CN100554933C - Reach thickness direction permeability proving installation and saturated permeability method of testing in the fiber lay down aspect - Google Patents

Reach thickness direction permeability proving installation and saturated permeability method of testing in the fiber lay down aspect Download PDF

Info

Publication number
CN100554933C
CN100554933C CNB2007100991606A CN200710099160A CN100554933C CN 100554933 C CN100554933 C CN 100554933C CN B2007100991606 A CNB2007100991606 A CN B2007100991606A CN 200710099160 A CN200710099160 A CN 200710099160A CN 100554933 C CN100554933 C CN 100554933C
Authority
CN
China
Prior art keywords
fiber
permeability
plate
lay down
layer
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CNB2007100991606A
Other languages
Chinese (zh)
Other versions
CN101051019A (en
Inventor
张佐光
李敏
顾轶卓
张大兴
孙志杰
李艳霞
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Beihang University
Original Assignee
Beihang University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Beihang University filed Critical Beihang University
Priority to CNB2007100991606A priority Critical patent/CN100554933C/en
Publication of CN101051019A publication Critical patent/CN101051019A/en
Application granted granted Critical
Publication of CN100554933C publication Critical patent/CN100554933C/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Abstract

The invention discloses and a kind ofly be applied to continuous fiber in the polymer matrix composites and strengthen the body proving installation of permeability and method of testing of saturated permeability thereof in roofing and on the thickness direction, overlap the permeability testing mould by having designed one, thereby realized the preparation of sample and the mensuration of interior direction of fiber lay down aspect and thickness direction saturated permeability.This method at first is laid in the fabric of prepreg or dry state in the testing mould, the network structure of fiber lay down layer is fixed up on four limits of spreader plate and die cavity about utilizing, re-use solvent the resin in the prepreg is removed, solved the problem that unidirectional pre-immersion material is difficult for sample preparation; By pressurized equipment the fiber lay down layer is exerted pressure, change its fiber volume fraction; Various annexes are installed on testing mould then,, are comprised the flow channel of direction in the fiber lay down aspect and the flow channel of thickness direction to form different flow channels; Under the effect of air pressure, low viscous liquid is injected in the testing mould, it is flowed in the fiber lay down layer, use the flow velocity of liquid under stopwatch and the graduated cylinder record different liquids intake pressure simultaneously; Based on the data that record and in conjunction with the concrete form of Darcy's law on different flow directions, calculate in the corresponding fibrous face and the thickness direction saturated permeability.

