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CN107099107B - A kind of preparation method of the two-dimensional orientation anisotropic composite material of fibre filling polytetrafluoroethyland - Google Patents

A kind of preparation method of the two-dimensional orientation anisotropic composite material of fibre filling polytetrafluoroethyland Download PDF

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Publication number
CN107099107B
CN107099107B CN201710431537.7A CN201710431537A CN107099107B CN 107099107 B CN107099107 B CN 107099107B CN 201710431537 A CN201710431537 A CN 201710431537A CN 107099107 B CN107099107 B CN 107099107B
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China
Prior art keywords
fiber
preparation
composite material
dimensional orientation
fibre filling
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Expired - Fee Related
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CN201710431537.7A
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Chinese (zh)
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CN107099107A (en
Inventor
丁庆军
王星
赵盖
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Nanjing University of Aeronautics and Astronautics
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Nanjing University of Aeronautics and Astronautics
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/04Ingredients treated with organic substances
    • C08K9/06Ingredients treated with organic substances with silicon-containing compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00Use of ingredients characterised by shape
    • C08K7/02Fibres or whiskers
    • C08K7/04Fibres or whiskers inorganic
    • C08K7/06Elements
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L27/00Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
    • C08L27/02Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L27/12Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • C08L27/18Homopolymers or copolymers or tetrafluoroethene
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/001Conductive additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/14Polymer mixtures characterised by other features containing polymeric additives characterised by shape
    • C08L2205/16Fibres; Fibrils

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Casting Or Compression Moulding Of Plastics Or The Like (AREA)

Abstract

The invention discloses a kind of preparation methods of the two-dimensional orientation anisotropic composite material of fibre filling polytetrafluoroethyland, it is related to material machine-shaping field, the ptfe composite that fiber is orientated to a high degree in the plane perpendicular to compression aspect can be made.The present invention is on the basis of the method for tradition preparation, and change cold moudling process, including following operating procedure: (1) bat wool is surface-treated;(2) fiber and polytetrafluoroethylene powder are uniformly mixed;(3) cold moudling is carried out in a mold, is repeatedly fed in batches;(4) it is sintered in sintering furnace by certain sintering degree.That the processing is simple is easy by the present invention, has a extensive future.

