CN109883853A - High throughput test fiber and resin micro interface performance Thermal-mechanical Coupling device and method - Google Patents
High throughput test fiber and resin micro interface performance Thermal-mechanical Coupling device and method Download PDFInfo
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- CN109883853A CN109883853A CN201910001817.3A CN201910001817A CN109883853A CN 109883853 A CN109883853 A CN 109883853A CN 201910001817 A CN201910001817 A CN 201910001817A CN 109883853 A CN109883853 A CN 109883853A
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Abstract
The invention discloses a kind of high-throughput test fiber and resin micro interface performance Thermal-mechanical Coupling devices, belong to advanced polymer-based composite technology fields of measurement, the present invention is by by the inside of the installation of TC Yu Weijian unsticking experimental provision, it is connected with signal amplifier, the output end of signal amplifier is connected to terminal plate, terminal plate is connected with data acquisition card, the output end of data acquisition card is connected with temperature integrated manipulator, temperature integrated manipulator is connected to the input terminal of signal output card, output is terminated at the middle part of terminal plate, the upper and lower input terminal for being terminated at relay of terminal plate, one end of output end of relay is connected to nichrome heater, one end is connected to power cathode, nichrome is another to be terminated at positive pole；Can learn that steady temperature or step temperature variation whether there is interfacial force using the method for the device influences, and is more in line with the application of advanced polymer-based composite in practice.
Description
Technical field
The present invention relates to advanced polymer-based composite technology fields of measurement, in particular to a kind of to act in Thermal-mechanical Coupling
Under the conditions of high-throughput test fiber and resin micro interface mechanical property device and method.
Background technique
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 industry 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 in conjunction with cloud database, and by high-throughput experiment screening, thus pole
The earth accelerates the innovation of advanced polymer-based composite, shortens the period of research and development.By known reliable experimental data, with reason
It goes to attempt true or unknown material as much as possible by simulation, establishes its component, the database of structure and various physical property passes through number
Material component is sought according to excavation, the relation schema between structure and performance, for instructing advanced polymer-based composite to design.
Characterization most important for advanced polymer-based composite performance is exactly interfacial force.Interfacial force, also referred to as interface
Adhesive strength is transmitted the ability of stress to fiber by polymer-based matrix, directly influences composite material that is, at fibrous fracture
Intensity, toughness and microcosmic, the macromechanics behavior such as failure mode.Therefore, the boundary between fiber and macromolecule matrix how is characterized
The microscopic property in face, to prediction material macro-mechanical performance, design, control and optimization fibre reinforced composites performance provide real
It tests and theoretical basis.
It is that microbond test is i.e. micro- that the world, which measures the main method of advanced polymer-based composite interfacial force, at present
The experiment of key unsticking.But existing micro- key unsticking experiment is to carry out the test of interfacial force to sample at normal temperature.And advanced
In the application field of polymer-based composite, the service condition of composite material usually can be under hot conditions, then in height
Whether the interfacial force measured under the conditions of the temperature of room temperature is same with normal temperature phase, or has He Bianhua, this research is for elder generation
Application into high score based composites in aerospace field has very important significance with regard to tool, therefore in the temperature strip for being higher than room temperature
Measuring under part to interfacial force is just particularly important.
A kind of high-throughput test fiber is thus developed just to show with resin micro interface performance Thermal-mechanical Coupling device and method
It obtains particularly important.
Summary of the invention
It is only capable of measuring under room temperature on the basis of interfacial force for the device of the micro- key unsticking experiment of existing test, the present invention increases
Add heating device, measures interfacial force under Thermal-mechanical Coupling action condition to consider；Also with the side of the device of the invention
Method is that heating obtained under the same material same time to multiple groups sample while respectively, and the interface under different Thermal-mechanical Couplings effects is strong
Degree, accelerates the efficiency of experiment screening and ensure that accuracy.
The present invention is implemented as follows:
A kind of high-throughput test fiber and resin micro interface performance Thermal-mechanical Coupling device, which is characterized in that the device packet
Thermocouple is included, the thermocouple includes the thermode of two unlike materials, and the thermode by being welded to connect, close by composition
Close circuit；The thermode is coated with insulating protective sleeve, and the thermocouple end is provided with terminal box, the thermoelectricity
Even to be connect by terminal box with signal amplifier input terminal, the signal amplifier output end is connect with terminal plate；Signal is adopted
Truck is not connected directly with signal amplifier, but passes through terminal plate indirect transfer signal, the positive and negative anodes point of signal amplifier
It is not connected to the upper and lower side of terminal plate, signal acquisition is connected in the middle part of terminal plate；The device further includes relay, described
The input terminal of relay is indirectly connected by terminal plate and signal output card, and there are two branches for the output end of the relay
End, one are terminated at power cathode, and the other end is connected to nichrome heater；Described nichrome heater one end with after
Electric appliance is connected, another to be terminated at positive pole；The integrated control of temperature is connected between the data acquisition card and signal output card
Device processed.
