartz Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 238000000961 QCM-D Methods 0.000 claims description 3
- MPNXSZJPSVBLHP-UHFFFAOYSA-N 2-chloro-n-phenylpyridine-3-carboxamide Chemical compound ClC1=NC=CC=C1C(=O)NC1=CC=CC=C1 MPNXSZJPSVBLHP-UHFFFAOYSA-N 0.000 claims description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 2
- 239000005864 Sulphur Substances 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 230000001476 alcoholic effect Effects 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 claims description 2
- LLLCSBYSPJHDJX-UHFFFAOYSA-M potassium;2-methylprop-2-enoate Chemical compound [K+].CC(=C)C([O-])=O LLLCSBYSPJHDJX-UHFFFAOYSA-M 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- 229920000867 polyelectrolyte Polymers 0.000 abstract description 9
- 230000008961 swelling Effects 0.000 abstract description 6
- 239000007788 liquid Substances 0.000 abstract description 4
- 239000010409 thin film Substances 0.000 abstract description 3
- 239000010408 film Substances 0.000 description 8
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 238000005259 measurement Methods 0.000 description 5
- 239000004793 Polystyrene Substances 0.000 description 4
- 229920002223 polystyrene Polymers 0.000 description 4
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 3
- 239000004593 Epoxy Substances 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000010100 anticoagulation Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 150000004678 hydrides Chemical class 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000013507 mapping Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000002572 peristaltic effect Effects 0.000 description 1
- 229920001983 poloxamer Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000006277 sulfonation reaction Methods 0.000 description 1
- HHPPHUYKUOAWJV-UHFFFAOYSA-N triethoxy-[4-(oxiran-2-yl)butyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCCC1CO1 HHPPHUYKUOAWJV-UHFFFAOYSA-N 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- Manufacture Of Macromolecular Shaped Articles (AREA)
- Moulding By Coating Moulds (AREA)
Abstract
The invention relates to a method for measuring the mass of a solution in a thin polymer film and the viscoelasticity of the thin polymer film. The method comprises the steps that (1) in a quartz crystal microbalance, frequency and dissipation change values of a standard chip caused by a solution and frequency and dissipation change values of a standard chip covered by the thin polymer film caused by the solution are recorded in real time, and are subtracted to obtain the frequency and dissipation change values of the solution in the thin polymer film; (2) a product of a frequency multiplying number and the dissipation change value of the solution in the thin polymer film is taken as an X-coordinate, and the ratio of the frequency change value of the solution in the thin polymer film to the frequency multiplying number is taken as a Y-coordinate to make a linear regression equation, so that the intercept of the linear regression equation on a Y-axis is the mass of the solution in the thin polymer film, and the slope of the linear regression equation is the retardation time of the thin polymer film. The method can be used for measuring the mass of the solution in the thin film and the viscoelasticity of the thin film in real time simply and accurately in a liquid environment. The method is particularly suitable for measuring a high-viscoelasticity polyelectrolyte brush brought by highly hydrated swelling.
Description
Technical field
The invention belongs to fields of measurement, be specifically related to a kind of solution quality and viscoelastic method thereof in real-time in-situ quantitative measurement thin polymer film.
Background technology
Polymkeric substance all has a wide range of applications in production and life, and the macromolecule particularly on solid-liquid surface and interface, greatly attracts the research interest of people.In such as oil exploitation, pluronic polymer is amphipathic, the high molecular lubrication in artificial joint place, high molecular anti-coagulation effect in colloidal interface place etc.Therefore the solution content characterizing accurately and quantitatively solid-liquid interface place has vital effect.
Dissipative type QCM (Quartz Crystal Microbalance) (Quartz Crystal Microbalance, QCM-D) is the new technology of a kind of meter interface quality and viscoelasticity change, has 10
-9the sensitivity of g level and the feature of Real-Time Monitoring.Its ultimate principle is based on inverse piezoelectric effect and Sauerbrey equation.Its uniform ground in a vacuum, isotropy, hard thin film study aspect obtain great success (as monitored vapour deposition speed in ultrahigh vacuum), are progressively applied to afterwards (if Real-Time Monitoring Proteins In Aqueous Solutions is at the absorption behavior of bioelectric interface) in the measurement of liquid phase environment.But it is well known that when Sauerbrey equation is applied in liquid phase, because film height is swelling, high viscoelasticity that is that bring can make solution content be underestimated.This makes the accuracy of QCM (Quartz Crystal Microbalance) decrease.Although based on Qtools software (the Q-sense company of viscoelastic model, Sweden) can address this problem, but outside the step removing it is comparatively loaded down with trivial details, fit solution unsatisfactory (polyelectrolyte brush film as high in viscoelasticity) in some cases.
