CN102183446B - Device and method for measuring sizes of flexible pores on basis of capillary pressure and viscous force grading - Google Patents
Device and method for measuring sizes of flexible pores on basis of capillary pressure and viscous force grading Download PDFInfo
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- CN102183446B CN102183446B CN201110054849.3A CN201110054849A CN102183446B CN 102183446 B CN102183446 B CN 102183446B CN 201110054849 A CN201110054849 A CN 201110054849A CN 102183446 B CN102183446 B CN 102183446B
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Abstract
The invention relates to a device and a method for horizontally measuring sizes and distribution of capillary pores on the basis of capillary pressure and viscous force grading and along the plane of a flexible sample. By the device and the method, deformation and size distortion of a flexible material caused by pressurizing and vacuumizing are avoided; and the defect that sizes of nano-grade pores are difficult to measure by a vertical mass grading method is overcome. An equation is established according to a capillary pressure and viscous force balance principle; a method for performing subtraction on liquid content of the adjacent fractions during osmotic balance of the liquid to the flexible sample is provided; corresponding aperture data is acquired according to a fraction liquid-containing formula and an aperture equation provided by the inventor. The test device is designed and comprises a sample-clamping and tension-adjusting mechanism, a free section inclined angle adjusting mechanism and a multi-head parallel cutting device. A residual liquid collecting and calculating method is adopted, so that measuring precision and reproducibility are improved. The method and the device are simple in operation, high in precision and high in data reproducibility. By the method and the device, practicability is achieved; and nano dimension aperture distribution of the flexible material can be quantitatively measured.
Description
Technical field
The present invention relates to a kind of determinator and method of flexible capillary pore diameter distribution.
Background technology
The microcellular structure of flexible material has significant impact to its performance.Particularly the pore structure of fabric is all vital for its wet processing and hot wet migration.As the pore aggregate of both ends open, partial order, the wetting state of fabric usually and its pore distribute closely related, because no matter be wet process or take in process, transporting of moisture, organic solvent and sweat is all mainly carried out in pore, and the processes such as the absorption wherein related to, diffusion, infiltration, evaporation all depend on the structure (shape, roughness, size, distribution etc.) of pore.In view of the complicacy of fabric construction, the method measuring wetting property of the fabric is for a long time mostly compared with the tolerance on pore more large scale, mainly comprise: capillary wicking method, sessile drop method, sedimentation etc., due to could not with the capillary structure direct correlation of fabric, constrain the essence of further investigation fabric wetting behavior and further quantification measures and accurate control to each process above-mentioned.Applicant has declared the patent of invention (application number: 200910194353.9), but also do not see the relevant report utilizing liquid capillary pressure and viscous force to carry out fractionation testing flexibility capillary pore diameter distribution so far of the pore diameter distribution method of testing along textile plane based on quality grading method early stage.Quality grading method, due to the limitation of vertical gravity effect, is difficult to manifest to the grading of liquid in small hole, can only measures the aperture of tens microns of-millimeter of magnitudes.And the driving force of Horizontal capillary infiltration depends primarily on the competition between viscous force and capillary pressure, the motion state difference of liquid in the formula that applicant derives and the hole that method of testing can disclose nanometer level, and then can according to the hole dimension of correlation parameter measurement and calculation nanoscale and distribution.These data and the complementation of quality grading method pore size distribution data, can contain the size distribution data of nano-micrometre-millimeter, more fully can react the microcellular structure of flexible material.
Summary of the invention
The object of the invention is for above-mentioned the deficiencies in the prior art, there is provided a kind of capillary pressure-viscous force grading method that adopts to the measurements and calculations method of flexible capillary pore diameter distribution, the present invention can measure the distribution of nanoscale along print plane capillary aperture, and by governing stage partial width flexible modulation test specification and precision, solve the deficiency that quality grading method can not measure nanometer range pore diameter distribution.
