CN103592211A - Porosity measuring method and device of porous material - Google Patents
Porosity measuring method and device of porous material Download PDFInfo
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- CN103592211A CN103592211A CN201310576359.9A CN201310576359A CN103592211A CN 103592211 A CN103592211 A CN 103592211A CN 201310576359 A CN201310576359 A CN 201310576359A CN 103592211 A CN103592211 A CN 103592211A
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Abstract
The invention relates to the field of porous material characterization, and particularly discloses a porosity measuring method and a device of a porous material. The porosity measuring method comprises the steps of immersing the porous material in a nonwetting solvent in a vacuum pressure vessel, recording the volume V1 of the nonwetting solvent before immersion, performing vacuum compression cycle to allow the nonwetting solvent to be squeezed into pores of the porous material and fully fill in the open pores of the porous material, recording the total volume V2 of the nonwetting solvent and the immersed porous material, removing the porous material immersed with the nonwetting solvent, recording the volume V3 of the residual nonwetting solvent, and calculating the porosity of the porous material according to a formula: the porosity (%) =[(V1-V3)/(V2-V3)]*100. According to the method and the device, a liquid displacement method is employed to measure the porosity of the porous material, the measuring method is simple, quick and convenient, the test cost and pollution are low, and the safety performance is high.
Description
Technical field
The present invention relates to porosint representational field, be specifically related to for measuring the method and apparatus of porosity of porous material.
Background technology
Porosity is the ratio (the related porosity of the application all refers to effective drainage porosity) of the cumulative volume of slight void and the appearance volume of this porous medium of being interconnected in porous medium.Porosity is the important physical that material itself has, and is used for poriness and the density of exosyndrome material, and it directly affects the physical and mechanical property of material, as strength and toughness, ventilative and water absorptivity etc.
Traditional and novel material porosity assay method has density measurement drainage, mercury injection apparatus method, scanning electron microscope sem imaging analysis, microcomputer layer scanning technology Micro-CT etc.
What density measurement drainage was measured is support overall porosity, computing formula: Porosity (%)=(1-ρ
apparent density/ ρ
density of material) * 100, ρ wherein
apparent densityweight support frame and support cumulative volume ratio, ρ
density of materialit is material intrinsic density.Density measurement drainage is simple to operate, is applicable to very much take water and is easily penetrated in material hole as non-wetting solvent, and do not cause that material expands and the support overall porosity mensuration of atrophy.
But densitometry has its limitation, while being used in particular for hydrophilic porous material porosity measurement, imbibition as easy in hydrophilic material bacteria cellulose, make the intrinsic difference of hydrophilic porous material entity volume that densitometry measures and material cumulative volume and material large, cause calculating the material porosity inaccuracy of hydrophilic material apparent density, density of material and subsequent calculations.
Mercury injection apparatus method is mainly used to measure brace aperture rate and aperture, and porosity is calculated formula: Porosity (%)=V
immerse volume/ V
support volume* 100, V wherein
immerse volumethat total mercury immersion volume is carrier openings volume of voids, V
support volumeit is support cumulative volume.Mercury injection apparatus method be take mercury as non-wetting solvent, under pressure, mercury is clamp-oned in the hole of porosint, immerses volume, by calculating brace aperture rate thereby obtain total pore size volume.
The non-wetting solvent of mercury injection apparatus method is fixed, and is also not suitable for measuring flexibly the porosity of singularity material, and mercury is also toxic heavy metal, to material and experiment people secure context, is all a kind of test.
Scanning electron microscope sem imaging and Matlab image handling implement are used for measuring and quantification sample porosity, and porosity is calculated formula: porosity (%)=(∑
void area/∑
image area) * 100." ∑ wherein
void area" be the total void area of image, " ∑
image area" be the total area of image.With scanning electron microscope sem, support is carried out to imaging, choose five images, by Matlab instrument, carry out the ratio that image is processed the total void area and the total image area that calculate image, obtain the porosity of support.
Microcomputer layer scanning technology Micro-CT measures brace aperture rate, computing formula:
wherein SV is support entity volume, and TV is support cumulative volume.Microcomputer layer scanning technology Micro-CT penetrates sample with X ray, each position by sample is different to the absorptivity of X ray, at X-ray detector, carry out non-destructive 3D imaging, in the situation that not destroying sample, represent the internal microstructure of sample.The setup parameter that Micro-CT measures support is voltage 45Kv, electric current 177 μ A, and minute 900ms, can obtain relative support volume fraction, thereby calculates the porosity of sample.
