CN103018493A - Device and method for preparing PVDF (polyvinylidene fluoride) microparticle probe by using melting-sintering method - Google Patents
Device and method for preparing PVDF (polyvinylidene fluoride) microparticle probe by using melting-sintering method Download PDFInfo
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- CN103018493A CN103018493A CN2012104763900A CN201210476390A CN103018493A CN 103018493 A CN103018493 A CN 103018493A CN 2012104763900 A CN2012104763900 A CN 2012104763900A CN 201210476390 A CN201210476390 A CN 201210476390A CN 103018493 A CN103018493 A CN 103018493A
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Abstract
The invention discloses a device and a method for preparing a PVDF (polyvinylidene fluoride) microparticle probe by using a melting-sintering method. The device comprises a micro-operation device and a microscope which are arranged on a foundation table, wherein an L-shaped probe clamp is arranged at the end head of the micro-operation device, and a lens of the microscope and the L-shaped probe clamp are oppositely arranged. The method comprises the following steps of: 1) preparing an aluminium alloy metal wire with a micron-scale tip; 2) dispersing PVDF microparticles; 3) sequentially adhering a non-PVDF solvent and the PVDF microparticles at the free end of a micro-suspension arm of an AFM (atomic force microscope) tipless probe which is installed on the L-shaped probe clamp; and 4) drying the obtained probe adhered with the PVDF microparticles in the step 3) in a constant-temperature oven for a period of time, so as to obtain the PVDF microparticle probe. The device and the method disclosed by the invention are simple and practicable, and strong in practicability; and the obtained PVDF microparticle probe is low in cost, wide in source, free from introducing adhesive pollution, easy to adsorb various organic pollutants, and capable of being widely applied to membrane pollution analysis.
Description
Technical field
The invention belongs to atomic force microscope (AFM) probe preparation field, be specifically related to the device and method of the standby PVDF microparticle probe of a kind of molten sintering legal system.
Background technology
Membrane separation technique develops rapidly in the application of giving the fields such as water treatment, advanced treatment of wastewater, becomes the important technical that solves source quality pollution and reutilization of the sewage etc.It still is its major obstacle of applying that but film pollutes the membrane flux and the irreversible attenuation problem of performance that cause.Research previously is that analyzing film pollutes on the macroscopic aspect mostly, not the interaction force between film/pollutant, pollutant/pollutant from microcosmic angle quantitative measurement film application process.And along with appearance and the development of atomic force microscope (AFM), it is with the advantage at the interaction force between effective mensuration AFM probe and the face under the varying environments such as air, vacuum, liquid state, solved rapidly the problems referred to above, become from microcosmic angle and resolve the basic means that film pollutes.But, common AFM probe all is to be prepared from by silicide, use the acting force between its diffusion barrier of measuring AFM probe and different pollution levels, what obtain is acting force between silicide and film and silicide and the pollutant, therefore can not effectively measure the interaction force between film/pollutant in the actual moving process, pollutant/pollutant, so microparticle probe modification technology (adhere to the known spheric grain of a composition at AFM probe micro-cantilever free end and measure microcosmic power) is introduced into diffusion barrier pollution parsing field.
Consider that major pollutants are humic acid in the sewage, polysaccharide, protein, so diffusion barrier researcher previously mainly is preparation-COOH,-OH and bovine serum albumin (BSA) microparticle probe replaces conventional probe, be used for measuring the interaction force between the film surface of above-mentioned probe and different pollution levels, although obtained certain achievement in research, but, above-mentioned probe expensive, kind is single, the preparation method is complicated, and easily sex change, yield rate is low, to preparation condition, the requirement of preservation condition and test environment is very strict, the simultaneously use of adhesive can be polluted the microparticle that adheres to; In addition, existing probe preparation facilities, for example, the disclosed two-way three-dimensional mobile platform legal system of patent CN101643195A is many for the related device quantity of colloid probe, flow process is complicated, complex operation.Based on this, the present invention use most widely used macromolecule member material it---PVDF, by the standby PVDF microparticle probe of molten sintering legal system, avoided the use of adhesive, the organic contaminant of the adsorbable various complexity of gained PVDF probe forms the pollutant probe simultaneously; And PVDF microparticle low price, not changeableness.Probe preparation facilities used in the present invention is simple, easy operating, yield rate are high, practical.The gained probe can measure under the multiple environmental baseline its from the film of different pollution levels between interaction force, effectively realized the quantitative measurement of film/pollutant and pollutant/pollutant interaction power, according to the gained micro force, can recover Choice of Countermeasures to the selection of membrane material, runtime film properties, suitablely provide guidance to regulation and control working procedure strategy etc.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, one of its purpose provides a kind of AFM microparticle probe preparation facilities, this device simple and fast, easy operating, practical, cost is low.