The present invention is achieved through the following technical solutions:
Relate to a kind of device measured in the horizontal direction along flexible print plane capillary dimensions and distribution based on capillary pressure and viscous force grading, comprising: print horizontally suspends the little bar cutter sweep of frame mounting, dailies roll winding apparatus, liquid tank, timer and statistics fraction.By liquid when horizontal print wettability equilibrium, along cutting into the little bar of some fractions for statistical treatment perpendicular to liquid working direction print wetted portions, measuring its liquid content and calculating corresponding pore size distribution data and chart.
Described print horizontally suspends rectangular frame device and carries out horizontal wicking for hanging rectangle print, this device is made up of two horizontal bar clevis plates and multiple connection adjuster bar, clamping plate clamp print main body from both sides along its length, the free segment that fraction does not clamp is left in print front end, and adjuster bar can the lateral adjustments clamping plate spacing tension force that makes print reach suitable.
Described dailies roll winding apparatus immerses the free segment of liquid for clamping print and regulates its tension force by winding.By a pair, the vertical and turning axle of the back up pad and a fastening print that are fixed on base plate forms this device, and this axle is through two plates, and there are turning handle and self-locking mechanism in its one end, regulates print free segment tension force and fixing print by rotational fastener axle.
Described liquid tank is for filling the wetting liquid of test and collecting device being put into bottom land, and liquid level wants the fastening turning axle of submergence collecting device.Trench bottom is equipped with multiple adjusting screw, for regulating height and keeping liquid level.Make to stretch out free segment print that liquid bath is connected with clamping plate keep suitable tight state and from the horizontal by 1-10 degree inclination angle by highly regulating.Print tension force with center section after free segment dampening liquid do not produce subside sagging for foundation; Angular adjustment is to little as far as possible, and to keep close to horizontal state to eliminate gravity shadow, free segment edge must not contact groove edge for principle as far as possible.
Described fraction little bar cutter sweep is used for the simultaneously little bar of accurate parallel cutting many fractions, eliminates the long content liquid caused due to Liquid Penetrant of shear time as far as possible and changes at print each several part, and then eliminate Measurement and Computation error;
The liquid that cutter sticks must calculate in fraction liquid content when cutting by described fraction little bar in the lump;
The present invention relates to the method for a kind of measurements and calculations in the horizontal direction based on capillary pressure and viscous force grading along flexible print plane capillary dimensions and distribution, comprise the following steps:
Step one, carries out pre-treatment to print, removing surface contaminants;
Step 2, it is constant that experimentation controls humiture;
Step 3, by long 0.5-2m, the print bar shaped clamping plate clamping of wide 0.05-0.5m, front end reserves the free segment of certain length for reeling and being placed in bottom land, regulate lateral separation between clamping plate with adjuster bar, print is suitably tightened, do not sink for limit with wetting rear center section;
Step 4, regulates liquid groove height, makes print free segment and horizontal sextant angle little as far as possible, but can not contact trough rim;
Step 5, adds wetting liquid, makes it the axle flooding winding stand, starts timing simultaneously, the distance of record different time liquid front linear distance liquid level, until liquid no longer obviously advances, now the time is as the time-parameters substituted in the formula of calculated hole diameters distribution;
Step 6, with fraction little bar cutter sweep along wets part being cut into the little fillet of multiple rectangle perpendicular to Liquid Penetrant direction simultaneously, little bar width is D
i, count from print metal line, the seepage distance H of each little bar
1, H
2, H
3... H
nbe corresponding in turn to as D
1, D
1+ D
2, D
1+ D
2+ D
3... D
1+ D
2+ D
3+ ... + D
n;
Step 7, weighs up the weight in wet base of each wet little bar, weighs up its dry weight respectively again, deduct by weight in wet base the liquid content G that dry weight obtains the little bar of each fraction after drying
i;
Step 8, according to step 5, six, seven data obtained, the data of proposition calculate and disposal route, it is characterized in that:
A. adjacent front little bar is deducted with the little bar in rear successively along infiltration direction
Liquid content G
i-G
i+1obtain the liquid content in distance respective radius residing for the little bar in rear (being obtained by formulae discovery below) hole, the formula X utilizing applicant to derive
i=∑ G
i/ G
1-G
nwhat calculate each little bar contains liquid number percent X
i, i.e. the frequency of this statistics fraction is also respective radius r
ithe percent by volume in hole;
B. the derivation of inventor to computing formula is as follows
Washburn equation according to laminar fluid permeates in pore:
H
2＝Kt (1)
In formula: H-seepage distance, t-time of penetration,
Wherein:
K＝rγcos θ/2η (2)
In formula:
R-fabric average pore size;
The interfacial tension of γ-liquid-gas;
θ-fabric and test fluid contact angle;
η-test fluid viscosity;
Transposition obtains:
K＝H
2/t (3)
Substitute into each parameter, obtain orifice size calculation formula
r＝2ηH
2/tγcosθ (4)
From formula (4), for t same observing time, capillary radius r is larger, seepage distance H is far away wherein for liquid, so liquid exists only in comparatively in macropore in adjacent two fraction middle distance fraction far away, in nearlyer fraction, liquid had then both been contained in and had comparatively also been contained in macropore slightly in aperture, the liquid that the liquid of nearlyer fraction deducts fraction far away just to obtain in nearlyer fraction, compared with the amount of liquid in aperture, correspond to the volume in this hole be proportional.Because different pore size pore is equally distributed vertically, so carry out adjacent fraction liquid content difference successively to subtract the volume and percent by volume that just can obtain distance correspondingly-sized hole residing for each fraction.