The novel technical methods such as scanning electron microscope sem imaging analysis, microcomputer layer scanning technology Micro-CT, assay method is simple and efficient, but instrument contributed capital is large, concerning medium-sized and small enterprises, cannot carry.
Hydrophilic material refers to that moistening corner is in 0 ° ≦ θ≤90 °, and between material molecule and hydrone, the power of attracting each other is greater than a class material of cohesion between hydrone.Known according to above description, due to the easy imbibition of hydrophilic porous material, cannot Measurement accuracy hydrophilic porous material porosity by conventional method.Also there is no at present the assay method for hydrophilic porous material porosity.
Summary of the invention
It is a kind of for measuring porosity of porous material that the technical problem to be solved in the present invention is to provide, especially the method for hydrophilic porous material porosity.
Technical scheme of the present invention comprises a kind of for measuring the method for porosity of porous material, comprises the following steps: in vacuum pressure container, described porosint is immersed to non wettability solvent, record the volume V of described non wettability solvent before immersion
1; Carry out vacuum compression circulation, so that described non wettability solvent is clamp-oned the hole of described porosint, and is full of the open pores of described porosint, record the cumulative volume V of the described porosint of described non wettability solvent and immersion
2; Remove the described porosint that is soaked with described non wettability solvent, record the volume V of remaining described non wettability solvent
3; According to formula: porosity (%)=[(V
1-V
3)/(V
2-V
3)] * 100, calculate the porosity of described porosint.
Described porosint can be hydrophilic porous material.Described non wettability solvent can be for being easy to infiltrate the hole of described porosint, and do not cause that described porosint expands or the solvent of atrophy, for example, be selected from ethanol, isopropyl alcohol, acetone, normal hexane, or their combination in any.
In described vacuum compression circulation, can use nitrogen or carbon dioxide, as gas-pressurized.
The mode of carrying out of described vacuum compression circulation can, for continuing respectively 5 to 20s at the vacuum pressure of 50Pa to 130Pa and the moulding pressure of 0.10MPa to 0.15MPa successively, circulate 2 to 10min.For example, can at the vacuum pressure of 50Pa and the moulding pressure of 0.10MPa, continue respectively 10s, circulation 5min successively.
It is a kind of for measuring the device of porosity of porous material that the present invention also provides on the other hand, comprising: vacuum pressure container, and it can bear the vacuum of 50Pa to 130Pa and the pressurization of 0.10MPa to 0.15MPa; Be placed in the measuring container of described vacuum pressure container; Be located on described vacuum pressure container, be with valvular vacuum interface and pressurization interface; Be connected to the vacuum pump of described vacuum interface; And the pressurized-gas source that is connected to described pressurization interface.
Vacuum tightness metering equipment can also be housed on described vacuum interface, on described pressurization interface, pressure measurement equipment can also be housed.
The present invention adopts liquid displacement technique to measure porosity of porous material, and not only assay method is simple and quick convenient, and testing cost is cheap, pollutes lowly, and security performance is high.This method is usingd the non-aqueous solvents such as ethanol, isopropyl alcohol, acetone, normal hexane as non-wetting solvent, is particularly useful for the measurement of hydrophilic porous material porosity.Solvent is not only easily penetrated in material hole, and can not cause expansion and the atrophy of material.By vacuum compression several times, circulate, force solvent to be full of the whole pore volume of material, through repeatedly duplicate measurements, can obtain accurate porosity of porous material.Measurement mechanism of the present invention is simple, can use small sterilizing pot to convert, and has reduced the cost that porosity characterizes, and is especially applicable to medium-sized and small enterprises and uses.
Accompanying drawing explanation
Fig. 1 schematically shows according to the present invention for measuring the apparatus and method of porosity of porous material.
Fig. 2, for using apparatus and method of the present invention, measures the porosity chart of bacteria cellulose film after processing with deionized water and acetic acid respectively.
Embodiment
The present invention adopts liquid displacement technique, through repeatedly vacuum compression circulation, non-wetting solvent is clamp-oned in the hole of porosint, by recording solvent volume, changes, and calculates the porosity of porosint.