Another object of the present invention is to provide the method based on the standby PVDF microparticle probe of molten sintering legal system of this AFM microparticle probe preparation facilities.The method flow process is simple, is easy to realize, and is practical, avoided simultaneously the use of adhesive to the pollution of adhesion PVDF microparticle.
The objective of the invention is to realize by following technical proposals.
The device of the standby PVDF microparticle probe of a kind of molten sintering legal system comprises the micromanipulator and the microscope that are arranged on the basic platform, and described micromanipulator termination is provided with " L-type " Probe clip, and described microscopical camera lens is oppositely arranged with " L-type " Probe clip.
Further, in the device of the present invention:
Described " L-type " Probe clip is combined by " L-type " connecting link probe station that is threaded, and described probe station end face is provided with the probe slot of placing the AFM tipless cantilever, is pressed with reed on the described probe slot; The elongated end of described reed, the end of probe station are provided with to prop " I type " copper post of reed.
Described " L-type " Probe clip is made by stainless steel material.
Correspondingly, the present invention has provided and has utilized said apparatus to carry out the method for the standby PVDF microparticle probe of molten sintering legal system, may further comprise the steps:
1) is that 7-10 ㎝, diameter are that an end of the Al-alloy metal silk of 2mm impregnated in 12-24h in the concentrated hydrochloric acid with length, obtains the most advanced and sophisticated tinsel of 20-40 μ m that is; Then be placed in the ultrapure water ultrasonic cleaning
5-15min；
2) the AFM tipless cantilever is installed in the probe slot that is arranged on the probe station, " L-type " Probe clip is linked to each other with micromanipulator, have the three-dimensional of the probe station of AFM tipless cantilever to move by micromanipulator control clamping;
3) the PVDF particle is scattered in microslide a surface; Use the wiry most advanced and sophisticated PVDF of the dispersion particle of step 1) at microscopically;
4) non-PVDF solvent droplets is moved to microslide b surface, then microslide b is placed field of microscope;
5) the rotating probe platform is so that the probe slot place flats down, and then the three-dimensional by micromanipulator control " L-type " Probe clip moves, so that the AFM tipless cantilever micro-cantilever free end that is clamped in the probe slot is stained with non-PVDF solvent;
6) microslide b is removed from field of microscope, the microslide a that step 3) is loaded with the PVDF microparticle moves in the optical microscope visual field;
7) the control clamping has the three-dimensional of the probe station of AFM tipless cantilever to move, and purpose PVDF microparticle is adsorbed on AFM tipless cantilever micro-cantilever free end;
The AFM tipless cantilever that 8) will be loaded with the PVDF microparticle takes off from probe station, then is placed in the constant temperature oven and leaves standstill, and obtains PVDF microparticle probe.
Further, in the method for the invention:
Described PVDF microparticle is the spheric grain of 5-20 μ m.
Described non-PVDF solvent includes but not limited to the arbitrary proportion mixed liquor of deionized water, glycerine, ethanol and above-mentioned several solvents.
Described constant temperature oven temperature is 112 ~ 145 ℃, and the time of repose of PVDF microparticle probe in baking oven is 10-40min.
Compared with prior art, advantage of the present invention and beneficial effect are: this invention equipment therefor simple and fast, easy operating, practical, cost is low.This invention has avoided the use of adhesive to the pollution of microparticle by using the standby PVDF microparticle probe of molten sintering legal system, has promoted the accuracy that microcosmic power is measured.Film pollution mechanism-COOH is resolved in the PVDF probe of this invention preparation and traditional being used for,-OH and BSA microparticle probe are compared, not only low, the wide material sources of price, to preparation and test environment no requirement (NR), non-changeableness, and adsorb easily various pollutants, realized effective quantitative measurement of film and pollutant and pollutant interaction power.