Description

Reach thickness direction permeability proving installation and saturated permeability method of testing in the fiber lay down aspect
Technical field
The present invention relates to a kind of permeability proving installation and permeability method of testing thereof, more particularly, be meant that being applied to continuous fiber in the polymer matrix composites strengthens body in roofing and the method for testing and the permeability proving installation of thickness direction saturated permeability.
Background technology
Permeability is the parameter that characterizes fluid mobile complexity in porous medium under the pressure effect, and the resistance to flow of the big more expression porous medium of permeability convection cell is more little.In the manufacture process of continuous fibre enhancement resin based composites, the permeability of fiber is one of key factor that influences the resin flows state, it is determined by the physical characteristics of fiber and the inner structure of network of fibers, and is simultaneously also relevant to the wet face state of fiber with physical characteristics, flow direction and the resin of resin.In addition, composite material process planning difference, the form of expression of permeability are also different.For example, resin flows under the effect of injection pressure in the fiber preform of dry state in liquid molding process, carries out simultaneously owing to resin flow with to the infiltration of fiber, and therefore corresponding permeability is called the unsaturation permeability; And often will be that starting material are made compound substance with the prepreg of forming by fiber and resin in hot press forming technology, and can think that generally the fiber in the prepreg has been soaked into fully by resin, resin flows in the fiber of hygrometric state in the technological process, and corresponding permeability is called saturated permeability.Because the influence of factors such as resin-fiber imbibition characteristic and network of fibers inner inclusion air, these two kinds of permeabilities often have tangible difference.
Permeability is the important parameter of research composite material forming process, especially resin flows process, and is requisite input parameter in simulation of composite material forming process computer and the process optimization.The simulation of the manufacturing of compound substance has in the last few years become a research focus, and foundation reliably, the permeability method of testing is one of precondition that guarantees the analog result accuracy accurately.The method of testing of unsaturation permeability is more at present, and cardinal principle is the variation of monitoring resin flows forward and resin pressure or resin flow velocity, calculates the value of permeability in conjunction with Darcy's law; And the research of saturated permeability focuses mostly in the Theoretical Calculation aspect, report seldom aspect method of testing, what time this is mainly because following causing: saturated liquid in the network structure of fiber before (1) test, do not have flow fronts when mobile, common unsaturation permeability method of testing can't be used; (2) for the composite product of non-thin-walled class formation, resin can flow to a plurality of directions simultaneously in forming process, because permeability belongs to tensor, permeability varies in size in different directions, need to measure respectively, this has higher requirement for the design of testing mould; (3) use the fiberless unidirectional pre-immersion material of broadwise in the heat pressing process in large quantities, resin viscosity in this prepreg is very big even be solid-state, can't be used as test liquid, need will soak into fiber again with the little liquid of viscosity after the resin removal and test, and the fiber broadwise does not have binding force in the sample making course, at random easily, cause fibrillar meshwork structure that very big change takes place, the permeability that records can't reflect the Penetration Signature of fibre reinforcement in the actual process process; (4) since sample can't cutting must be in full accord with die size, causing carrying out in the slit of fluid between fibrage and mould the edge flows, this makes that the permeability determination value is bigger than normal, and the fiber lay down coating systems that heat pressing process is used, its fiber volume fraction is generally than higher, permeability is very little, and the influence of edge effect is bigger.This shows that the foundation of fiber lay down layer saturated permeability method of testing and proving installation not only has important significance for theories and using value, and have certain technical difficulty that the influence that need take into account many-sided factor could realize measuring accurately.
Summary of the invention
One of purpose of the present invention provides in a kind of fiber lay down aspect and thickness direction permeability proving installation, the combination that this device goes out to flow plate by cavity and last spreader plate, following spreader plate, left side influent stream plate, right side, realized in same mould, finishing saturated permeability test in the fiber lay down aspect, and the test of fiber lay down layer thickness direction saturated permeability.
Two of purpose of the present invention is to propose in a kind of fiber lay down aspect and thickness direction saturated permeability method of testing, this method of testing can be measured direction saturated permeability in fiber lay down layer thickness direction and the face simultaneously, can be by regulating the pressure control fiber volume fraction, realize the measurement of permeability under the different fiber volume fractions, guaranteeing simultaneously in the specimen preparation process that fiber is not at random and control the edge effectively flows, thereby reduces measuring error to greatest extent.
The present invention is a kind of proving installation that is applied to continuous fiber enhancing body permeability in roofing and on the thickness direction in the polymer matrix composites, this proving installation is made up of air compressor, fluid reservoir, tensimeter, graduated cylinder and mould, air compressor is connected by the A pipeline with fluid reservoir, fluid reservoir is connected by the B pipeline with the liquid feeding end of mould, the B pipeline is provided with and is used for measuring the tensimeter that enters mould test fluid pressure, graduated cylinder is placed on the outlet end of mould, is used for measuring the amount that test fluid flows out from mould.Can realize in the fiber lay down aspect and the test of thickness direction saturated permeability according to the assembling that changes mould.
The present invention a kind ofly is applied to continuous fiber in the polymer matrix composites and strengthens body in roofing and the method for testing of thickness direction saturated permeability, because test fluid is different with the flow direction of thickness direction in the fiber lay down aspect, carries out the substep explanation in the present invention respectively.
The key that the present invention solve the technical problem is to have designed a cover permeability testing mould, thereby has realized the preparation of sample and the mensuration of interior direction of fiber lay down aspect and thickness direction saturated permeability.This method at first is laid in the fabric of prepreg or dry state in the testing mould, the network structure of fiber lay down layer is fixed up on four limits of spreader plate and die cavity about utilizing, re-use solvent the resin in the prepreg is removed, solved the problem that unidirectional pre-immersion material is difficult for sample preparation; By pressurized equipment the fiber lay down layer is exerted pressure, change its fiber volume fraction; Various annexes are installed on testing mould then,, are comprised the flow channel of direction in the fiber lay down aspect and the flow channel of thickness direction to form different flow channels; Under the effect of air pressure, low viscous liquid is injected in the testing mould, it is flowed in the fiber lay down layer, use the flow velocity of liquid under stopwatch and the graduated cylinder record different liquids intake pressure simultaneously; Based on the data that record and in conjunction with the concrete form of Darcy's law on different flow directions, calculate in the corresponding fibrous face and the thickness direction saturated permeability.
