CN108152198A - A kind of high throughput resin fibre micro interface Mechanics Performance Testing die device and method - Google Patents

A kind of high throughput resin fibre micro interface Mechanics Performance Testing die device and method Download PDF

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Publication number
CN108152198A
CN108152198A CN201711399067.7A CN201711399067A CN108152198A CN 108152198 A CN108152198 A CN 108152198A CN 201711399067 A CN201711399067 A CN 201711399067A CN 108152198 A CN108152198 A CN 108152198A
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monofilament
mold
fixing groove
resin
matrix resin
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陶杰
靳凯
王浩
王建华
陈虞杰
袁其炜
丁青云
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Nanjing University of Aeronautics and Astronautics
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Nanjing University of Aeronautics and Astronautics
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N19/00Investigating materials by mechanical methods
    • G01N19/04Measuring adhesive force between materials, e.g. of sealing tape, of coating

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
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  • General Physics & Mathematics (AREA)
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  • Pathology (AREA)
  • Investigating Strength Of Materials By Application Of Mechanical Stress (AREA)

Abstract

The invention discloses a kind of high-throughput resin fibre micro interface Mechanics Performance Testing die device and methods, the die device includes mold and die fixture, the mold is formed by processing a series of monofilament fixing groove of openings on the plank of one block of metal or other non-metallic materials, and monofilament and macromolecule matrix resin are put by the monofilament fixing groove;The monofilament fixing groove is rectangular channel, die fixture is wherein fixed for mold to be put into, its inside of die fixture is hollow, and monofilament locating slot is provided on the top of die fixture, and the position of monofilament locating slot is corresponding with the groove center of mold.The present invention helps to establish the component, structure and performance database of advanced polymer composite, for advanced polymer-based composite to be instructed to design, accelerates the innovation of advanced polymer-based composite by high-throughput experiment screening, shortens the period of research and development.