Description of drawings
Fig. 1 is AFM probe preparation facilities system diagram;
Fig. 2 is " L-type " Probe clip synoptic diagram;
Fig. 3 is view under the PVDF microparticle probe microscope of 8 μ m;
Fig. 4 is view under the PVDF microparticle probe microscope of 5 μ m;
Fig. 5 is view under the PVDF microparticle probe microscope of 9 μ m;
Fig. 6 is view under the PVDF microparticle probe microscope of 10 μ m;
Fig. 7 is view under the PVDF microparticle probe microscope of 20 μ m.
Among the figure: 1, micromanipulator; 2, " L-type " Probe clip; 3, microscope; 4, connecting link; 5, probe station; 6, screw; 7, reed; 8, probe slot; 9, " I type " copper post.
Embodiment
Below in conjunction with instantiation the present invention is further detailed, but described example is not construed as limiting the invention.
Device of the present invention comprises the micromanipulator 1 and the microscope 3 that are arranged on the basic platform as shown in Figure 1, and micromanipulator 1 termination is provided with " L-type " Probe clip 2, and the camera lens of microscope 3 is oppositely arranged with " L-type " Probe clip 2.
As shown in Figure 2, " L-type " Probe clip 2 is combined by " L-type " connecting link 4 probe station 5 that is threaded, and probe station 5 end faces are provided with the probe slot 8 of placing the AFM tipless cantilever, and the upper end of probe slot 8 is provided with by the fixing reed 7 of screw 6; The end of the elongated end of reed 7, probe station 5 is provided with to prop " I type " copper post 9 of reed 7.Should adopt stainless steel material to make by " L-type " Probe clip 2.
Method of the present invention elaborates by following embodiment.
Embodiment 1
1) is that 10 ㎝, diameter are that an end of the Al-alloy metal silk of 2mm impregnated in 24h in the concentrated hydrochloric acid with length, obtains the tinsel that the tip is 21 μ m; Then be placed in the ultrapure water ultrasonic cleaning 15min;
2) unclamp screw 6, to place the reed 7 of probe slot 8 tops along 90 ° of transfers, the AFM tipless cantilever that commerce is bought is installed in the probe slot 8, and reed 7 is depressed on the AFM tipless cantilever that is placed in the probe slot 8 along-90 ° of transfers, then tightens the screw 6 of clip 7; Link to each other with micromanipulator 1 with the A end of the fixed screw on the micromanipulator 1 with connecting link 4 at last, the three-dimensional of controlling the AFM tipless cantilever by microoperation 1 moves;
3) adopt 1000 eye mesh screens that the PVDF particle is scattered in microslide a surface; Use for 3 times the tinsel tip of step 1) gained to disperse the PVDF particle at optical microscope, in case a large amount of particle packing is on the surface of microslide a;
4) use 5 μ L liquid-transfering guns that the glycerine drop is moved to microslide b surface, then microslide b is placed microscope 3 visuals field;
5) take the B of connecting link 4 end as axle, rotating probe platform 5 is so that the flatting down of probe slot 8 places; Then the three-dimensional by micromanipulator 1 control " L-type " Probe clip 2 moves, move the top to bottom, left and right, front and rear that are the AFM tipless cantilever, thereby regulate the relative position of AFM tipless cantilever micro-cantilever free end and glycerine, control moving up and down of AFM tipless cantilever micro-cantilever by micromanipulator 1 after mixing up, so that the sticking glycerine that is stained with of AFM tipless cantilever cantilever free end;
6) microslide b is removed from microscope 3 visuals field, the microslide a that the step 3) gained is loaded with the PVDF microparticle moves in the optical microscope visual field;
7) find the purpose PVDF microparticle of 8 μ m on the microslide a surface that is loaded with the PVDF microparticle, three-dimensional movement by micromanipulator 1 control " L-type " Probe clip 2 comes adjustable clamp to hold the relative position of AFM tipless cantilever micro-cantilever free end and PVDF microparticle, then adopt moving up and down of micromanipulator 1 control probe station 5, by the capillary force between the free-ended glycerine of AFM tipless cantilever micro-cantilever and the purpose PVDF microparticle purpose PVDF particle is adsorbed on the micro-cantilever free end;
8) with " I type " copper post 9 jack-up reeds 7, unclamp the screw 6 of clip, take off gained PVDF microparticle probe with tweezers, then be placed in 145 ° the constant temperature oven and leave standstill 10min, obtain PVDF microparticle probe, preparation finishes.