Further, the signal amplifier includes NPN type silicon triode, is provided with and is connect with thermocouple end by conducting wire
Wire box is connected.
Further, the temperature integrated manipulator includes DI intelligent industrial adjuster, chip of micro-computer, using height
Flux concurrent system is connected by USB end interface with data acquisition card and signal output card.
Further, the relay includes electromagnetic system, time-delay mechanism and contact.
Further, the thermocouple and nichrome heater are located at the inside of micro- key unsticking experimental provision, by resistance to
High temp glass is isolated from the outside world；Micro- key unsticking experimental provision includes mold and die fixture.
Further, the inside of the nichrome heater base and micro- key unsticking experimental provision is equipped with cooling system
System, to guarantee the safety of experiment condition and equipment.
Further, the data acquisition card includes single-ended 32 road I/O board, A/D chip and FIFO.
The invention also discloses the method for a kind of high-throughput test fiber and resin micro interface performance Thermal-mechanical Coupling device,
It is characterized in that, specific step is as follows:
The first step assembles each component: by the inside of the installation of TC Yu Weijian unsticking experimental provision, by the wiring of thermocouple end
Box is connected with the input terminal of signal amplifier, and the output end of signal amplifier draws the upper and lower side that positive and negative anodes are connected to terminal plate,
The central port of terminal plate is connected to the input terminal of data acquisition card, and the output end of data acquisition card passes through USB interface and temperature collection
It is connected at controller, another USB interface of temperature integrated manipulator is connected to the input terminal of signal output card；The signal is defeated
Card release exports the middle part for being terminated at terminal plate, the upper and lower input terminal for being terminated at relay of terminal plate, the output end one of relay
It is terminated at nichrome heater, an end is connected to power cathode, and nichrome heater is another to be terminated at positive pole；
Second step, is packed into the monfil of several attached cured epoxy resin drops of drop in micro- key unsticking experimental provision, and two
End is fixed；
Third step, the heating device first respectively heat several groups experimental situation, pass through micro- key after reaching set temperature
Unsticking experimental provision applies load, cutter gradually cutting resin, measures boundary strength under the collective effect of power and heat, final
The size of interfacial force under to Thermal-mechanical Coupling action condition.
Further, in the second step, the monfil of 40 attached cured epoxy resin drops of drop, 40 rings are packed into
Oxygen resin liquid drop is respectively divided into 8 assemblings key unsticking experimental provision in a subtle way, and epoxy resin drop solidifies at 80 DEG C, to 5 groups of realities
Environment is tested to be heated；The length that Thermal-mechanical Coupling acts on the monfil that lower high throughput prepares resin droplet is generally 5-7mm.
Further, micro- key unsticking experimental provision is microscopic fibers tensile strength test macro laboratory apparatus, dress
There are 1 × 250gf load cell and 2 × 24-Bit USB analog-digital converter.
The beneficial effects of the present invention are:
1, the device of the invention can not only measure interfacial force at normal temperature, but also can measure boundary under the collective effect of load and heat
The size of face power, can learn that steady temperature or step temperature variation whether there is interfacial force influences, and is more in line with
The application of advanced polymer-based composite in practice；
2, heating device can simultaneously heat the multiple groups sample (up to 40 groups) in micro- adhering device, comparative strong, sieve
Select accuracy that is high-efficient, and ensuring experimental data；Temperature integrated manipulator is using high-throughput concurrent system, efficiently, quasi-
Really, high-throughput characteristic has been fully demonstrated；
3, the component, structure and performance database for facilitating to enrich advanced polymer composite, for instructing advanced macromolecule
Based composites design accelerates the innovation of advanced polymer-based composite by high-throughput experiment screening, shortens the week of research and development
Phase.