Description

A kind of high throughput resin fibre micro interface Mechanics Performance Testing die device and method
Technical field
The invention belongs to advanced polymer-based composite technical fields, and it is high to be related specifically to advanced polymer composite Flux prepares research and development and the Demonstration Application on aircraft of new generation and measures composite material micro-property structure database field.
Background technology
Advanced polymer-based composite is as current advanced material, in engineering fields such as Aeronautics and Astronautics, ship, high ferros Using more and more extensive.The effect of performance is more and more important, and higher requirement is proposed to the performance of material.For advanced high score Its performance of subbase composite material depends primarily on reinforcement fiber, resin matrix and fiber and resin boundary surface performance, wherein fiber Interfacial force between resin is most important.Pass through polymer-based base at interfacial force, also referred to as interfacial bond strength, i.e. fibrous fracture Body transmits the ability of stress to fiber, directly influences that the intensity, toughness and failure mode of composite material etc. is microcosmic, macromechanics Behavior.Therefore, the microscopic property at the interface between fiber and matrix phase how is characterized, to predicting material macro-mechanical performance, if Meter, control and optimization fibre reinforced composites performance provide experiment and theoretical foundation.
At present at home, people are not high to the fiber and resin micro interface various parameters degree of recognition that measure, even if sometimes It is that similary fiber and naval stores enterprise, the test data of user and testing agency are all not the same, many users is caused to make Do not know how to choose in, influenced evaluation, application and popularization of the China to fiber.
Domestic mainstream measures fiber and the method for resin boundary surface parameter, and for efficiency than relatively low, cost is also higher, it is believed that caused Data error is big, is typically that a mold prepares a monofilament sample respectively, once only measures one between monofilament and resin Interface parameter, it is impossible to meet the big data, high-throughput requirement that country advocates now and cannot be while measure interface parameter Microscopic appearance when accurate expression resin is separated with fiber interface, failure mechanism when analysis is extracted.
With the proposition and implementation of U.S. material genome plan in 2011, the high-throughput testing of materials and material number are combined According to the high-throughput material integral design method in library, the great attention of scientific circles and industrial quarters has been obtained.Advanced polymer-based multiple In the design and research and development of condensation material, using experiment and computer simulation method come the best composition of research material, structure and performance Relationship, the new material for meeting particular requirement is designed with reference to cloud database, and pass through high-throughput experiment screening, so as to pole The earth accelerates the innovation of advanced polymer-based composite, shortens the period of research and development.
It thus develops a kind of high-throughput resin fibre micro interface Mechanics Performance Testing die device and method is particularly heavy It will.
Invention content
The technical problems to be solved by the invention are " the material genome meter for overcoming drawbacks described above and the proposition of response country Draw " advanced polymer-based composite high throughput prepares research and development and its Demonstration Application on aircraft of new generation.It proposes a kind of high Flux resin fibre micro interface Mechanics Performance Testing die device and method:
A kind of high throughput resin fibre micro interface Mechanics Performance Testing die device, dress is fixed including mold and mold It puts, the mold is a series of monofilament fixing groove by processing openings on the plank of one block of metal or other non-metallic materials It is formed, monofilament and macromolecule matrix resin is put by the monofilament fixing groove;The monofilament fixing groove is rectangular channel, and mold is fixed Device is wherein fixed for mold to be put into, its inside of die fixture is hollow, and in the upper of die fixture Portion is provided with monofilament locating slot, and the position of monofilament locating slot is corresponding with the groove center of mold, and depth is mold groove depth Half ensure to be put into the center that monofilament after monofilament is located at mold, mold is put into die fixture to fixed, monofilament Locating slot faces the center of monofilament fixing groove, monofilament is put into monofilament locating slot, monofilament is placed exactly in mold at this time Sample is made after resin solidification is added in the monofilament fixing groove of mold in heart position.
The die device, the monofilament fixing groove are two rows.
The die device, the width of monofilament locating slot is 10-20um.
It is real according to the test method of any high-throughput resin fibre micro interface Mechanics Performance Testing die device It is as follows to test step:
Mold is put into die fixture fixed by the first step, assembly mold;By treated, carbon mono-filaments are put into In die fixture monofilament locating slot, monofilament is located at the center of mold, is put into sequence from left to right, piles successively;
Second step adds in surface of the macromolecule matrix resin package monofilament in monofilament fixing groove in monofilament fixing groove, Macromolecule matrix resin is full of monofilament fixing groove;
Third walks, and cures macromolecule matrix resin;After the monofilament fixing groove of mould upstream completes curing, mold is taken out, it will Mold lower part monofilament fixing groove is placed in die fixture upward, and repetition is above-mentioned to be put into monofilament and filling matrix resin, curing The step of;