C. when permeating close to balance, namely liquid front no longer changed in section in observing time, was decided to be the time t measuring pore diameter distribution the wherein the shortest time
m, cut rapidly simultaneously, will fix along print axis liquid gradient, then each cutting fraction little bar center line is decided to be H from the distance of liquid level
i, calculate corresponding each seepage distance H by (4) formula
ifraction aperture r
i,
A. the X of the little bar of corresponding each fraction
iand r
idraw pore diameter distribution histogram, curve map and cumulative chart.
Compared with prior art, owing to not needing pressurization or vacuumizing the present invention, there is the distortionless feature of maintenance flexible material pore structure, also there is the feature that measurement size is little, nanoscale capillary aperture and distribution can be measured, device is simple, method is easy to operate, and complementary with quality grading method, the difficult problem that long-standing problem flexible material pore diameter distribution measures can be solved, namely pressurize or vacuumize the difficult problem making flexible hole metamorphopsic distortion.
Accompanying drawing illustrates:
Fig. 1 is apparatus of the present invention structural representations;
Fig. 2 is the test result of the embodiment of the present invention: 150D × 530D × 564 × 264/72F twill polyamide fibre pore diameter distribution histogram;
Fig. 3 is the test result of the embodiment of the present invention: 150D × 530D × 564 × 264/72F twill polyamide fibre pore diameter distribution histogram;
Fig. 4 is the test result of the embodiment of the present invention: 150D × 530D × 564 × 264/72F twill polyamide fibre pore diameter distribution cumulative chart.
Embodiment
Elaborate to embodiments of the invention below, the present embodiment is implemented under technical solution of the present invention prerequisite, gives detailed embodiment and concrete operating process, but the embodiment that protection scope of the present invention does not limit what following.
The present invention proposes determinator and the method for a kind of flexible capillary pore diameter distribution of a kind of quality grading method complementation, mainly according in material capillary hole liquid capillary pressure drive and viscous force retardation opening relationships formula and related device and method are proposed.
As shown in Figure 1, the present embodiment relates to a kind of device measured in the horizontal direction along flexible print plane capillary dimensions and distribution based on capillary pressure and viscous force grading, comprising: print horizontally suspends the little bar cutter sweep of frame mounting, dailies roll winding apparatus, liquid tank, timer and statistics fraction.By liquid when horizontal print wettability equilibrium, along cutting into the little bar of some fractions perpendicular to liquid working direction print wetted portions, measuring its liquid content and calculating corresponding pore size distribution data and chart.