Detailed description of the invention
Fig. 1 is the schematic diagram of temperature measuring equipment thermocouple in the present invention；
Fig. 2 is the schematic illustration of signal amplifier in the present invention；
Fig. 3 is that micro- key unsticking tests schematic diagram in the present invention；
Fig. 4 is Thermal-mechanical Coupling schematic device in the present invention；
Wherein, 1- terminal box, 2- insulating protective sleeve, 3- thermode, 4- cutter, 5- epoxy resin drop, 6- monfil, 7- are micro-
Key unsticking experimental provision, 8- thermocouple, 9- signal amplifier, 10- terminal plate, 11- data acquisition card, 12- temperature integrated control
Device, 13- signal output card, 14- relay, 15- nichrome heater.
Specific embodiment
It is clear to keep the purpose of the present invention, technical solution and effect clearer, example is exemplified below to the present invention into one
Step is described in detail.It should be understood that specific implementation described herein is not intended to limit the present invention only to explain the present invention.
As shown in Fig. 1 ~ 4, the inventive system comprises thermocouple 8, signal amplifier 9, terminal plates 10, data acquisition card
11, temperature integrated manipulator 12, signal output card 13, relay 14, nichrome heater 15 and micro- key unsticking experimental provision,
The thermocouple 8 includes thermode 3, insulating protective sleeve 2 and the terminal box 1 of two unlike materials, and two thermodes pass through welding
It connects, constitutes closed circuit, insulating protective sleeve is respectively fitted on two thermodes, and two contacts of thermode 3 is avoided to be formed
Short circuit, terminal box 1 are located at the end of thermocouple 8 to connect with signal amplifier 9；The signal amplifier 9 includes NPN type silicon three
Pole pipe is connected by conducting wire with the terminal box 1 of 8 end of thermocouple；The data acquisition card 11 includes single-ended 32 road I/O plate
Card, A/D chip and FIFO.Data acquisition card 12 is not connected directly with signal amplifier 9, but indirect by terminal plate 10
Signal is transmitted, the positive and negative anodes of signal amplifier 9 are connected to the upper and lower side of terminal plate 10 respectively, and data acquisition card 11 is connected to terminal plate 10
Middle part
Temperature integrated manipulator 12 includes DI intelligent industrial adjuster, chip of micro-computer, using high-throughput concurrent system
System, is connected by USB end interface with data acquisition card 11 and signal output card 13；The relay 14 includes electromagnetic system, prolongs
When mechanism and contact, input terminal is indirectly connected by terminal plate 10 with signal output card 13, and one end of output end is connected to power cathode,
One end is connected to nichrome heater 15；Described 15 one end of nichrome heater is connected with relay 14, and an end is connected to power supply
Anode；Micro- key unsticking experimental provision includes mold and die fixture.
Using shown in the following specific embodiment of the method for apparatus of the present invention.
Embodiment 1
Study boundary strength at different temperatures between surface size and the carbon fiber and resin of not starching.
Experimental material: the modified polyacrylonitrile-radical T800 monofilament carbon fiber in the surface aqueous sizing agent DGEBA-MDI-TX-100
Dimension, diameter 6um, length 6mm, density 1.78g/cm3, quantity 20；Unmodified similar monofilament carbon fiber, diameter 6um, length
6mm, density 1.78g/cm3, quantity 20；E54 bisphenol A type epoxy resin.Steps are as follows for specific experiment:
Step 1: assembling heating device is divided into 4 assemblings for 20, monofilament carbon fiber that use sizing agent surface modified with reference to Fig. 4
In a subtle way in key debonding device, both ends are fixed；It is divided into 4 assemblings key debonding device in a subtle way for surface unmodified 20, monofilament carbon fiber
In, both ends are fixed.
It is numbered step 2: modified to surface with unmodified 8 groups of monofilament carbon fibers, each group heating temperature is implemented such as
Under: under first group of the monofilament carbon fiber modified experimental situation in room temperature of surface；Second group under 50 DEG C of experimental situation；
Third group is under 100 DEG C of experimental situation；4th group under 150 DEG C of experimental situation.The modified monofilament carbon fiber in non-surface
The 5-8 group of dimension is using experimental situation identical with the modified monofilament carbon fiber in surface.
Step 3: heating device simultaneously heats 8 groups of experimental situations, after reaching set temperature, pass through micro- key unsticking
Experimental provision applies load, and cutter gradually cutting resin completes the measurement to interfacial force under the collective effect of power and heat.
Embodiment 2
Study boundary strength at different temperatures between the carbon fiber and resin under the different surfaces acid processing time.
Experimental material: the polyacrylonitrile-radical T800 monofilament carbon fiber of nitric acid surface treatment, acid processing time 15min, diameter
6um, length 6mm, density 1.78g/cm3, quantity 20；The polyacrylonitrile-radical T800 monofilament carbon fiber of nitric acid surface treatment, acid
Handle time 30min, diameter 6um, length 6mm, density 1.78g/cm3, quantity 20.E54 bisphenol A type epoxy resin.