Fig. 1 is measurement mechanism of the present invention and principle schematic.As seen from the figure, porosity measurement device of the present invention comprises the vacuum pressure container that can bear vacuum and pressurization, and it can be converted by small sterilizing pot.This vacuum pressure container, should be able to bear the vacuum of 50Pa to 130Pa and the pressurization of 0.10MPa to 0.15MPa, so that carry out vacuum pressed circulation.
This porosity measurement device is also included in the measuring container in this vacuum pressure container, and it is for holding the non-wetting solvent of metering; Be located on vacuum pressure container, be with valvular vacuum interface and pressurization interface; Be connected to the vacuum pump of described vacuum interface; And the pressurized-gas source that is connected to described pressurization interface, as gas cylinder.Gas-pressurized can be nitrogen, carbon dioxide etc.By vacuum pump, vacuumizing and open pressurization valve realizes vacuum compression and circulates.Measuring container records the volume change of non-wetting solvent.
Meticulous adjustable in order to make to operate, vacuum tightness metering equipment can also be housed on vacuum interface, as vacuum meter, on described pressurization interface, pressure measurement equipment is also housed, as tensimeter.
When using ethanol as non-wetting solvent, measuring method specifically can be as follows: first initial volume V will be housed
1the measuring graduates of ethanol is put into container, and porosint (for example, can be hydrophilic material) is immersed in the ethanolic solution of measuring graduates, closes vacuum pressure container.Open the vacuum compression circulation system, according to the hydrophilic hydrophobic property of porosint in practice, concrete non-wetting solvent of use etc., can select at the vacuum pressure of 50Pa to 130Pa and the moulding pressure of 0.10MPa to 0.15MPa, to continue respectively 5 to 20s successively, circulate 2 to 10min.For example, can, when using ethanol as non-wetting solvent, at the vacuum pressure of 50Pa and the moulding pressure of 0.10MPa, continue respectively 10s, circulation 5min successively.This time is enough to force ethanol to be clamp-oned in the hole of porosint, and is full of porosint open pores.
After vacuum compression circulation finishes, open immediately vacuum pressure container, record ethanol and the cumulative volume V that immerses porosint in graduated cylinder
2.Then remove the porosint that is soaked with ethanolic solution, record and in graduated cylinder, remain ethanol volume V
3.
Porosint volume of voids is V
1-V
3, porosint cumulative volume is V
2-V
3, according to following formula, can obtain the porosity of porosint: porosity (%)=[(V
1-V
3)/(V
2-V
3)] * 100.
The present invention uses the replaceable non-wetting solvent of non-water, for being penetrated into material hole, can measure the porosity of different materials.Particularly, according to the concrete property of porosint, the hydrophilic and hydrophobic intensity in its hole there are differences, and correspondingly selects suitable non wettability solvent, guarantees that solvent is easily penetrated in material hole, does not cause that again material expands or atrophy.For example, non-wetting solvent can be ethanol, isopropyl alcohol, acetone, normal hexane etc.Wherein, ethanol is the non-wetting solvent that is suitable as very much hydrophilic material.
Use repeatedly vacuum compression circulation, can force non-wetting solvent rapid osmotic in material hole, and complete and be full of, guaranteed to measure the degree of accuracy of material porosity.Pressurized cylinder in the present invention in vacuum compression system used also can be selected suitable gas pressurization by material requirements, guarantees that material immerses non-wetting solvent and do not affect again material shape simultaneously.
Porosity of porous material determinator of the present invention can adopt small sterilizing pot to convert, and be equipped with tensimeter, vacuum meter, force pipe, vacuum tube, operation valve, measuring graduates, vacuum pump, nitrogen cylinder etc., with low cost, be particularly suitable for medium-sized and small enterprises and use.
Mesoporosity of the present invention rate assay method and device, simple to operate, consuming time short, with low cost and safety non-pollution.Compare with current material porosity measurement method, be not subject to the restriction of material self character (water wettability, hydrophobicity), range of applicability is wide.Especially the porosity measurement technology to hydrophilic porous material that provides prior art to realize.For the feature of hydrophilic porous material high-hydroscopicity, selecting ethanol is non-wetting solvent, at vacuum compression cycling condition, makes ethanol in hydrophilic porous material hole, to realize and being full of completely, and does not cause that material expands and atrophy.And only to limit to mercury unlike mercury injection apparatus method be non wettability solvent, method of the present invention is nontoxic, and security protection requires low.