The edge that cause fiber lay down layer and die clearance flows and can obviously increase the error of permeability test result, and this gap is difficult to avoid.Use width and all less sealing joint strip of thickness among the present invention, be pasted between fiber lay down layer and the mould, squeezing action when utilizing fiber lay down layer pressurized simultaneously is fully with the shutoff of slit, edge, thereby reduced the error that the edge flows and brings under the situation that does not influence fibrillar meshwork structure and fiber volume fraction as much as possible.By above every design, state and the state in the actual production during sample testing are very close, and can measure the saturated permeability change curve on the different directions simultaneously, so the gained result has very high practical value.
The advantage of fiber lay down layer saturated permeability method of testing of the present invention is: (1) can use a sample to realize in the fiber lay down aspect simultaneously and the mensuration of thickness direction permeability, the testing efficiency height; (2) be applicable to various continuous fibers such as glass fibre, carbon fiber, aramid fiber, also be applicable to various fabric type and prepreg, be particularly useful for the unidirectional pre-immersion material that commonsense method is difficult to measure; (3) can realize different ply sequences, the different shop mensuration of permeability under number, the different fiber volume fractions layer by layer; (4) measuring error is little, and the gained data have higher reliability and repeatability; (5) simple to operate and do not need complexity, expensive equipment.
Description of drawings
Fig. 1 is the external structure diagrammatic sketch of permeability proving installation of the present invention.
Figure 1A goes up influent stream plate upward view.
Figure 1B is following spreader plate configuration diagram.
Fig. 1 C goes out to flow the plate structure diagrammatic sketch under being.
Fig. 2 is a fiber lay down layer thickness direction infiltration mold cavity configuration diagrammatic sketch of the present invention.
Fig. 3 is an infiltration mold cavity configuration diagrammatic sketch in the fiber lay down aspect of the present invention.
Fig. 4 is the wiring layout of test fiber lay down layer thickness direction saturated permeability.
Fig. 5 is the wiring layout of saturated permeability in the test fiber lay down aspect.
Fig. 6 is the relation curve of fiber volume fraction and permeability.
Among the figure: 1. cavity 101. infiltration chamber 102. boss, 103. locking nail 104.A through holes, 105. screwed hole 106.B through holes, 107. right side flow-out holes, 108. left side flow-in holes go out to flow 203. times spout 3. right sides of plate 201.H through hole 202.C groove for 2. times and go out to flow on the plate 301. right conduit 4. left side influent stream plates 401. left conduits 5. 7. times flow distribution plates of flow distribution plate 601.D groove, 701. pod apertures 702.D through hole 703.E through hole 704.F through hole 705.B groove 706.G through holes, 11. air compressors, 12. fluid reservoirs, 13. Pressure gauges, 14. graduated cylinders, 15. mould 16.A pipeline 17.B pipelines on the influent stream plate 501.A groove 502. right handle 503. left handle 504.C through hole 505. enterprising stem bars 6.
Embodiment
The present invention is described in further detail below in conjunction with accompanying drawing.
The present invention be a kind of be applied to continuous fiber in the polymer matrix composites strengthen body in roofing and on the thickness direction proving installation of permeability (see also Fig. 4, shown in Figure 5), this proving installation is by air compressor 11, fluid reservoir 12, tensimeter 13, graduated cylinder 14 and mould 15 are formed, air compressor 11 is connected by A pipeline 16 with fluid reservoir 12, fluid reservoir 12 is connected by B pipeline 17 with the liquid feeding end of mould 15, B pipeline 17 is provided with and is used for measuring the tensimeter 13 that enters mould 15 test fluid pressure, graduated cylinder 14 is placed on the outlet end of mould 15, is used for measuring the amount that test fluid flows out from mould 15.
Referring to Fig. 1 and shown in Figure 2, described mould 15 by cavity 1, go up influent stream plate 5, down spreader plate 7, go out to flow plate 2, right side down and go out to flow plate 3, left side influent stream plate 4, go up spreader plate 6 and form, the top of cavity 1 is to go up influent stream plate 5, the below of cavity 1 is following spreader plate 7, the bottom of following spreader plate 7 goes out to flow plate 2 under being, the left surface of cavity 1 is provided with left side influent stream plate 4, and the right flank of cavity 1 is provided with the right side and goes out to flow plate 3; Mould 15 of the present invention adopts No. 45 steels to do, and has higher rigidity and very long serviceable life, to reduce the test error that die deformation brings.
The center of described cavity 1 is provided with infiltration chamber 101, wall has a plurality of boss 102 (referring to shown in Figure 2) respectively in the infiltration chamber 101, have left side flow-in hole 108 on the left plate in infiltration chamber 101, have right side flow-out hole 107 (referring to shown in Figure 3) on the right plate in infiltration chamber 101, have A through hole 104, threaded hole 105, B through hole 106 on the end face of cavity 1.Last spreader plate 6 is placed in the infiltration chamber 101 (referring to shown in Figure 2).Be equipped with locking nail 103 (referring to shown in Figure 2) on the boss 102 in the infiltration chamber 101, be used to regulate the fiber volume fraction of fiber lay down layer.The diameter of left side flow-in hole 108, right side flow-out hole 107 is 2~6mm, and liquid can be flowed along direction in the fiber lay down aspect equably.
Described center of going up influent stream plate 5 is provided with enterprising stem bar 505, has C through hole 504 all around, and the left side is provided with left handle 503, and the right side is provided with right handle 502 (referring to shown in Figure 1), and the bottom centre of last influent stream plate 5 has A groove 501 (shown in Figure 1A).
Described spreader plate 7 down is provided with B groove 705, has pod apertures 701 in the B groove 705, and four jiaos of B groove 705 have F through hole 704, have D through hole 702, G through hole 706, E through hole 703 around the following spreader plate 7.The diameter of pod apertures 701 is 2~6mm, make liquid can be equably along fiber lay down layer thickness direction flow (shown in Figure 1B).The diameter of the pod apertures on the last spreader plate 6 is 2~6mm, make liquid can be equably along fiber lay down layer thickness direction flow (referring to shown in Figure 2).
The described bottom centre that goes out to flow plate 2 down is provided with down spout 203, has H through hole 201 all around, and the central upper portion that goes out to flow plate 2 down has C groove 202 (shown in Fig. 1 C).
Described right side goes out to flow plate 3 and is provided with right conduit 301, and described left side influent stream plate 4 is provided with left conduit 401 (referring to shown in Figure 2).When carrying out the test of thickness direction permeability, on right conduit 301, left conduit 401, overlap upper cap nut respectively, prevent that liquid from flowing along direction in the fiber lay down aspect.When directional permeability is tested in carrying out face, in the groove of last spreader plate 6, following spreader plate 7, install cover plate additional respectively, prevent that liquid from flowing along fiber lay down layer thickness direction.