Summary of the invention
The object of the invention is to provide one to measure solution quality and viscoelastic method thereof in thin polymer film in real time, simply and effectively.
In thin polymer film provided by the present invention, solution quality and viscoelastic method thereof, comprise the steps:
1) standard chips is placed in QCM (Quartz Crystal Microbalance), makes quartz crystal be periodically free oscillation, then pass into solution, frequency change (the △ F of the standard chips caused by real time record solution
s,n) and dissipate varied value (△ D
s,n);
2) the described standard chips being coated with thin polymer film is placed in QCM (Quartz Crystal Microbalance), make quartz crystal be step 1) described in periodically free oscillation, then pass into the step 1 of same amount by same traffic) described in solution, frequency change (the △ F being coated with the standard chips of thin polymer film caused by real time record solution
n) and dissipate varied value (△ D
n);
3) by step 2) and step 1) in the frequency change of same time point and dissipate varied value subtract each other respectively, namely obtain frequency change (the △ F of the standard chips caused by the solution in thin polymer film
r, n) and dissipate varied value (△ D
r,n);
4) with dissipate varied value (the △ D of the standard chips caused by the solution in different frequency (n) and thin polymer film
r,n) product (n △ D
r,n) be horizontal ordinate, with dissipate varied value (the △ F of the standard chips caused by the solution in thin polymer film
r,n) and ratio (the △ F of frequency (n)
r,n/ n) make equation of linear regression for ordinate, the intercept of equation of linear regression on axis of ordinates of gained is solution quality (m) in thin polymer film; The slope of equation of linear regression be the retardation time of thin polymer film according to τ=η/μ, calculate the elastic modulus of thin polymer film, wherein, τ is the retardation time of thin polymer film, and η is the viscosity of thin polymer film, and μ is the elastic modulus of thin polymer film.
In said method, step 1) in, the INSTRUMENT MODEL of described QCM (Quartz Crystal Microbalance) is E1 type QCM-D, and purchased from Q-Sense company of Sweden, fundamental frequency is 5MHz.
Described standard chips is the dry state standard chips through removing surface, and as production code member QSX-303, purchased from Q-Sense company of Sweden, removing surface is UV-ozone cleaning.
The free-running oscillation frequency of described periodicity is 5MHz-65MHz.
Described solution is deionized water, salt solusion, methyl alcohol and ethanol etc., and described salt solusion is the alcoholic solution of sodium chloride salt aqueous solution, potassium chloride salt aqueous solution and sodium chloride, and the concentration range of described salt solusion is 10
-5mol/L-2mol/L.
Described solution pass into flow velocity 50 μ L/min-150 μ L/min.
In said method, step 2) in, the thickness of described thin polymer film is not more than 100nm, described thin polymer film is the thin polymer film of high-hydrophilic, as polyelectrolyte brush, specifically can be kayexalate brush, polymethyl acyloxyethyl trimethyl ammonium chloride brush, polymethylacrylic acid 3-sulphur methacrylate potassium salt brush etc.
The film of high-hydrophilic can have high viscoelasticity because of water suction.
In said method, step 3) in, frequency change and the dissipate varied value of the standard chips caused by thin polymer film are made up of two parts: a part for thin polymer film is interior and between polymkeric substance with fluid mechanics interact the solution molecule combined quality caused by frequency change and dissipate varied, do not comprise the contribution of polymkeric substance in thin polymer film; The frequency change of another part caused by the viscoelasticity of thin polymer film self and dissipate varied.
In said method, step 4) in, described frequency is 3,5,7,9,11 and 13.
Measuring method of the present invention, in maintenance QCM (Quartz Crystal Microbalance) 10
-9on the basis of the sensitivity of g level and real-time measuring characteristic, provide real-time in liquid environment, simple and easy and the solution quality obtained exactly in film and the viscoelastic method of film.Be specially adapted to the research of the viscoelastic polyelectrolyte brush of height brought because high degree of hydration is swelling.
Accompanying drawing explanation
Fig. 1 is the frequency change of self and the dissipate varied value of kayexalate brush in embodiment 1, and wherein numeral 3 is 3 frequencys multiplication of QCM (Quartz Crystal Microbalance), and two arrows represent 1 × 10 from left to right respectively
-3mol/L NaCl salt solusion and deionized water replace the time of forma solution, and figure top " flowing " and " static " is illustrated as the state of peristaltic pump, wherein, and σ=0.07chainsnm in figure
-2represent grafting density (the macromolecular chain number of grafting in unit area).