Step 1: the acid processing time is divided into 4 with reference to Fig. 4 for 20, monofilament carbon fiber of 15min by assembling heating device
In assembling key debonding device in a subtle way, both ends are fixed；It is 20, monofilament carbon fiber of 30min for the acid processing time to be divided into 4 and be assembled into
In micro- key debonding device, both ends are fixed.
Step 2: 8 groups of monofilament carbon fibers under the different acid processing times are numbered, each group heating temperature is implemented such as
Under: under first group of the monofilament carbon fiber experimental situation in room temperature that the acid processing time is 15min；Second group is in 50 DEG C of reality
It tests under environment；Third group is under 100 DEG C of experimental situation；4th group under 150 DEG C of experimental situation.Remaining 5-8 group is adopted
Experimental situation identical with the monofilament carbon fiber for being 15min with the acid processing time.
Step 3: heating device simultaneously heats 8 groups of experimental situations, after reaching set temperature, pass through micro- key unsticking
Experimental provision applies load, and cutter gradually cutting resin completes the measurement to interfacial force under the collective effect of power and heat.
Embodiment 3
Research surface obtains the boundary strength between the carbon fiber of different functional groups and resin at different temperatures.
Experimental material: anodized rear surface has the polyacrylonitrile-radical T800 of hydrophily oxygen-containing functional group hydroxyl OH
Carbon fiber, diameter 6um, length 6mm, density 1.78g/cm3, quantity 20；Plasma oxidation handles rear surface with hydrophilic
The polyacrylonitrile-radical T800 carbon fiber of property oxygen-containing functional group carboxyl, diameter 6um, length 6mm, density 1.78g/cm3, quantity 20
Root.E54 bisphenol A type epoxy resin.
Step 1: assembling heating device, with reference to Fig. 4, by hydroxyl OH is contained on surface, 20, monofilament carbon fiber are divided into 4 assemblings
In a subtle way in key debonding device, both ends are fixed；By carboxy CO OH is contained on surface, 20, monofilament carbon fiber are divided into 4 assemblings key in a subtle way and take off
In viscous device, both ends are fixed.
Step 2: 8 groups of monofilament carbon fibers that hydroxyl OH and carboxy CO OH is contained on surface are numbered, each group heating temperature
Implement as follows: under first group of the monofilament carbon fiber experimental situation in room temperature that hydroxyl OH is contained on surface；Second group is in 50 DEG C
Experimental situation under；Third group is under 100 DEG C of experimental situation；4th group under 150 DEG C of experimental situation.Contain on surface
The 5-8 group of the monofilament carbon fiber of carboxy CO OH contains the identical experimental situation of the monofilament carbon fiber of hydroxyl OH using with surface.
Step 3: heating device simultaneously heats 8 groups of experimental situations, after reaching set temperature, pass through micro- key unsticking
Experimental provision applies load, and cutter gradually cutting resin completes the measurement to interfacial force under the collective effect of power and heat.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the principle of the present invention, several improvement can also be made, these improvement also should be regarded as of the invention
Protection scope.
Claims (10)
1. a kind of high-throughput test fiber and resin micro interface performance Thermal-mechanical Coupling device, which is characterized in that the device
Including thermocouple (8), the thermocouple (8) includes the thermode (3) of two unlike materials, and the thermode (3) passes through
It is welded to connect, constitutes closed circuit；The thermode (3) is coated with insulating protective sleeve (2), the thermocouple (8) end
Portion is provided with terminal box (1), and the thermocouple (8) is connect by terminal box (1) with signal amplifier (9) input terminal, described
Signal amplifier (9) output end connect with terminal plate (10)；Data acquisition card (11) and the not direct phase of signal amplifier (9)
Even, but by terminal plate (10) indirect transfer signal, the positive and negative anodes of signal amplifier (9) are connected to the upper of terminal plate (10) respectively
Lower end, data acquisition card (11) are connected to the middle part of terminal plate (10)；
The device further includes relay (14), and the input terminal of the relay (14) is defeated by terminal plate (10) and signal
Card release (13) is indirectly connected, and there are two branch ends for the output end of the relay (14), and one is terminated at power cathode, another
End is connected to nichrome heater (15)；Described nichrome heater (15) one end is connected with relay (14), another
It is terminated at positive pole；
Temperature integrated manipulator (12) are connected between the data acquisition card (11) and signal output card (13).