4th step is being the position at L by monofilament and macromolecule matrix resin apart from macromolecule matrix resin one end length It cuts off together, is then eliminated with blade and be packed into the groove of monofilament and resin and the extra resin of mold solid object surface;
5th step, mold is fitted into draw-off gear, and with clamp monofilament, fixture applies monofilament pulling capacity, synchronous Obtain microscopic appearance picture of monofilament when being detached with matrix resin, be finally completed experiment, obtain test result, by test result and In microscopic appearance picture automated import of data library when monofilament is detached with matrix resin, high-throughput resin fibre micro interface is completed Mechanics Performance Testing.
The test method during third walks, cures 24 hours, cures 15 hours at a temperature of 60 DEG C at room temperature.
The test method, in the 5th step, the speed of drawing is set as 1um/s.
The test method, monofilament be A-42 monofilament carbon fibers, filament length 20mm, L length be 7mm, filament diameter For 7um.
The test method, the draw-off gear test system experimentation instrument, dress for microscopic fibers tensile strength There are 1x250gf load cells and 2x24-Bit USB analog-digital converters.
The beneficial effects of the present invention are:
1st, it can reduce and prepare monofilament and macromolecule matrix resin samples time, save material and time, can once make Standby up to 50 monofilament and resin test sample, complete to carry out interface performance test to 50 monofilament, and meeting high-throughput test will It asks, improves measurement efficiency and measurement accuracy, reduce the fluctuating error of artificial caused experimental data;
2nd, it accurately obtains microscopic appearance when multigroup resin is separated with fiber interface and data can be clearly right Than the interface performance for going out various advanced polymer-based composites, relationship and destruction mechanics between assay surface layer and structure It is significant, select the polymer-based composite of function admirable;
3rd, contribute to establish the component, structure and performance database of advanced polymer composite, for instructing advanced height Molecule based composite material designs, and accelerates the innovation of advanced polymer-based composite by high-throughput experiment screening, shortens and research and develop Period.
Description of the drawings
Fig. 1 high throughput resin fibre micro interface Mechanics Performance Testing molds;
Fig. 2 high throughput resin fibre micro interface Mechanics Performance Testing schematic diagrams;
Fig. 3 high throughput resin fibre micro interface Mechanics Performance Testing die fixture front views;
Fig. 4 high throughput resin fibre micro interface Mechanics Performance Testing die fixture vertical views;
In Fig. 2,1 matrix resin cut-off part, 2 monofilament, 3 macromolecule matrix resins, the diameter of d monofilament, F pulling force, 4 monofilament Locating slot, 5 monofilament fixing grooves.
Specific embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
High-throughput resin fibre micro interface Mechanics Performance Testing device includes mold and die fixture, the mold It is to be formed by processing a series of monofilament fixing groove 5 of openings on the plank of one block of metal or other non-metallic materials, passes through The monofilament fixing groove 5 is put into monofilament 2 and macromolecule matrix resin 3.The monofilament fixing groove 5 be rectangular channel, die fixture It is wherein fixed for mold to be put into, its inside of die fixture is hollow, and opened on the top of die fixture There is monofilament locating slot 4, the position of monofilament locating slot 4 is corresponding with the groove center of mold, and depth is mold groove depth Half ensures to be put into the center that monofilament after monofilament is located at mold, mold is put into die fixture fixed, and monofilament is fixed Position slot 4 faces the center of monofilament fixing groove, monofilament is put into monofilament locating slot 4, monofilament 2 is placed exactly in mold at this time Sample is made after resin solidification is added in the monofilament fixing groove 5 of mold in heart position.
Embodiment 1
After studying nitric acid and sulfuric acid mixing, carbon fiber surface is handled with mixed acid solution, to enhance carbon fibre Adhesion strength between dimension and resin, mixed acid solution Treatment of Carbon surface Best Times need experimental verification.Experiment material: PAN base AKSAca A-42 carbon fibers, density 1.78g/cm3, a diameter of 7um of individual thread;EPR-L20 epoxy resin.Choose length 40, the monofilament A-42 carbon fibers of 20mm are spent, is put into mixed acid and handles, processing time is 15 minutes to 60 minutes, is divided into 15 Minute, 10 per treatment, by treated, carbon fiber clear water rinses surface, and it is 7 to reach surface PH.Specific experiment step is such as Under:
Mold is put into die fixture fixed by the first step, assembly mold;With reference to figure 1,2,3,4, by treated Carbon mono-filaments are put into die fixture monofilament locating slot 4, and monofilament 2 is placed exactly in the center of mold at this time, is put into Sequence from left to right, is piled successively;
Second step with reference to figure 1,2,3,4, EPR-L20 epoxy resin is added in monofilament fixing groove 5 and wraps up monofilament in monofilament Surface in fixing groove 5, macromolecule matrix resin are full of monofilament fixing groove 5;
Third walks, and cures 24 hours at room temperature, cures 15 hours at a temperature of 60 DEG C;The monofilament fixing groove of mould upstream After 5 curings, mold is taken out, mold lower part monofilament fixing groove 5 is placed in die fixture upward, repetition is above-mentioned to be put into monofilament The step of with filling matrix resin, curing.
4th step with reference to figure 2, cuts monofilament and resin for 1 position of matrix resin cut-off part at 7mm in L length together It is disconnected, it is then eliminated with blade and is packed into the groove of monofilament and resin and the extra resin of mold solid object surface;