In the present invention, C through hole 504, A through hole 104, D through hole 702 and H through hole 201 are used for bolt to be passed through, and G through hole 706 and threaded hole 105 are used for screw to be passed through, and E through hole 703 and B through hole 106 are used for pin to be passed through.
The present invention a kind ofly is applied to continuous fiber in the polymer matrix composites and strengthens body in roofing and the method for testing of thickness direction saturated permeability, because test fluid is different with the flow direction of thickness direction in the fiber lay down aspect, when when fiber lay down layer thickness direction being carried out the permeability test, its thickness direction permeability method of testing has the following steps:
The first step: sample is chosen
Sample is cut into and the size of permeating chamber 101 adaptive sizes, and the sample area is S; Count n layer by layer according to ply sequence and shop then and carry out laying formation fiber lay down layer;
Described sample can be not resiniferous fabric, also can be prepreg.Described fabric is plain cloth, twills, satin fabric etc.; Resin is epoxy resin, phenolics, cyanate ester resin, bismaleimide resin etc. in the described prepreg; Fiber is glass fibre, carbon fiber, aramid fiber or basalt fibre etc. in the described prepreg.
Described ply sequence has unidirectional shop layer, quadrature shop layer, quasi-isotropic shop layer etc.
Described shop is counted n layer by layer 10~60 layers.
Second step: permeability test pre-preparation
Cavity 1 is inverted, in infiltration chamber 101, is put into spreader plate 6, described fiber lay down layer, following spreader plate 7 sequentially; Screw will descend spreader plate 7 to be fixed on the bottom of cavity 1 by G through hole 706 and threaded hole 105, realize described fiber lay down layer is clamped in the infiltration chamber 101.Before laying down spreader plate 7,0.5~2mm is wide with being cut into, the sealing of the sealing joint strip of 0.2~1 millimeters thick at periphery that the fiber lay down layer contact with infiltration chamber 101 inwalls, and liquid can't be mobile at place, slit, edge when guaranteeing the permeability test.
Fit on locking nail 103 in boss 102 can make spreader plate 6 and described fiber lay down laminating tight by regulating locking nail 103.The right side goes out to flow plate 3 and is installed in cavity 1 right side, and left side influent stream plate 4 is installed in cavity 1 left side.Assembling obtains to exert pressure mould.
The 3rd step: the control of fiber lay down layer fiber volume fraction
In the present invention, in order to determine fiber lay down layer permeability and fiber volume fraction V fBetween quantitative relationship, before measuring permeability, need to obtain the fiber volume fraction V of fiber lay down layer f, permeability and fiber volume fraction V fBetween the typical relation curve as shown in Figure 6.
Exerted pressure mould in second step is placed on the pressurized equipment pressure 0~2MPa; The pressure head of pressurized equipment contacts with last spreader plate 6, with the height h of vernier caliper measurement cavity 1 upper surface apart from last spreader plate 6.
After treating that spreader plate 6 drop-out values are stable, regulate locking nail 103, prevent fiber resilience after the release, note height h; Release and mould taken off from pressurized equipment then.
Can change fiber volume fraction by the method for regulating pressure thus V f = na f ρ f h f , H wherein f=h 0-h.
To go up influent stream plate 5 and be installed in cavity 1 top, going out to flow plate 2 is installed in down spreader plate 7 bottoms down, and assembling obtains the permeability testing mould.
The 4th step: fiber lay down layer thickness directional permeability test (parts assemble referring to shown in Figure 4)
Difference socket one nut on left conduit 401, right conduit 301 prevents that test fluid is along flowing in the fiber lay down aspect;
One end of B pipeline 17 is connected with the enterprising stem bar 505 of described permeability testing mould;
With graduated cylinder 14 be placed on down spout 203 under;
Open the air pressure of air compressor 11 outputs 0~0.1MPa and give fluid reservoir 12, test fluid in the fluid reservoir 12 under the promotion of air pressure earlier after enterprising stream plate 5, on spreader plate 6, fiber lay down layer, down spreader plate 7, go out to flow plate 2 down and flow out, the test fluid volume V that is received in the time according to 30~300s by graduated cylinder 14 obtains the flow velocity Q of test fluid.
When measuring fiber lay down layer thickness directional permeability, the pressurized air that has utilized air compressor 11 to provide injects the last influent stream plate 5 of the test fluid in the fluid reservoir 12 from mould 15, test fluid flows along fiber lay down layer thickness direction, and finally under go out to flow plate 2 and flow into the graduated cylinder 14.Can change the size of test fluid intake pressure P by regulating tensimeter 13, thereby change test fluid flow velocity Q, can obtain thickness direction saturated permeability k according to Darcy's law.
Described thickness direction saturated permeability k Z = Qη h f PS , In the formula, k ZExpression thickness direction saturated permeability, Q represents the test fluid flow velocity, η represents the viscosity of test fluid, h fThe fiber lay down layer thickness that forms behind the tiling fiber number of plies n in the expression infiltration chamber 101, P represents manometric displayed value, S represents the surface area of top layer in the fiber lay down layer.
The present invention a kind ofly is applied to continuous fiber in the polymer matrix composites and strengthens body in roofing and the method for testing of thickness direction saturated permeability, because test fluid is different with the flow direction of thickness direction in the fiber lay down aspect, when carrying out the permeability test in to the fiber lay down aspect, its face intrinsic permeability method of testing has the following steps:
The first step: sample is chosen
Sample is cut into and the size of permeating chamber 101 adaptive sizes, and the sample area is S; Count n layer by layer according to ply sequence and shop then and carry out laying formation fiber lay down layer;
Described sample can be not resiniferous fabric, also can be prepreg.Described fabric is plain cloth, twills, satin fabric etc.; Resin is epoxy resin, phenolics, cyanate ester resin, bismaleimide resin etc. in the described prepreg; Fiber is glass fibre, carbon fiber, aramid fiber or basalt fibre etc. in the described prepreg.
Described ply sequence has unidirectional shop layer, quadrature shop layer, quasi-isotropic shop layer etc.
Described shop is counted n layer by layer 10~60 layers.
Second step: permeability test pre-preparation
Cavity 1 is inverted, in infiltration chamber 101, is put into spreader plate 6, described fiber lay down layer, following spreader plate 7 sequentially; Screw will descend spreader plate 7 to be fixed on the bottom of cavity 1 by G through hole 706 and threaded hole 105, realize described fiber lay down layer is clamped in the infiltration chamber 101.Before laying down spreader plate 7,0.5~2mm is wide with being cut into, the sealing of the sealing joint strip of 0.2~1 millimeters thick at periphery that the fiber lay down layer contact with infiltration chamber 101 inwalls, and liquid can't be mobile at place, slit, edge when guaranteeing the permeability test.
Fit on locking nail 103 in boss 102 can make spreader plate 6 and described fiber lay down laminating tight by regulating locking nail 103.The right side goes out to flow plate 3 and is installed in cavity 1 right side, and left side influent stream plate 4 is installed in cavity 1 left side.Assembling obtains to exert pressure mould.
The 3rd step: the control of fiber lay down layer fiber volume fraction
In the present invention, in order to determine fiber lay down layer permeability and fiber volume fraction V fBetween quantitative relationship, before measuring permeability, need to obtain the fiber volume fraction V of fiber lay down layer f, permeability and fiber volume fraction V fBetween the typical relation curve as shown in Figure 6.