Described print horizontally suspends rectangular frame device, horizontal wicking is carried out for hanging rectangle print, this device is by two wide 1cm, 6 horizontal bar clevis plates of thickness 1.5cm, long 15cm and 6 connection adjuster bar compositions equidistantly placed, print is 150D × 530D × 564 × 264/72F twill polyamide fibre, wide 10cm, long 100cm, the long print main body of 90cm clamped along its length by clamping plate from both sides, the long free segment of 10cm is left in front end.Six adjuster bars are fixed on bottom two clamping plate, divide equally distance along its length to place from two ends, each bar two ends are along left-hand thread screw mandrel, connect corresponding both sides clamping plate respectively, make clamping plate keeping parallelism, screw mandrel using nuts regulates clamping plate laterally apart from the tension force making print reach suitable, not sink to being as the criterion in the middle of print time wetting.
Described dailies roll winding apparatus, immerses the free segment of liquid for clamping print and regulates its tension force by winding.This device is made up of the turning axle of the back up pad and a fastening print that are fixed on base plate side by side a pair, this axle is through two plates, its one end has turning handle and self-locking mechanism for fixing print and regulates print free segment tension force by rotational fastener axle, and to soak, print center section is not sagging is afterwards as the criterion its size.Because collecting device is fixed in trough floor, along with groove is elevated the level inclination of adjustable free segment.
Described liquid tank, for filling the wetting liquid of test and collecting device being put into bottom land, liquid level wants the fastening turning axle of submergence collecting device.Trench bottom is equipped with multiple adjusting screw, for regulating height and keeping liquid level.Make to stretch out free segment print that liquid bath is connected with clamping plate keep suitable tight state and from the horizontal by 8 degree of inclination angles by highly regulating.Now after free segment print dampening liquid, center section does not produce and subsides sagging, and free segment edge must not contact groove edge;
The little bar cutter sweep of described fraction is combination bull parallel shears, 7 the little bars of fraction of accurate parallel cutting simultaneously can be used for by clip simultaneously, eliminate the long content liquid caused due to Liquid Penetrant of shear time to change at print each several part as far as possible, and then eliminate Measurement and Computation error;
The little bar cutter sweep of described fraction is furnished with imbibition paper handkerchief, the draws fluid that cutter sticks also must be weighed in the lump and is calculated in fraction liquid content during cutting;
Based on the measurements and calculations in the horizontal direction of capillary pressure and viscous force grading along a method for flexible print plane capillary dimensions and distribution, it is characterized in that, comprise the following steps:
Step one, carries out pre-treatment to print, removing surface contaminants;
Step 2, it is constant that experimentation controls humiture;
Step 3, by long 0.5-2m, the print bar shaped clamping plate clamping of wide 0.05-0.5m, front end reserves the free segment of certain length for reeling and being placed in bottom land, and regulate lateral separation between clamping plate with adjuster bar, print is suitably tightened, and center section does not sink after wetting;
Step 4, regulates liquid groove height, makes print free segment and horizontal sextant angle 3-8 degree, but can not contact trough rim;
Step 5, adds distilled water, makes it the axle flooding winding stand, starts timing simultaneously, and the distance of record different time distilled water frontal line distance liquid level, until liquid no longer obviously advances;
Step 6, wets part is cut into the little fillet of multiple rectangle along perpendicular to distilled water infiltration direction by rapid fraction little bar cutter sweep simultaneously, and little bar width is 2.5cm, counts from print metal line, the seepage distance H of each little bar
1, H
2, H
3... H
nbe corresponding in turn to as 2.5cm, 5.0cm, 7.5cm,
Step 7, weighs up the weight in wet base of each wet little bar, weighs up its dry weight respectively again, deduct by weight in wet base the liquid content G that dry weight obtains the little bar of each fraction after drying
i;
Step 8, according to step 5, six, seven data obtained, the data of proposition calculate and disposal route, it is characterized in that:
B. adjacent front little bar is deducted with the little bar in rear successively along infiltration direction
Liquid content G
i-G
i+1obtain the liquid content in distance respective radius hole residing for the little bar in rear, the formula X utilizing applicant to derive
i=∑ G
i/ (G
1-G
n) calculate each little bar containing liquid number percent X
i, i.e. the frequency of this statistics fraction is also the percent by volume in correspondingly-sized hole;
C. by Washiburn equation, H
2=Kt can calculate equilibration time t and corresponding each seepage distance H
ipermeability K
i, be also namely positioned at H
ithe little bar radius R of distance fraction
ihole in the infiltration rate constant K of capillary liquid
i;
D. according to the formula K derived
i=R
iγ cos θ/2 η (wherein R
ifor pore radius, γ is surface tension of liquid, and θ is contact angle, and η is liquid viscosity) calculate distance for H
ipore radius R corresponding to the little bar of each fraction
i;
D. the X of the little bar of corresponding each fraction
ipore diameter distribution histogram, curve map and cumulative chart is drawn with R;
Experimental data is as follows
The average pore size scope of 150D × 530D × 564 × 264/72F twill polyamide fibre cloth specimen is 0.83-75.62nm.