Gained PVDF microparticle probe as shown in Figure 3.
Embodiment 2-embodiment 5
Embodiment 2-embodiment 5 preparation processes and apparatus and process flow process be with embodiment 1, concrete preparation condition such as following table:
The above; only for the better embodiment of the present invention, but protection scope of the present invention is not limited to this, anyly is familiar with those skilled in the art in the technical scope that the present invention discloses; the variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.
Claims (7)
1. the device of the standby PVDF microparticle probe of a molten sintering legal system, it is characterized in that, comprise the micromanipulator (1) and the microscope (3) that are arranged on the basic platform, described micromanipulator (1) termination is provided with " L-type " Probe clip (2), and the camera lens of described microscope (3) is oppositely arranged with " L-type " Probe clip (2).
2. molten sintering legal system according to claim 1 is for the device of PVDF microparticle probe, it is characterized in that, described " L-type " Probe clip (2) is combined by " L-type " connecting link (4) probe station (5) that is threaded, described probe station (5) end face is provided with the probe slot (8) of placing the AFM tipless cantilever, is pressed with reed (7) on the described probe slot (8); The end of the elongated end of described reed (7), probe station (5) is provided with to prop " I type " the copper post (9) of reed (7).
3. the device of the standby PVDF microparticle probe of molten sintering legal system according to claim 1 is characterized in that described " L-type " Probe clip (2) is made by stainless steel material.
4. the method based on the standby PVDF microparticle probe of molten sintering legal system of the described device of claim 1 is characterized in that, may further comprise the steps:
1) is that 7-10 ㎝, diameter are that an end of the Al-alloy metal silk of 2mm impregnated in 12-24h in the concentrated hydrochloric acid with length, obtains the most advanced and sophisticated tinsel of 20-40 μ m that is; Then be placed in the ultrapure water ultrasonic cleaning 5-15min;
2) the AFM tipless cantilever is installed in the probe slot (8) that is arranged on the probe station (5), " L-type " Probe clip (2) is linked to each other with micromanipulator (1), have the three-dimensional of the probe station (5) of AFM tipless cantilever to move by micromanipulator (1) control clamping;
3) the PVDF particle is scattered in microslide a surface; At the lower step 1) gained most advanced and sophisticated PVDF of the dispersion particle wiry that uses of microscope (3);
4) non-PVDF solvent droplets is moved to microslide b surface, then microslide b is placed microscope (3) visual field;
5) rotating probe platform (5) so that probe slot (8) place flat down, then the three-dimensional by micromanipulator (1) control " L-type " Probe clip (2) moves, so that the AFM tipless cantilever micro-cantilever free end that is clamped in the probe slot (8) is stained with non-PVDF solvent;
6) microslide b is removed from microscope (3) visual field, the microslide a that step 3) is loaded with the PVDF microparticle moves in the optical microscope visual field;
7) the control clamping has the three-dimensional of the probe station (5) of AFM tipless cantilever to move, and purpose PVDF microparticle is adsorbed on AFM tipless cantilever micro-cantilever free end;
The AFM tipless cantilever that 8) will be loaded with the PVDF microparticle takes off from probe station (5), then is placed in the constant temperature oven and leaves standstill, and obtains PVDF microparticle probe.
5. the method for the standby PVDF microparticle probe of a kind of molten sintering legal system according to claim 4 is characterized in that described PVDF microparticle is the spheric grain of 5-20 μ m.
6. the method for the standby PVDF microparticle probe of a kind of molten sintering legal system according to claim 4 is characterized in that described non-PVDF solvent includes but not limited to the arbitrary proportion mixed liquor of deionized water, glycerine, ethanol and above-mentioned several solvents.
7. the method for the standby PVDF microparticle probe of a kind of molten sintering legal system according to claim 4 is characterized in that described constant temperature oven temperature is 112 ~ 145 ℃, and the time of repose of PVDF microparticle probe in baking oven is 10-40min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103389391A (en) * | 2013-07-23 | 2013-11-13 | 西安建筑科技大学 | Method for preparing different polymer film probes by bonding coating method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103389391A (en) * | 2013-07-23 | 2013-11-13 | 西安建筑科技大学 | Method for preparing different polymer film probes by bonding coating method |
| CN103389391B (en) * | 2013-07-23 | 2015-07-15 | 西安建筑科技大学 | Method for preparing different polymer film probes by bonding coating method |
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