Exerted pressure mould in second step is placed on the pressurized equipment pressure 0~2MPa; The pressure head of pressurized equipment contacts with last spreader plate 6, with the height h of vernier caliper measurement cavity 1 upper surface apart from last spreader plate 6.
After treating that spreader plate 6 drop-out values are stable, regulate locking nail 103, prevent fiber resilience after the release, note height h; Release and mould taken off from pressurized equipment then.
Can change fiber volume fraction by the method for regulating pressure thus V f = na f ρ f h f , H wherein f=h 0One h.
To go up influent stream plate 5 and be installed in cavity 1 top, going out to flow plate 2 is installed in down spreader plate 7 bottoms down, and assembling obtains the permeability testing mould.
The 4th step: fiber lay down aspect intrinsic permeability test (parts assemble referring to shown in Figure 5)
At first take off the last influent stream plate 5 of penetration testing mould in the 3rd step, and in the D of last spreader plate 6 groove 601, press cover plate, will go up influent stream plate 5 then and be installed in cavity 1 top once more; Then, difference socket nut on enterprising stem bar 505, following spout 203 prevents that test fluid from flowing along fiber lay down layer thickness direction;
With graduated cylinder 14 be placed on right conduit 301 under;
One end of B pipeline 17 is connected with the left conduit 401 of described penetration testing mould; Open the air pressure of air compressor 11 outputs 0~0.1MPa and give fluid reservoir 12; Earlier after left conduit 401, left side flow-in hole 108, fiber lay down layer, right side flow-out hole 107, right conduit 301 flow out, the test fluid volume V that is received in the time according to 30~300s by graduated cylinder 14 obtains the flow velocity Q of test fluid to test fluid in the fluid reservoir 12 under the promotion of air pressure.
When test fiber lay down aspect intrinsic permeability, the pressurized air that has utilized air compressor 11 to provide injects the left side influent stream plate 4 of the test fluid in the fluid reservoir 12 from mould 15, test fluid flows along direction in the fiber lay down aspect, and finally goes out to flow plate 3 from the right side and flow into the graduated cylinder 14.Can change the size of liquid-inlet pressure P by regulating tensimeter 13, thereby change test fluid flow velocity Q, can obtain saturated permeability k in the face according to Darcy's law p
Described interior saturated permeability k p = Qη P h f , In the formula, k pSaturated permeability in the presentation surface, Q represents the test fluid flow velocity, η represents the viscosity of test fluid, h fThe fiber lay down layer thickness that forms behind the tiling fiber number of plies n in the expression infiltration chamber 101, P represents manometric displayed value.
In the present invention is directed to permeability saturation testing method, the 4th step of thickness direction permeability test and the 4th step of face intrinsic permeability test are coordination.In this step, because the difference of test fluid outflow end causes mould different at fit on.Thereby make proving installation of the present invention have the test that can realize two kinds of permeabilities, reduced the sample production cost effectively.In order to test the permeability in the fiber lay down aspect, its step goes on foot in the first step, second with fiber lay down layer thickness directional permeability, the 3rd step is identical, and difference was for the 4th step.
In the present invention, described test fluid is soybean oil, corn steep liquor or unsaturated polyester (UP) etc.
In the present invention, when institute's test specimens is prepreg, after second step, need prepreg is carried out pre-treatment.Described pre-treatment is meant puts into the resin that solvent removes prepreg with the described mould of exerting pressure.Described solvent is acetone, ethanol, methylene chloride, tetrahydrofuran etc.
If will measure the saturated permeability under the higher fiber volume fraction, can apply bigger pressure the thickness of fiber lay down layer is further reduced, test by foregoing the 3rd step, the 4th step then.So also constantly regulating pressure carries out permeability determination in circulation, can obtain the change curve that saturated permeability reduces with the fiber volume fraction increase in fiber lay down layer thickness direction and the face.
Embodiment 1:
High-strength glass fibre/epoxy E51 resin unidirectional pre-immersion material is a tested object to adopt S-2.Prepreg is cut into 10 * 10cm 240 layers of back laies, ply sequence are unidirectional shop layer; With acetone with epoxy E51 resin dissolves after, soak into the fiber lay down layer with soybean oil, be pressurized equipment then with the small-sized press, with the soybean oil is test liquid, measure in the fiber lay down aspect of fiber volume fraction in 47~71% scopes and the thickness direction saturated permeability, pressure P is regulated in 0.01~0.08MPa scope, and experimental temperature is 20 ℃, the soybean oil viscosity is 0.06Pas under this temperature, and test result sees Table 1 and table 2.
The test result of saturated permeability in the table 1. fiber lay down aspect
Fiber volume fraction (%) Face intrinsic permeability (10 -12m 2)
47.0 23.3
51.6 15.3
56.6 10.5
63.0 6.2
67.8 3.5
70.0 1.3
71.0 0.9
The test result of table 2. fiber lay down layer thickness direction saturated permeability
Fiber volume fraction (%) Thickness direction permeability (10 -14m 2)
47.0 25.1
51.6 12.2
56.6 4.6
63.0 2.4
67.8 1.1
70.0 1.0
71.0 0.8
Embodiment 2:
Adopting T700 carbon fiber plain fabric is tested object.Fabric is cut into 10 * 10cm 220 layers of back laies, ply sequence are quadrature shop layer; With the small-sized press is pressurized equipment, with the corn steep liquor is test liquid, measure fiber volume fraction in 60% o'clock fiber lay down aspect and the thickness direction saturated permeability, pressure P is regulated in 0.03~0.05MPa scope, experimental temperature is 15 ℃, the viscosity of corn steep liquor is 0.04Pas under this temperature, is respectively 6.2 * 10 with the thickness direction saturated permeability in the fiber lay down aspect of test gained -12m 2With 7.8 * 10 -13m 2
Embodiment 3:
Adopting T300 carbon fiber twill fabric is tested object.Fabric is cut into 10 * 10cm 235 layers of back laies, ply sequence are quasi-isotropic shop layer; With the small-sized press is pressurized equipment, with the soybean oil is test liquid, measure fiber volume fraction in 55% o'clock fiber lay down aspect and the thickness direction saturated permeability, pressure P is regulated in 0.07~0.09MPa scope, experimental temperature is 25 ℃, the soybean oil viscosity is 0.03Pas under this temperature, is respectively 13.2 * 10 with the thickness direction saturated permeability in the fiber lay down aspect of test gained -12m 2With 10.1 * 10 -14m 2
The physical significance of quotation mark is among the present invention:
V f The expression fiber volume fraction.
n Count layer by layer the shop of expression fiber lay down layer, is called for short the fiber number of plies.
a f Represent fibrolaminar fiber areal densities, unit is kg/m 2
ρ f The volume density of expression fiber, unit is kg/m 3
h f The thickness of fiber lay down layer in the expression infiltration chamber 101, unit is m.
h 0 Cavity 1 upper surface was not apart from the height of last spreader plate 6 when the fiber lay down layer was put in expression, and unit is m.
h Expression cavity 1 upper surface is apart from the height of last spreader plate 6, and unit is m.
k p Saturated permeability in the expression fiber lay down aspect, unit is m 2
Q The volume flow rate of expression test fluid, unit is m 3/ s.
η The viscosity of expression test fluid, unit is Pas.
P The displayed value of expression tensimeter 13, unit is Pa.
k Z The saturated permeability of expression fiber lay down layer thickness direction, unit is m 2
S Expression sample area, promptly fibrolaminar length * wide, unit is m 2