This enforcement only gives the example of an embody rule, but for the patent personnel being engaged in flexible material Estimation of Pore Size, also can design the modified product of various ways according to above enlightenment, this is still considered to be covered by among the present invention.
Claims (4)
1. the device measured in the horizontal direction along flexible print plane capillary dimensions and distribution based on capillary pressure and viscous force grading, comprise: print horizontally suspends the little bar cutter sweep of frame mounting, dailies roll winding apparatus, liquid tank, timer and fraction, by liquid when horizontal print wettability equilibrium, along cutting into rapidly the little bar of some fractions perpendicular to liquid working direction print wetted portions, measuring its liquid content and being subtracted and formula r by adjacent level divided data difference
i=2 η H
i 2/ t
mγ cos θ, in formula, γ is surface tension of liquid, and θ is contact angle, and η is liquid viscosity, by different time t
mliquid Penetrant distance H
i, calculate corresponding pore size distribution data and chart further;
Print horizontally suspends rectangular frame device and carries out horizontal wicking for hanging rectangle print, this device is made up of two horizontal bar clevis plates and multiple connection adjuster bar, clamping plate clamp print main body from both sides along its length, the free segment that fraction does not clamp is left in print front end, and adjuster bar can the lateral adjustments clamping plate spacing tension force that makes print reach suitable;
Dailies roll winding apparatus immerses the free segment of liquid for clamping print and regulates its tension force by winding, by a pair, the vertical and turning axle of the back up pad and a fastening print that are fixed on base plate forms this device, this axle is through two plates, there are turning handle and self-locking mechanism in its one end, regulates print free segment tension force and fixing print by rotational fastener axle;
Liquid tank is for filling the wetting liquid of test and collecting device being put into bottom land, and liquid level wants the rotational fastener axle of submergence collecting device; Trench bottom is equipped with multiple adjusting screw, for regulating height and keeping liquid level, make to stretch out free segment print that liquid bath is connected with clamping plate keep suitable tight state and from the horizontal by inclination angle little as far as possible by highly regulating, not producing with center section after free segment print dampening liquid subsides sagging for foundation, is generally 1-10 degree.Free segment edge must not contact groove edge.
2. according to device according to claim 1, it is characterized in that, described fraction little bar cutter sweep is used for the simultaneously little bar of accurate parallel cutting many fractions, eliminates the long content liquid caused due to Liquid Penetrant of shear time as far as possible and changes at print each several part, and then eliminate Measurement and Computation error.
3. device according to claim 1, is characterized in that, the liquid that cutter sticks must be calculated in the lump in fraction liquid content when the little bar of described fraction cuts.