5th step, mold is fitted into draw-off gear, and with clamp monofilament 2, fixture applies pulling capacity, drawing to monofilament Speed be set as 1um/s, the synchronous microscopic appearance picture obtained when monofilament is detached with matrix resin is finally completed experiment, obtains Go out test result, it is complete in microscopic appearance picture automated import of data library when test result and monofilament are detached with matrix resin Into high-throughput resin fibre micro interface Mechanics Performance Testing, comparison obtains best sour processing time, is handled when with mixed acid When 15min, resin matrix has good bond strength with carbon fiber, and all tests once can be completed, largely save Make an appointment and improve testing efficiency.
Embodiment 2
Bond strength between the carbon fiber and resin that are not modified with original surface after research carbon fiber surface modification.Experiment Material:Surface is modified to contain NH2The A-42 monofilament carbon fibers of functional group, length 20mm, diameter 7um, quantity 20;Surface There is no any chemically treated A-42 monofilament carbon fiber, length 20mm, diameter 7um, quantity 20;EPR-L20 epoxy resin.
Mold is put into die fixture fixed by the first step, assembly mold;With reference to figure 1,2,3,4, by table after processing Face is modified to contain NH2The A-42 monofilament carbon fiber of functional group and surface do not have any chemically treated A-42 monofilament carbon fiber to put Enter in die fixture monofilament locating slot, be put into sequence and from left to right pile successively;
Second step with reference to figure 1,2,3,4, EPR-L20 epoxy resin package monofilament is added in mold groove and is consolidated in monofilament Determine the surface in slot 5, macromolecule matrix resin is full of monofilament fixing groove 5;
Third walks, and cures 24 hours at room temperature, cures 15 hours at a temperature of 60 DEG C;The monofilament fixing groove of mould upstream After 5 curings, mold is taken out, mold lower part monofilament fixing groove 5 is placed in die fixture upward, repetition is above-mentioned to be put into monofilament The step of with filling matrix resin, curing.
4th step with reference to figure 2, cuts monofilament and resin for 1 position of matrix resin cut-off part at 7mm in L length together It is disconnected, it is then eliminated with blade and is packed into the groove of monofilament and resin and the extra resin of mold solid object surface;
5th step, mold is fitted into draw-off gear, and with clamp monofilament 2, fixture applies pulling capacity, drawing to monofilament Speed be set as 1um/s, the synchronous microscopic appearance picture obtained when monofilament is detached with matrix resin is finally completed experiment, obtains Go out test result, it is complete in microscopic appearance picture automated import of data library when test result and monofilament are detached with matrix resin Into high-throughput resin fibre micro interface Mechanics Performance Testing, comparison obtains, NH is contained after carbon fiber surface modification2Functional group All tests of bond strength between resin can be increased, once can be completed, the time is largely saved and improve and test Efficiency.
Embodiment 3
Research is chemically treated carbon fiber surface, and surface obtains different types of functional group, compares which kind of functional group It is most advantageous to the bond strength for improving carbon fiber and resin boundary surface.Experiment material:A-42 containing OH functional groups after surface treatment Monofilament carbon fiber, length 20mm, diameter 7um, quantity are 10;The A-42 monofilament carbon containing CO functional groups is fine after surface treatment Dimension, length 20mm, diameter 7um, quantity are 10;A-42 monofilament carbon fibers containing COOH functional groups, length after surface treatment 20mm, diameter 7um, quantity are 10;EPR-L20 epoxy resin.
Mold is put into die fixture fixed by the first step, assembly mold;With reference to figure 1,2,3,4, respectively by surface The modified A-42 monofilament carbon fibers containing OH, CO, COOH functional group are sequentially placed into die fixture monofilament locating slot, are put Enter sequence from left to right, pile successively;
Second step with reference to figure 1,2,3,4, EPR-L20 epoxy resin package monofilament is added in mold groove and is consolidated in monofilament Determine the surface in slot 5, macromolecule matrix resin is full of monofilament fixing groove 5;
Third walks, and cures 24 hours at room temperature, cures 15 hours at a temperature of 60 DEG C;The monofilament fixing groove of mould upstream After 5 curings, mold is taken out, mold lower part monofilament fixing groove 5 is placed in die fixture upward, repetition is above-mentioned to be put into monofilament The step of with filling matrix resin, curing.
4th step with reference to figure 2, cuts monofilament and resin for 1 position of matrix resin cut-off part at 7mm in L length together It is disconnected, it is then eliminated with blade and is packed into the groove of monofilament and resin and the extra resin of mold solid object surface;
5th step, mold is fitted into draw-off gear, and with clamp monofilament 2, fixture applies pulling capacity, drawing to monofilament Speed be set as 1um/s, the synchronous microscopic appearance picture obtained when monofilament is detached with matrix resin is finally completed experiment, obtains Go out test result, in microscopic appearance picture automated import of data library when test result and monofilament are detached with matrix, complete high Flux resin fibre micro interface Mechanics Performance Testing, comparison obtain, OH, CO, COOH official are contained after carbon fiber surface modification In rolling into a ball, bond strength most favorably all tests of the COOH functional groups to raising carbon fiber and resin boundary surface once can be completed, It largely saves the time and improves testing efficiency.
It should be understood that for those of ordinary skills, can be improved or converted according to the above description, And all these modifications and variations should all belong to the protection domain of appended claims of the present invention.