Claims (6)

1, a kind of proving installation that is applied to continuous fiber enhancing body permeability in roofing and on the thickness direction in the polymer matrix composites, it is characterized in that: by air compressor (11), fluid reservoir (12), tensimeter (13), graduated cylinder (14) and mould (15) are formed, air compressor (11) is connected by A pipeline (16) with fluid reservoir (12), fluid reservoir (12) is connected by B pipeline (17) with the liquid feeding end of mould (15), B pipeline (17) is provided with and is used for measuring the tensimeter (13) that enters mould (15) test fluid pressure, and graduated cylinder (14) is placed on the outlet end of mould (15);
Described mould (15) by cavity (1), go up influent stream plate (5), down spreader plate (7), go out to flow plate (2), right side down and go out to flow plate (3), left side influent stream plate (4), go up spreader plate (6) and form, the top of cavity (1) is to go up influent stream plate (5), the below of cavity (1) is following spreader plate (7), the bottom of following spreader plate (7) goes out to flow plate (2) under being, the left surface of cavity (1) is provided with left side influent stream plate (4), and the right flank of cavity (1) is provided with the right side and goes out to flow plate (3); The center of described cavity (1) is infiltration chamber (101), the interior wall in infiltration chamber (101) has a plurality of boss (102) respectively, have left side flow-in hole (108) on the left plate in infiltration chamber (101), have right side flow-out hole (107) on the right plate in infiltration chamber (101), have A through hole (104), threaded hole (105), B through hole (106) on the end face of cavity (1); Last spreader plate (6) is placed in the infiltration chamber (101); Be equipped with locking nail (103) on the boss (102) in the infiltration chamber (101);
The diameter of described left side flow-in hole (108), right side flow-out hole (107) is 2~6mm;
Described center of going up influent stream plate (5) is provided with enterprising stem bar (505), has C through hole (504) all around, and the left side is provided with left handle (503), and the right side is provided with right handle (502), and the bottom centre of last influent stream plate (5) has A groove (501);
Described spreader plate (7) down is provided with B groove (705), has pod apertures (701) in the B groove (705), and four jiaos of B groove (705) have F through hole (704), have D through hole (702), G through hole (706), E through hole (703) around the following spreader plate (7); The diameter of pod apertures (701) is 2~6mm;
The described spreader plate (6) of going up is provided with D groove (601), and the diameter of the pod apertures on the last spreader plate (6) is 2~6mm;
The described bottom centre that goes out to flow plate (2) down is provided with down spout (203), has H through hole (201) all around, and the central upper portion that goes out to flow plate (2) down has C groove (202);
Described right side goes out to flow plate (3) and is provided with right conduit (301);
Described left side influent stream plate (4) is provided with left conduit (401).
2, permeability proving installation according to claim 1, it is characterized in that: C through hole (504), A through hole (104), D through hole (702) and H through hole (201) are used for bolt to be passed through, G through hole (706) and threaded hole (105) are used for screw to be passed through, and E through hole (703) and B through hole (106) are used for pin to be passed through.
3, permeability proving installation according to claim 1 is applied to the method that continuous fiber enhancing body carries out the permeability test in fiber lay down layer thickness direction in the polymer matrix composites, and it is characterized in that: thickness direction permeability method of testing has the following steps:
The first step: sample is chosen
Sample is cut into and the size of permeating the adaptive size in chamber (101), and the sample area is S; Count n layer by layer according to ply sequence and shop then and carry out laying formation fiber lay down layer;
Second step: permeability test pre-preparation
Cavity (1) is inverted, in infiltration chamber (101), is put into spreader plate (6), described fiber lay down layer, following spreader plate (7) sequentially; Screw will descend spreader plate (7) to be fixed on the bottom of cavity (1) by G through hole (706) and threaded hole (105); It is preceding to lay down spreader plate (7), and 0.5~2mm is wide with being cut into, the sealing of the sealing joint strip of 0.2~1 millimeters thick at periphery that the fiber lay down layer contact with infiltration chamber (101) inwall, and liquid can't be mobile at place, slit, edge when guaranteeing the permeability test;
Fit on locking nail (103) in boss (102), right side go out to flow plate (3) and are installed in cavity (1) right side, and left side influent stream plate (4) is installed in cavity (1) left side, and assembling obtains to exert pressure mould;
The 3rd step: the control of fiber lay down layer fiber volume fraction
Exerted pressure mould in second step is placed on the pressurized equipment pressure 0~2MPa; The pressure head of pressurized equipment contacts with last spreader plate (6), with the height h of vernier caliper measurement cavity (1) upper surface apart from last spreader plate (6);
After treating that spreader plate (6) drop-out value is stable, regulate locking nail (103), prevent fiber resilience after the release, note height h; Release and mould taken off from pressurized equipment then;
Change fiber volume fraction by the method for regulating pressure thus V f = na f ρ f h f , H wherein f=h 0-h, in the formula, V fExpression fiber volume fraction, n represent that fibrolaminar shop is several layer by layer, a fThe fibrolaminar fiber areal densities of expression expression, ρ fThe volume density of expression fiber, h fThe thickness of fiber lay down layer in the expression infiltration chamber (101), h 0Cavity (1) upper surface was not apart from the height of last spreader plate (6) when the fiber lay down layer was put in expression;
To go up influent stream plate (5) and be installed in cavity (1) top, and go out to flow plate (2) down and be installed in down spreader plate (7) bottom, assembling obtains the permeability testing mould;
The 4th step: fiber lay down layer thickness directional permeability test
Go up socket one nut respectively at left conduit (401), right conduit (301), prevent that test fluid is along flowing in the fiber lay down aspect;