4. adopt the method measuring the device along flexible print plane capillary dimensions and distribution in the horizontal direction based on capillary pressure and viscous force grading according to claim 1, it is characterized in that, comprise the following steps:
Step one, carries out pre-treatment to print, removing surface contaminants;
Step 2, it is constant that experimentation controls humiture;
Step 3, by long 0.5-2m, the print of wide 0.05-0.5m is fixed on print and horizontally suspends frame mounting, front end reserves the free segment of certain length for reeling and being placed in bottom land, regulate dailies roll winding apparatus, print is suitably tightened, and center section does not sink after wetting;
Step 4, regulates liquid groove height, makes print free segment and horizontal sextant angle little as far as possible, but can not contact trough rim;
Step 5, adds wetting liquid, makes it the axle flooding collecting device, starts timing simultaneously, and the distance of record different time liquid front linear distance liquid level, until liquid no longer obviously advances;
Step 6, rapid fraction little bar cutter sweep is simultaneously along cutting into the little fillet of multiple rectangle perpendicular to Liquid Penetrant direction by wets part, and little bar width is D
i, count from print metal line, the seepage distance H of each little bar
1, H
2, H
3... H
nbe corresponding in turn to as D
1, D
1+ D
2, D
1+ D
2+ D
3... D
1+ D
2+ D
3+ ... + D
n;
Step 7, weigh up the weight in wet base of each wet little bar, wherein weight in wet base comprises the residual liquid that cutter sticks, and weighs up its dry weight respectively again after drying, deducts by weight in wet base the liquid content G that dry weight obtains the little bar of each fraction
i;
Step 8, according to step 5, six, seven data obtained, calculates radius and percent by volume that the little bar of each fraction includes liquid pore, it is characterized in that:
A. deduct the liquid content G of the little bar in adjacent front successively with the little bar in rear along infiltration direction
i-G
i+1obtain the liquid content in distance respective radius hole residing for the little bar in rear, because containing than more liquid in the little bar in next-door neighbour front in the little bar in rear, have more liquid in part i.e. corresponding aperture, this position pore, in hole, contained liquid equals pore volume and tintometric product, utilizes formula X
i=∑ G
i/ (G
1-G
n) calculate each little bar containing liquid number percent X
i, i.e. the frequency of this statistics fraction is also the percent by volume in correspondingly-sized hole;
By Washiburn equation, H
2=Kt=(r γ cos θ/2 η) t, from testing the H obtained
2liquid Penetrant distance H no longer time dependent flex point place equilibration time t is found out in-t corresponding diagram
m, substitute into above formula and calculate corresponding each seepage distance H
ithe little cylindrical void of fraction in liquid at t
mthe permeability K in moment
i,
By K
isubstitute into following formula:
r
i＝2ηH
i 2/t
mγcosθ
Obtain being in different distance H
ithe little bar of fraction includes the radius r of liquid pore
i, in formula, γ is surface tension of liquid, and θ is contact angle, and η is liquid viscosity;
B. the X of the little bar pore of corresponding each fraction
iand r
idraw pore diameter distribution histogram, curve map and cumulative chart.
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|---|---|---|---|
| CN201110054849.3A CN102183446B (en) | 2011-03-08 | 2011-03-08 | Device and method for measuring sizes of flexible pores on basis of capillary pressure and viscous force grading |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110054849.3A CN102183446B (en) | 2011-03-08 | 2011-03-08 | Device and method for measuring sizes of flexible pores on basis of capillary pressure and viscous force grading |
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| CN102183446B true CN102183446B (en) | 2015-02-25 |
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| JP2002048694A (en) * | 2000-08-01 | 2002-02-15 | Sekisui Chem Co Ltd | Test method for water permeability of constructional material |
| CN101216410A (en) * | 2008-01-11 | 2008-07-09 | 东华大学 | Testing device and method for simulating skin water vapour permeability |
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-
2011
- 2011-03-08 CN CN201110054849.3A patent/CN102183446B/en not_active Expired - Fee Related
Patent Citations (4)
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|---|---|---|---|---|
| US5425265A (en) * | 1993-12-20 | 1995-06-20 | Jaisinghani; Rajan A. | Apparatus and method for measuring the capillary pressure distribution of porous materials |
| JP2002048694A (en) * | 2000-08-01 | 2002-02-15 | Sekisui Chem Co Ltd | Test method for water permeability of constructional material |
| CN101216410A (en) * | 2008-01-11 | 2008-07-09 | 东华大学 | Testing device and method for simulating skin water vapour permeability |
| CN101738359A (en) * | 2009-11-25 | 2010-06-16 | 五邑大学 | Method for determining capillary radius distribution of flexible porous system by mass classification |
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| Title |
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| 基于质量分级法的织物毛细孔径分布测定方法;齐宏进 等;《纺织学报》;20100131;第31卷(第1期);48-52 * |
| 王其 等.有孔隙的纤维、纱线和织物导湿结构模型研究.《东华大学学报(自然科学版)》.2002,第28卷(第4期),68-71. * |
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