Claims (8)

1. a kind of high throughput resin fibre micro interface Mechanics Performance Testing die device, which is characterized in that including mold and mould Has fixing device, the mold is a series of list by processing openings on the plank of one block of metal or other non-metallic materials Silk fixing groove is formed, and monofilament and macromolecule matrix resin are put by the monofilament fixing groove;The monofilament fixing groove is rectangular channel, Die fixture is wherein fixed for mold to be put into, its inside of die fixture is hollow, and fixed in mold The top of device is provided with monofilament locating slot, and the position of monofilament locating slot is corresponding with the groove center of mold, and depth is mold The half of depth of groove ensures to be put into the center that monofilament after monofilament is located at mold, mold is put into die fixture solid Fixed, monofilament locating slot faces the center of monofilament fixing groove, monofilament is put into monofilament locating slot, monofilament is placed exactly in mould at this time Sample is made after resin solidification is added in the monofilament fixing groove of mold in the center of tool.
2. die device according to claim 1, which is characterized in that the monofilament fixing groove is two rows.
3. die device according to claim 1, which is characterized in that the width of monofilament locating slot is 10-20um.
4. according to the survey of any high-throughput resin fibre micro interface Mechanics Performance Testing die devices of claim 1-3 Method for testing, which is characterized in that experimental procedure is as follows:
Mold is put into die fixture fixed by the first step, assembly mold;By treated, carbon mono-filaments are put into mold In fixing device monofilament locating slot, monofilament is located at the center of mold, is put into sequence from left to right, piles successively;
Second step adds in surface of the macromolecule matrix resin package monofilament in monofilament fixing groove, high score in monofilament fixing groove Sub- matrix resin is full of monofilament fixing groove;
Third walks, and cures macromolecule matrix resin;After the monofilament fixing groove of mould upstream completes curing, mold is taken out, by mold Lower part monofilament fixing groove is placed in die fixture upward, and repetition is above-mentioned to be put into monofilament and filling matrix resin, cured step Suddenly;
4th step, apart from macromolecule matrix resin one end length for the position at L by monofilament and macromolecule matrix resin together Then cut-out is eliminated with blade and is packed into the groove of monofilament and resin and the extra resin of mold solid object surface;
5th step, mold is fitted into draw-off gear, and with clamp monofilament, fixture applies monofilament pulling capacity, synchronous to obtain Microscopic appearance picture when monofilament is detached with matrix resin, is finally completed experiment, obtains test result, by test result and monofilament In microscopic appearance picture automated import of data library when being detached with matrix resin, high-throughput resin fibre micro interface mechanics is completed Performance test.
5. test method according to claim 4, which is characterized in that in third step, cure 24 hours at room temperature, 60 Cure 15 hours at a temperature of DEG C.
6. test method according to claim 4, which is characterized in that in the 5th step, the speed of drawing is set as 1um/s.
7. test method according to claim 4, which is characterized in that monofilament be A-42 monofilament carbon fibers, filament length 20mm, L length are 7mm, filament diameter 7um.
8. test method according to claim 4, which is characterized in that the draw-off gear is microscopic fibers tensile strength System experimentation instrument is tested, 1x250gf load cells and 2x24-Bit USB analog-digital converters are housed.
CN201711399067.7A 2017-12-22 2017-12-22 A kind of high throughput resin fibre micro interface Mechanics Performance Testing die device and method Pending CN108152198A (en)

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Application publication date: 20180612