Below in conjunction with specific embodiment, the present invention is described in further detail.
raw material
Bacteria cellulose, the accessory substance that acetobacter xylinum fermentation produces, laboratory preparation;
Regenerated silk albumen, mulberry silk extracts and obtains, laboratory preparation;
Hydroxyapatite, aldrich chemical company;
PLA, Boehringer Ingelheim company;
Ethanol: analyze pure, Shanghai Ling Feng chemical reagent company limited;
Normal hexane: analyze pure, Shanghai Ling Feng chemical reagent company limited.
embodiment 1-bacteria cellulose film porosity measurement
Deionized water is processed bacteria cellulose: by 2.5cm
2bacteria cellulose film piece soaks 12h in 50mL deionized water.
1% acetic acid is processed bacteria cellulose: by 2.5cm
2bacteria cellulose film piece soaks 12h in 50mL1% acetum.
Freeze-dried bacteria cellulose: the bacteria cellulose soaking is taken out, be placed on-80 ℃ of pre-freeze 4h, then at-76 ℃, vacuum pressure is dry 48h in the freeze drier of 10Pa, obtains dry bacteria cellulose film.
Porosity measurement: first pack the ethanol of 50mL in the graduated cylinder in vacuum pressure container into, will be immersed in ethanol respectively through deionized water and the acid-treated bacteria cellulose film of 1% vinegar piece.The circulation of unlatching vacuum compression, wherein vacuum pressure is that 50Pa continues 10 seconds, moulding pressure is that 0.10MPa continues 10 seconds, circulates approximately 5 minutes, ethanol is clamp-oned in the hole of bacteria cellulose, and be full of open pores.After vacuum compression circulation finishes, open vacuum pressure container, the cumulative volume that records the bacteria cellulose of ethanol in graduated cylinder and immersion is respectively 57.8mL and 53.8mL.Remove the bacteria cellulose that is soaked with ethanol, record remaining ethanol volume in graduated cylinder and be respectively 42.1mL and 37.6mL.
According to formula: porosity (%)=[(V
1-V
3)/(V
2-V
3)] * 100, the porosity that calculates the bacteria cellulose of processing through deionized water is 50.32%; Porosity through the acid-treated bacteria cellulose of 1% vinegar is 76.54%.
Fig. 2 illustrates the porosity comparison diagram of two kinds of treated bacteria celluloses.These data can be used to proof and process by acetic acid the porosity that the method combining with freeze drying has been improved porosint.
embodiment 2-regenerated silk albumen porosity measurement
By regenerated silk albumen, make three-dimensional rack: first, teflon right cylinder is dipped in 5.8% (w/v) regenerated silk protein aqueous solution to 5 to 6min, add 15% methanol solution, form regenerated silk protein gel, regenerated silk protein gel is placed on to-80 ℃ of pre-freeze 4h, then at-76 ℃, vacuum pressure is dry 48h in the freeze drier of 10Pa, and freeze drying obtains the three-dimensional rack of regenerated silk albumen.
Porosity measurement: first pack the normal hexane of 50mL in the graduated cylinder in vacuum pressure container into, the three-dimensional rack of regenerated silk albumen is immersed in normal hexane.The circulation of unlatching vacuum compression, wherein vacuum pressure is that 50Pa continues 10 seconds, moulding pressure is that 0.10MPa continues 10 seconds, circulates approximately 5 minutes, normal hexane is clamp-oned in the hole of three-dimensional rack, and be full of open pores.After vacuum compression circulation finishes, open vacuum pressure container, record the cumulative volume 50.3mL of the three-dimensional rack of normal hexane in graduated cylinder and immersion.Remove the support that is soaked with normal hexane, record remaining normal hexane volume 23.3mL in graduated cylinder.
According to formula: porosity (%)=[(V
1-V
3)/(V
2-V
3)] * 100, the porosity that calculates the three-dimensional rack being made by regenerated silk albumen is about 99%.
In this embodiment, use normal hexane as non-wetting solvent, record that timbering material porosity is accurate and the running time is short.
embodiment 3-hydroxyapatite-lactic acid composite material porosity measurement
The making of compound substance: polylactic acid-glycolic base apatite-dioxy cyclohexane mixed liquor of getting 10mL joins in the beaker of 30mL, is preheating to 50 ℃.In refrigerator, make the solvent in mixed liquor solidify 2h the beaker fast transfer that mixed solution is housed, lure Solid-Liquid Separation into.Then with liquid nitrogen, impel solidified sample deep freezing, freeze sample freeze drying 4 days under 0.5mmHg condition, obtain hydroxyapatite-lactic acid composite material.