Fig. 2 is the real time data fit procedure figure of the kayexalate brush in embodiment 1, and wherein digital n is the n frequency multiplication (be 3,5,7,9,11,13 amount to 6 numerical value) of QCM (Quartz Crystal Microbalance).
Fig. 3 is the data fitting result figure of the kayexalate brush in embodiment 1, comprise two physical quantitys retardation time (τ) of (a) solution quality (m) and (b) film in film, in figure, arrow represents that sodium chloride salt aqueous solution starts to replace the moment of deionized water.
Embodiment
Method of the present invention is described by specific embodiment below in conjunction with accompanying drawing; but the present invention is not limited thereto; all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Experimental technique described in following embodiment, if no special instructions, is conventional method; Described reagent and material, if no special instructions, all can obtain from commercial channels.
Solution quality and viscoelastic the real time measure thereof in embodiment 1, kayexalate brush
1) preparation of kayexalate brush: had on surface the chip of silicon dioxide coating to do hydrophilic treatment, makes its rich surface containing silicone hydroxyl.The silicon chip of drying is placed in the anhydrous cyclohexane solvent of epoxy radicals silicone hydride reagent (5,6-epoxyhexyl triethoxysilane) and carries out self assembly, make its rich surface containing epoxy radicals.Be amino polystyrene (PS-NH by end
2, M
n=32 × 10
3gmol
-1; M
w/ M
n=1.04) toluene solution is spun on the chip surface being rich in epoxy radicals, in vacuum drying oven, react 24h at 160 DEG C.Fall the polystyrene molecule of non-grafting afterwards with toluene drip washing, namely wash surperficial unreacted polystyrene molecule off, obtained polystyrene brush.Then with 1 of sulfuric acid and acetic anhydride (volume ratio is for 1:3), 2-dichloroethane solution carries out soft sulfonation process as sulfonated reagent p-poly-phenyl ethene brush, obtain kayexalate brush, the dry brush thickness that elliptical polarizer characterizes is about 15nm, and the swelling rear thickness of deionized water is about 40nm.
2) the real time measure of kayexalate brush frequency and dissipation: have the chip of polyelectrolyte brush to be placed in QCM (Quartz Crystal Microbalance) by long for surface under dry state, open circuit, crystal is made to be periodically free oscillation (fundamental frequency is 5MHz), then solution (as deionized water or salt solusion) is passed into, the frequency change of the polyelectrolyte brush chip that real time record solution causes and dissipate varied value (△ F
nwith △ D
n).Use QCM (Quartz Crystal Microbalance) measurement standard chip to repeat above-mentioned steps, frequency change that solution causes and dissipate varied value (△ F can be obtained
s,nwith △ D
s,n).Above-mentioned corresponding frequency change and dissipate varied value are subtracted each other, frequency and dissipate varied (the △ F of kayexalate brush self can be obtained
r,nwith △ D
r,n).The frequency change in each stage and the relation of dissipate varied value are as shown in Figure 1, as can be seen from Figure 1: the frequency under each frequency or dissipate varied curve widely different, cannot calculate by traditional method (Sauerbrey equation) solution content obtained in polyelectrolyte brush.
3) solution quality and viscoelastic the real time measure thereof in kayexalate brush: extract frequency change (the △ F under each frequency (n)
r, n/ n) product (n △ D to frequency and dissipate varied
r, n) mapping, carry out matching.Fit procedure as shown in Figure 2, can obtain from Fig. 2: the linear fit situation all very good (degree of fitting is greater than 0.99) each moment t corresponding with Fig. 1, namely the method is very suitable for obtaining the solution content in kayexalate, the 435s moment of each bar straight line from left to right successively in representative graph 1,470s moment, 507s moment and 576s moment in Fig. 2.
The solution quality (m) polyelectrolyte brush can be obtained from ordinate intercept, and the retardation time (τ=η/μ, η are viscosity, and μ is elastic modulus) of polyelectrolyte brush can be obtained from slope.Fitting result as shown in Figure 3, as can be seen from Figure 3: according to the experimental technique in Fig. 2, just can obtain the swelling curve of the kayexalate brush corresponding with Fig. 1 in real time.This is significant to the Swelling Dynamics studying hydrophilic film in real time.Fig. 3 (a) and (b) represent corresponding solution quality (m) and retardation time (τ) over time respectively, and horizontal ordinate and Fig. 1 are strictly corresponding.