One end of B pipeline (17) is connected with the enterprising stem bar (505) of described permeability testing mould;
With graduated cylinder (14) be placed on down spout (203) under;
Open the air pressure of air compressor (11) output 0~0.1MPa and give fluid reservoir (12), test fluid in the fluid reservoir (12) under the promotion of air pressure earlier after enterprising stream plate (5), go up spreader plate (6), fiber lay down layer, down spreader plate (7), go out to flow plate (2) down and flow out, the test fluid volume V that is received in the time according to 30~300s by graduated cylinder (14) obtains the flow velocity Q of test fluid;
Obtain the thickness direction saturated permeability according to Darcy's law k z = Qηh f PS , In the formula, k zExpression thickness direction saturated permeability, Q represents the test fluid flow velocity, η represents the viscosity of test fluid, h fThe fiber lay down layer thickness that forms behind the tiling fiber number of plies n in the expression infiltration chamber (101), P represents manometric displayed value, S represents the surface area of top layer in the fiber lay down layer.
4, permeability proving installation according to claim 1 is applied to the method that continuous fiber enhancing body carries out the permeability test in the polymer matrix composites in the fiber lay down aspect, and it is characterized in that: face intrinsic permeability method of testing has the following steps:
The first step: sample is chosen
Sample is cut into and the size of permeating the adaptive size in chamber (101), and the sample area is S; Count n layer by layer according to ply sequence and shop then and carry out laying formation fiber lay down layer;
Second step: permeability test pre-preparation
Cavity (1) is inverted, in infiltration chamber (101), is put into spreader plate (6), described fiber lay down layer, following spreader plate (7) sequentially; Screw will descend spreader plate (7) to be fixed on the bottom of cavity (1) by G through hole (706) and threaded hole (105); It is preceding to lay down spreader plate (7), and 0.5~2mm is wide with being cut into, the sealing of the sealing joint strip of 0.2~1 millimeters thick at periphery that the fiber lay down layer contact with infiltration chamber (101) inwall, and liquid can't be mobile at place, slit, edge when guaranteeing the permeability test;
Fit on locking nail (103) in boss (102), right side go out to flow plate (3) and are installed in cavity (1) right side, and left side influent stream plate (4) is installed in cavity (1) left side, and assembling obtains to exert pressure mould;
The 3rd step: the control of fiber lay down layer fiber volume fraction
Exerted pressure mould in second step is placed on the pressurized equipment pressure 0~2MPa; The pressure head of pressurized equipment contacts with last spreader plate (6), with the height h of vernier caliper measurement cavity (1) upper surface apart from last spreader plate (6);
After treating that spreader plate (6) drop-out value is stable, regulate locking nail (103), prevent fiber resilience after the release, note height h; Release and mould taken off from pressurized equipment then;
Change fiber volume fraction by the method for regulating pressure thus V f = na f ρ f h f , H wherein f=h 0-h, in the formula, V fExpression fiber volume fraction, n represent that fibrolaminar shop is several layer by layer, a fThe fibrolaminar fiber areal densities of expression expression, ρ fThe volume density of expression fiber, h fThe thickness of fiber lay down layer in the expression infiltration chamber (101), h 0Cavity (1) upper surface was not apart from the height of last spreader plate (6) when the fiber lay down layer was put in expression;
To go up influent stream plate (5) and be installed in cavity (1) top, and go out to flow plate (2) down and be installed in down spreader plate (7) bottom, assembling obtains the permeability testing mould;
The 4th step: fiber lay down aspect intrinsic permeability test
At first take off the last influent stream plate (5) of penetration testing mould in the 3rd step, and in the D groove (601) of last spreader plate (6), press cover plate, will go up influent stream plate (5) then and be installed in cavity (1) top once more; Then, go up socket nut respectively, prevent that test fluid from flowing along fiber lay down layer thickness direction at enterprising stem bar (505), following spout (203);
With graduated cylinder (14) be placed on right conduit (301) under;
One end of B pipeline (17) is connected with the left conduit (401) of described penetration testing mould; Open the air pressure of air compressor (11) output 0~0.1MPa and give fluid reservoir (12); Earlier after left conduit (401), left side flow-in hole (108), fiber lay down layer, right side flow-out hole (107), right conduit (301) flow out, the test fluid volume V that is received in the time according to 30~300s by graduated cylinder (14) obtains the flow velocity Q of test fluid to test fluid in the fluid reservoir (12) under the promotion of air pressure;
Can obtain saturated permeability in the face according to Darcy's law k p = Qη Ph f , In the formula, k pSaturated permeability in the presentation surface, Q represents the test fluid flow velocity, η represents the viscosity of test fluid, h fThe fiber lay down layer thickness that forms behind the tiling fiber number of plies n in the expression infiltration chamber (101), P represents manometric displayed value.
5, according to claim 3 or 4 described permeability method of testings, it is characterized in that: sample described in the first step is not resiniferous fabric or prepreg; Described fabric is plain cloth, twills or satin fabric; Resin is epoxy resin, phenolics, cyanate ester resin or bismaleimide resin in the described prepreg; Fiber is glass fibre, carbon fiber, aramid fiber or basalt fibre in the described prepreg.
6, according to claim 3 or 4 described permeability method of testings, it is characterized in that: ply sequence described in the first step has unidirectional shop layer, quadrature shop layer or quasi-isotropic shop layer, and described shop is counted n layer by layer 10~60 layers.
CNB2007100991606A 2007-05-15 2007-05-15 Reach thickness direction permeability proving installation and saturated permeability method of testing in the fiber lay down aspect Expired - Fee Related CN100554933C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CNB2007100991606A CN100554933C (en) 2007-05-15 2007-05-15 Reach thickness direction permeability proving installation and saturated permeability method of testing in the fiber lay down aspect