Porosity measurement: first pack the ethanol of 50mL in the graduated cylinder in vacuum pressure container into, hydroxyapatite-lactic acid composite material is immersed in ethanol.The circulation of unlatching vacuum compression, wherein vacuum pressure is that 50Pa continues 10 seconds, moulding pressure is that 0.10MPa continues 10 seconds, circulates approximately 5 minutes, ethanol is clamp-oned in the hole of compound substance, and be full of open pores.After vacuum compression circulation finishes, open vacuum pressure container, record the cumulative volume 51.2mL of the compound substance of ethanol in graduated cylinder and immersion.Remove the compound substance that is soaked with ethanol, record remaining ethanol volume 27.2mL in graduated cylinder.
According to formula: porosity (%)=[(V
1-V
3)/(V
2-V
3)] * 100, the porosity that calculates hydroxyapatite-lactic acid composite material is 95%.
Hydrophobic characteristics due to polymkeric substance, hydrosolvent is difficult to be penetrated in compound substance hole, with ethanol as non wettability solvent, not only easily be penetrated in the hole of compound substance, and hydroxyapatite and lactic acid composite material do not expand and atrophy, by liquid displacement technique porosity measurement device of the present invention, the simple and efficient porosity that obtains accurately compound substance.
Porosity measurement method of the present invention dirigibility is high, and contributed capital is few, and the existence of the vacuum compression circulation system can be permeated non-wetting solvent completely and is full of material open pores, thereby obtains the accurate porosity of material.
The above the specific embodiment of the present invention, does not form limiting the scope of the present invention.Various other corresponding changes and distortion that any technical conceive according to the present invention has been done, all should be included in the protection domain of the claims in the present invention.
Claims (9)
1. for measuring a method for porosity of porous material, it is characterized in that, comprise the following steps:
In vacuum pressure container, described porosint is immersed to non wettability solvent, record the volume V of described non wettability solvent before immersion
1;
Carry out vacuum compression circulation, so that described non wettability solvent is clamp-oned the hole of described porosint, and is full of the open pores of described porosint, record the cumulative volume V of the described porosint of described non wettability solvent and immersion
2;
Remove the described porosint that is soaked with described non wettability solvent, record the volume V of remaining described non wettability solvent
3;
According to formula: porosity (%)=[(V
1-V
3)/(V
2-V
3)] * 100, calculate the porosity of described porosint.
2. the method for claim 1, wherein described porosint is hydrophilic porous material.
3. the method for claim 1, wherein described non wettability solvent is the hole that is easy to infiltrate described porosint, and does not cause that described porosint expands or the solvent of atrophy.
4. method as claimed in claim 3, wherein, described non wettability solvent is selected from ethanol, isopropyl alcohol, acetone, normal hexane, or their combination in any.
5. the method for claim 1, wherein in described vacuum compression circulation, use nitrogen or carbon dioxide, as gas-pressurized.
6. the method for claim 1, wherein the mode of carrying out of described vacuum compression circulation, for continuing 5 to 20s respectively at the vacuum pressure of 50Pa to 130Pa and the moulding pressure of 0.10MPa to 0.15MPa successively, circulates 2 to 10min.
7. method as claimed in claim 6, wherein, the mode of carrying out of described vacuum compression circulation is for continuing respectively 10s, circulation 5min at the vacuum pressure of 50Pa and the moulding pressure of 0.10MPa successively.
8. for measuring a device for porosity of porous material, it is characterized in that, described device comprises:
Vacuum pressure container, it can bear the vacuum of 50Pa to 130Pa and the pressurization of 0.10MPa to 0.15MPa;
Be placed in the measuring container of described vacuum pressure container;
Be located on described vacuum pressure container, be with valvular vacuum interface and pressurization interface;
Be connected to the vacuum pump of described vacuum interface; And
Be connected to the pressurized-gas source of described pressurization interface.
9. device as claimed in claim 8, wherein, is also equipped with vacuum tightness metering equipment on described vacuum interface, on described pressurization interface, pressure measurement equipment is also housed.
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