2. a kind of high-throughput test fiber according to claim 1 and resin micro interface performance Thermal-mechanical Coupling device,
It is characterized in that, the signal amplifier (9) includes NPN type silicon triode, is provided with and is connect with thermocouple (8) end by conducting wire
Wire box (1) is connected.
3. a kind of high-throughput test fiber according to claim 1 and resin micro interface performance Thermal-mechanical Coupling device,
It is characterized in that, the temperature integrated manipulator (12) includes DI intelligent industrial adjuster, chip of micro-computer, using high pass
Concurrent system is measured, is connected by USB end interface with data acquisition card (11) and signal output card (13).
4. a kind of high-throughput test fiber according to claim 1 and resin micro interface performance Thermal-mechanical Coupling device,
It is characterized in that, the relay (14) includes electromagnetic system, time-delay mechanism and contact.
5. a kind of high-throughput test fiber according to claim 1 and resin micro interface performance Thermal-mechanical Coupling device,
It is characterized in that, the thermocouple (8) is located at the inside of micro- key unsticking experimental provision with nichrome heater (15), by resistance to
High temp glass is isolated from the outside world；Micro- key unsticking experimental provision includes mold and die fixture.
6. a kind of high-throughput test fiber according to claim 5 and resin micro interface performance Thermal-mechanical Coupling device,
It is characterized in that, the inside of nichrome heater (15) bottom and micro- key unsticking experimental provision is equipped with cooling system.
7. a kind of high-throughput test fiber according to claim 1 and resin micro interface performance Thermal-mechanical Coupling device,
It is characterized in that, the data acquisition card (11) includes single-ended 32 road I/O board, A/D chip and FIFO.
8. a kind of any high-throughput test fiber is attached together with resin micro interface performance thermo-mechanical Coupled according to claim 1 ~ 7
The method set, which is characterized in that specific step is as follows:
The first step, each component of assembling: thermocouple (8) is installed on to the inside of micro- key unsticking experimental provision, by thermocouple (8) end
Terminal box (1) be connected with the input terminal of signal amplifier (9), the output end of signal amplifier (9) is drawn positive and negative anodes and is connected to
The central port of the upper and lower side of terminal plate (10), terminal plate (10) is connected to the input terminal of data acquisition card (11), data acquisition card
(11) output end is connected by USB interface with temperature integrated manipulator (12), another USB of temperature integrated manipulator (12)
Interface is connected to the input terminal of signal output card (13)；Signal output card (13) output is terminated in terminal plate (10)
Portion, the upper and lower input terminal for being terminated at relay (14) of terminal plate (10), one end of output end of relay (14) are connected to nickel chromium triangle conjunction
Golden heater (15), an end are connected to power cathode, and nichrome heater (15) is another to be terminated at positive pole；
Second step, the monfil (6) of the attached cured epoxy resin drop (5) of loading drop in micro- key unsticking experimental provision, two
End is fixed；
Third step, the heating device first respectively heat different groups of experimental situations, pass through micro- key after reaching set temperature
Unsticking experimental provision applies load, and cutter (4) gradually cutting resin measures boundary strength under the collective effect of power and heat, most
The size of interfacial force under Thermal-mechanical Coupling action condition is obtained eventually.
9. the side of a kind of high-throughput test fiber and resin micro interface performance Thermal-mechanical Coupling device according to claim 8
Method, which is characterized in that in the second step, be packed into the monfil of 40 attached cured epoxy resin drops of drop, 40 rings
Oxygen resin liquid drop is respectively divided into 8 assemblings key unsticking experimental provision in a subtle way, and epoxy resin drop solidifies at 80 DEG C, to 5 groups of realities
Environment is tested to be heated；The length that Thermal-mechanical Coupling acts on the monfil (6) that lower high throughput prepares resin droplet is 5-7mm.
10. a kind of high-throughput test fiber according to claim 8 and resin micro interface performance Thermal-mechanical Coupling device
Method, which is characterized in that micro- key unsticking experimental provision is microscopic fibers tensile strength test macro laboratory apparatus, dress
There are 1 × 250gf load cell and 2 × 24-Bit USB analog-digital converter.
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| CN114486525A (en) * | 2022-01-25 | 2022-05-13 | 南京航空航天大学 | Fiber monofilament force resistance response online testing device and testing method |
| CN114486525B (en) * | 2022-01-25 | 2024-05-17 | 南京航空航天大学 | Online testing device and testing method for force resistance response of fiber monofilaments |
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