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CNB2007100991606A CN100554933C (en) 2007-05-15 2007-05-15 Reach thickness direction permeability proving installation and saturated permeability method of testing in the fiber lay down aspect

Publications (2)

Publication Number Publication Date
CN101051019A CN101051019A (en) 2007-10-10
CN100554933C true CN100554933C (en) 2009-10-28

Family

ID=38782538

Family Applications (1)

Application Number Title Priority Date Filing Date
CNB2007100991606A Expired - Fee Related CN100554933C (en) 2007-05-15 2007-05-15 Reach thickness direction permeability proving installation and saturated permeability method of testing in the fiber lay down aspect

Country Status (1)

Country Link
CN (1) CN100554933C (en)

Families Citing this family (26)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101819129B (en) * 2010-05-07 2011-06-22 中国人民解放军国防科学技术大学 Testing method of external permeability of fiber fabric surface and testing mold
CN102507405B (en) * 2010-07-26 2013-07-17 水利部交通运输部国家能源局南京水利科学研究院 Large-sized numerical control two-way permeameter
CN102141504B (en) * 2011-01-27 2013-06-12 中国商用飞机有限责任公司 Testing device and method for testing gas penetration rate in thickness direction of overlay
CN102183444B (en) * 2011-01-27 2013-09-25 中国商用飞机有限责任公司 Device and method for testing gas permeability in inner direction of paving layer surface
CN102288526B (en) * 2011-05-17 2014-01-29 东华大学 Device and method for detecting permeability of unwoven fabrics
CN102313686B (en) * 2011-07-28 2013-03-06 哈尔滨工业大学 Method for measuring internal permeability of prepreg with three-dimensional space analysis
CN102692369B (en) * 2012-05-14 2014-06-11 西北工业大学 Measuring device and measuring method for measuring axial steady state permeability of continuous fiber bundle
CN102778424B (en) * 2012-08-22 2014-12-17 山东大学 Fabric thickness directional permeability testing device and testing method
CN102778423B (en) * 2012-08-22 2015-04-01 山东大学 Fabric one-way surface permeability testing device and testing method
CN102809530B (en) * 2012-08-22 2014-11-05 山东大学 Device and method for testing intrinsic permeability of radial surface of fiber fabric
CN102937561B (en) * 2012-10-17 2014-07-02 西北工业大学 Determination method for orthogonal non-woven three-dimensional rectangular fabric permeability
KR101421690B1 (en) 2013-05-09 2014-07-22 명지대학교 산학협력단 Apparatus for measuring coefficient of permeability
CN104297122B (en) * 2013-07-17 2017-02-08 中国科学院宁波材料技术与工程研究所 Measurement method for natural fiber fabric in-plane saturated permeability
CN104297121B (en) * 2013-07-17 2017-04-12 中国科学院宁波材料技术与工程研究所 Measurement method for in-plane unsaturated permeability rates of natural fiber fabric
CN103439235A (en) * 2013-08-27 2013-12-11 西北工业大学 Method for measuring permeability of different flat-plate fiber preformed bodies
CN105466828B (en) * 2014-09-09 2018-03-16 核工业北京地质研究院 A kind of encapsulating method of crack rock resistance to hypertonic pressure under shear action
CN104897541B (en) * 2015-05-07 2017-04-19 中南大学 Combined type multifunctional fiber fabric in-plane permeability integrated test device
CN105954169A (en) * 2016-04-20 2016-09-21 西北工业大学 Measuring method and measuring system for thickness-direction steady-state permeation rate of fiber fabric
CN106525692B (en) * 2016-12-22 2023-04-25 合肥学院 Porous material permeability testing device and system
CN108982323A (en) * 2018-07-20 2018-12-11 东北林业大学 Measuring device and its method for plate preform fiber pervasion rate
CN109406371A (en) * 2018-12-17 2019-03-01 西安石油大学 It is a kind of coupled based on man-made fracture with intrinsic fracture under permeability survey method and measuring system
CN110779846B (en) * 2019-10-15 2021-02-19 北京航空航天大学 Method for testing gas in-plane permeability of unsaturated impregnated fiber/resin prepreg
CN110763591A (en) * 2019-12-02 2020-02-07 核工业理化工程研究院 Method and device for testing fiber gum dipping and fluffing amount
CN112345432B (en) * 2021-01-08 2021-04-09 中海储能科技(北京)有限公司 Testing device and testing method for permeability of carbon fiber cloth in laying direction
CN112903562A (en) * 2021-01-25 2021-06-04 北京临近空间飞行器系统工程研究所 Device and method for testing permeability of resin-based composite material
CN115422785B (en) * 2022-11-04 2023-03-14 中国航发北京航空材料研究院 Method and device for determining permeability of component contact surface in RTM (resin transfer molding) simulation

Non-Patent Citations (8)

* Cited by examiner, † Cited by third party
Title
RTM工艺增强纤维渗透率测量方法研究. 李海晨,张明福,王彪.航空材料学报,第21卷第1期. 2001
RTM工艺增强纤维渗透率测量方法研究. 李海晨,张明福,王彪.航空材料学报,第21卷第1期. 2001 *
真空压力下液体沿炭纤维织物铺层厚度方向的渗透特性. 徐伟,李敏,张佐光.复合材料学报,第23卷第3期. 2006
真空压力下液体沿炭纤维织物铺层厚度方向的渗透特性. 徐伟,李敏,张佐光.复合材料学报,第23卷第3期. 2006 *
纤维堆积体厚度方向浸渗特性. 罗慧珍,张佐光,李敏.复合材料学报,第22卷第5期. 2005
纤维堆积体厚度方向浸渗特性. 罗慧珍,张佐光,李敏.复合材料学报,第22卷第5期. 2005 *
铺层方式对织物渗透率的影响. 陈萍,李宏运,陈祥宝.复合材料学报,第18卷第1期. 2001
铺层方式对织物渗透率的影响. 陈萍,李宏运,陈祥宝.复合材料学报,第18卷第1期. 2001 *

Also Published As

Publication number Publication date
CN101051019A (en) 2007-10-10

Similar Documents

Publication Publication Date Title
CN100554933C (en) Reach thickness direction permeability proving installation and saturated permeability method of testing in the fiber lay down aspect
CN102183444B (en) Device and method for testing gas permeability in inner direction of paving layer surface
CN102141504B (en) Testing device and method for testing gas penetration rate in thickness direction of overlay
Scholz et al. Measurement of transverse permeability using gaseous and liquid flow
Babu et al. Experimental investigation of the effect of fiber-mat architecture on the unsaturated flow in liquid composite molding
Chen et al. Flow modeling and simulation for vacuum assisted resin transfer molding process with the equivalent permeability method
Li et al. A simple method for the measurement of compaction and corresponding transverse permeability of composite prepregs
CN102778424B (en) Fabric thickness directional permeability testing device and testing method
CN101049722B (en) Device for testing condition for forming pore bugs in hyperpressure forming process, and method for eliminating pores
Bickerton et al. Resin infusion/liquid composite moulding (LCM) of advanced fibre-reinforced polymer (FRP)
Korkiakoski et al. Experimental compaction characterization of unidirectional stitched noncrimp fabrics in the vacuum infusion process
CN103439235A (en) Method for measuring permeability of different flat-plate fiber preformed bodies
CN105954169A (en) Measuring method and measuring system for thickness-direction steady-state permeation rate of fiber fabric
CN104297121B (en) Measurement method for in-plane unsaturated permeability rates of natural fiber fabric
CN106353236A (en) Device for testing in-plane and out-plane permeability of fabric
CN108982323A (en) Measuring device and its method for plate preform fiber pervasion rate
CN104833728B (en) A kind of composite material porosity detection mark block and preparation method thereof
CN108051350A (en) A kind of porous material testing permeability device and test method
US20180250894A1 (en) Impregnation test apparatus and method for evaluating impregnation property using the same
Tan et al. A method to estimate the accuracy of radial flow—based permeability measuring devices
CN205836037U (en) A kind of preparation facilities testing use composite board sample
Kim et al. Observation of permeability dependence on flow rate and implications for liquid composite molding
CN104786523A (en) Resin-transfer-molded composite material porosity testing standard block and preparation method thereof
Roy et al. A method to estimate the accuracy of 1-D flow based permeability measuring devices
Becker et al. An experimental study of the influence of process parameters on the textile reaction to transverse impregnation

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
C17 Cessation of patent right
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20091028

Termination date: 20120515