Claims (4)
1. measure solution quality and a viscoelastic method thereof in thin polymer film, comprise the steps:
1) standard chips is placed in QCM (Quartz Crystal Microbalance), makes quartz crystal be periodically free oscillation, then pass into solution, the frequency change of the standard chips caused by real time record solution and dissipate varied value;
2) standard chips being coated with thin polymer film is placed in QCM (Quartz Crystal Microbalance), make quartz crystal be and step 1) in the vibration of same period free love, then pass into the step 1 of same amount) described in solution, the frequency change being coated with the standard chips of thin polymer film caused by real time record solution and dissipate varied value;
3) by step 2) and step 1) in the frequency change of same time point and dissipate varied value subtract each other respectively, namely obtain frequency change and the dissipate varied value of the standard chips in thin polymer film caused by solution;
4) with the product of the dissipate varied value of the standard chips in frequency and thin polymer film caused by solution for horizontal ordinate, with the ratio of the frequency change of the standard chips in thin polymer film caused by solution and frequency for ordinate makes equation of linear regression, then the intercept of equation of linear regression on axis of ordinates is solution quality in thin polymer film; The slope of equation of linear regression is the retardation time of thin polymer film, according to τ=η/μ, calculates the elastic modulus of thin polymer film, and wherein, τ is the retardation time of thin polymer film, and η is the viscosity of thin polymer film, and μ is the elastic modulus of thin polymer film.
2. method according to claim 1, is characterized in that: step 1) in, the INSTRUMENT MODEL of described QCM (Quartz Crystal Microbalance) is E1 type QCM-D;
The fundamental frequency of described instrument is 5MHz;
Described standard chips is the dry state standard chips through removing surface;
The free-running oscillation frequency of described periodicity is 5MHz-65M Hz;
Described solution is deionized water, salt solusion, methyl alcohol and ethanol;
Described salt solusion is the alcoholic solution of sodium chloride salt aqueous solution, potassium chloride salt aqueous solution and sodium chloride, and the concentration range of described salt solusion is 10
-5mol/L-2mol/L;
The flow that passes into of described solution is 50 μ L/min-150 μ L/min.
3. method according to claim 1 and 2, is characterized in that: step 2) in, the thickness of described thin polymer film is not more than 100nm;
Described thin polymer film is high-hydrophilic thin polymer film;
Described thin polymer film is selected from the polymer brush that any one polymkeric substance following is formed: kayexalate, polymethyl acyloxyethyl trimethyl ammonium chloride and polymethylacrylic acid 3-sulphur methacrylate potassium salt.
4. the method according to any one of claim 1-3, is characterized in that: step 4) in, described frequency is 3,5,7,9,11 and 13.
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|---|---|---|---|
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|---|---|---|---|
| CN201410609737.3A CN104390878B (en) | 2014-11-03 | 2014-11-03 | Solution quality and viscoelastic method thereof in a kind of real-time in-situ quantitative determination thin polymer film |
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| CN104390878B CN104390878B (en) | 2016-09-07 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105675442A (en) * | 2016-01-26 | 2016-06-15 | 浙江理工大学 | Method for measuring viscosity of substrate support polymer film |
| CN106248528A (en) * | 2016-09-27 | 2016-12-21 | 中国石油天然气股份有限公司 | Method for evaluating elasticity of polymer |
| CN106422795A (en) * | 2016-09-21 | 2017-02-22 | 西安建筑科技大学 | Preparation method of polyamide quartz crystal chip |
| CN109682709A (en) * | 2017-10-19 | 2019-04-26 | 中国科学院化学研究所 | A kind of method of the relaxation behavior of measurement polyelectrolyte brush inside counter ion counterionsl gegenions pair |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105675442A (en) * | 2016-01-26 | 2016-06-15 | 浙江理工大学 | Method for measuring viscosity of substrate support polymer film |
| CN106422795A (en) * | 2016-09-21 | 2017-02-22 | 西安建筑科技大学 | Preparation method of polyamide quartz crystal chip |
| CN106422795B (en) * | 2016-09-21 | 2018-11-02 | 西安建筑科技大学 | A kind of preparation method of polyamide quartz crystal chip |
| CN106248528A (en) * | 2016-09-27 | 2016-12-21 | 中国石油天然气股份有限公司 | Method for evaluating elasticity of polymer |
| CN109682709A (en) * | 2017-10-19 | 2019-04-26 | 中国科学院化学研究所 | A kind of method of the relaxation behavior of measurement polyelectrolyte brush inside counter ion counterionsl gegenions pair |
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| Publication number | Publication date |
|---|---|
| CN104390878B (en) | 2016-09-07 |
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