Description

A kind of system of the two-dimensional orientation anisotropic composite material of fibre filling polytetrafluoroethyland Preparation Method
Technical field
The invention belongs to material material molding technology fields more particularly to a kind of two dimension of fibre filling polytetrafluoroethyland to take To the preparation method of anisotropic composite material.
Background technique
The characteristic of composite material depends on the micro-structure of its matrix, the performance of filler and their formation.Macromolecule is compound In material binary system, if wherein a phase (for example, thermal conductivity high a phase) is evenly dispersed but without any orientation, opposite The promotion of thermal conductivity is very limited under low filer content.When filer content is very high, ideal conductive and heat-conductive can achieve Rate, but the good characteristic to lose macromolecule itself and raising cost is costs.However one hand down hot-fluid when thermal conductivity is high Direction is parallel and forms perforative structure, and thermal conductivity can be promoted significantly.Therefore, this anisotropic structure is to reduce filler Content but a kind of effective ways for assigning polymer filler function.The ptfe composite of fiber filling is in many fields It is all widely used, but what is applied at present is all the composite material made of common cold pressing, sintering process, is all each To the same sex, the effectiveness of functional stuffing can not be played to the greatest extent.
Summary of the invention
The present invention provides a kind of preparation sides of the two-dimensional orientation anisotropic composite material of fibre filling polytetrafluoroethyland Method improves the cold moudling process of classical ptfe composite preparation method, can prepare to a certain degree The anisotropic ptfe composite of two-dimensional orientation, it is different according to the characteristic of fiber, can be improved in some plane Or wearability, electric conductivity, thermal conductivity, mechanical property on certain directions etc..
In order to achieve the above objectives, the present invention adopts the following technical scheme:
A kind of preparation method of the two-dimensional orientation anisotropic composite material of fibre filling polytetrafluoroethyland, including following behaviour Make step:
A. fiber is surface-treated;
B. treated fiber and polytetrafluoroethylene powder are uniformly mixed, and obtain the mixture of fiber and polytetrafluoroethylene (PTFE);
C. fiber and teflon mixture are subjected to cold moudling in a mold, repeatedly fed in batches, every time It is once pressurizeed after charging, after for the last time adding material, pressure is added to the value of process stipulation, and keep pressure;
D. it is sintered in sintering furnace.
Fiber described in above step is staple fiber;Fiber described in step b and polytetrafluoroethylene (PTFE) press the volume of fiber Percentage is uniformly mixed for 5%-35%;Each feeding quantity described in step c makes thick flake thickness degree after pressurization increase 2-5 millimeters, The pressure value pressurizeed after charging every time is 5-8MPa, and the dwell time is not less than 5 seconds, the pressure process specified value of last time pressurization For 15-40MPa, the dwell time is not less than 10 minutes.
The beneficial effects of the invention are as follows preparing the anisotropic ptfe composite of a degree of two-dimensional orientation, It is different according to the characteristic of fiber, it can be improved in some plane or wearability, electric conductivity, mechanical property on certain directions etc..
Detailed description of the invention
It to describe the technical solutions in the embodiments of the present invention more clearly, below will be to needed in the embodiment Attached drawing is briefly described.
Fig. 1 is test bars machining sketch chart (compression aspect when P is material cold pressing).
Specific embodiment
Technical solution in order to enable those skilled in the art to better understand the present invention, with reference to the accompanying drawing and specific embodiment party Present invention is further described in detail for formula, and embodiment 1 is traditional preparation method, as a comparison embodiment, and others are implemented Example all uses preparation method of the invention.
Embodiment 1
Polytetrafluoroethylene (PTFE) selects fine polytetrafluoroethylpowder powder, and fiber selects chopped carbon fiber, and carbon fiber percent by volume is 20%, after carbon fiber is using silane resin acceptor kh-550 processing, polytetrafluoroethylene powder and carbon fiber are uniformly mixed, disposably will Mold is added in mixture, slowly applies pressure to 30MPa, and pressure maintaining 15 minutes, heating sintering finally kept the temperature 3 hours at 375 DEG C, Cool down with furnace.Test bars, such as Fig. 1 are processed by different directions.
Embodiment 2
Polytetrafluoroethylene (PTFE) selects fine polytetrafluoroethylpowder powder, and fiber selects chopped carbon fiber, and carbon fiber percent by volume is 20%, after carbon fiber is using silane resin acceptor kh-550 processing, polytetrafluoroethylene powder and carbon fiber are uniformly mixed, by the present invention Technique mixture is added portionwise, be forced into 10MPa after being added every time, pressure maintaining 5 seconds, each feeding quantity increased thick flake thickness degree Add 2 millimeters or so.Last time mixture is forced into 30MPa after adding, pressure maintaining 15 minutes, heat up and be sintered by established procedure, most 3 hours are kept the temperature at 375 DEG C eventually, is cooled down with furnace.Test bars, such as Fig. 1 are processed by different directions.
Embodiment 3
Polytetrafluoroethylene (PTFE) selects fine polytetrafluoroethylpowder powder, and fiber selects chopped carbon fiber, and carbon fiber percent by volume is 20%, after carbon fiber is using silane resin acceptor kh-550 processing, polytetrafluoroethylene powder and carbon fiber are uniformly mixed, by the present invention Technique mixture is added portionwise, be forced into 10MPa after being added every time, pressure maintaining 5 seconds, charging was so that thick flake thickness degree increases every time 5 millimeters or so.Last time mixture is forced into 30MPa after adding, pressure maintaining 15 minutes, heat up and be sintered by established procedure, finally 3 hours are kept the temperature at 375 DEG C, is cooled down with furnace.Test bars, such as Fig. 1 are processed by different directions.
Embodiment 4
Polytetrafluoroethylene (PTFE) selects fine polytetrafluoroethylpowder powder, and fiber selects chopped carbon fiber, and carbon fiber percent by volume is 5%, After fiber is using silane resin acceptor kh-550 processing, polytetrafluoroethylene powder and fiber are uniformly mixed, it will by technique of the invention Mixture is added portionwise, and 10MPa is forced into after being added every time, pressure maintaining 5 seconds, charging was so that thick flake thickness degree increases by 2 millimeters of left sides every time It is right.Last time mixture slowly applies pressure to 30MPa after adding, pressure maintaining 15 minutes, heat up and be sintered by established procedure, finally 3 hours are kept the temperature at 375 DEG C, is cooled down with furnace.Test bars, such as Fig. 1 are processed by different directions.
Embodiment 5
Polytetrafluoroethylene (PTFE) selects fine polytetrafluoroethylpowder powder, and fiber selects chopped carbon fiber, and carbon fiber percent by volume is 35%, after carbon fiber is using silane resin acceptor kh-550 processing, polytetrafluoroethylene powder and carbon fiber are uniformly mixed, by the present invention Technique mixture is added portionwise, be forced into 10MPa after being added every time, pressure maintaining 5 seconds, charging was so that thick flake thickness degree increases every time 2 millimeters or so.Last time mixture slowly applies pressure to 30MPa after adding, pressure maintaining 15 minutes, heat up and burn by established procedure Knot finally keeps the temperature 3 hours at 375 DEG C, cools down with furnace.Test bars, such as Fig. 1 are processed by different directions.
Embodiment 6
Polytetrafluoroethylene (PTFE) selects fine polytetrafluoroethylpowder powder, and fiber selects stainless steel fibre, stainless steel fibre percent by volume It is 8%, after fiber is using alkali cleaning, pickling, silane resin acceptor kh-550 processing, polytetrafluoroethylene powder and fiber is uniformly mixed, pressed Mixture is added portionwise technique of the invention, 10MPa is forced into after being added every time, pressure maintaining 5 seconds, charging was so that thick flake thickness every time Degree increases by 2 millimeters or so.Last time mixture slowly applies pressure to 30MPa after adding, and pressure maintaining 15 minutes, by established procedure Heating sintering, finally keeps the temperature 3 hours at 375 DEG C, cools down with furnace.Test bars, such as Fig. 1 are processed by different directions.
See Table 1 for details for data in above-described embodiment 1-6.
The tensile strength ratio of 1 embodiment test specimens of table and conductive ratio
Embodiment The tensile strength of batten 1 and batten 2 ratio The conductivity of batten 1 and batten 2 ratio
1 1.27 1.79
2 1.87 7.1
3 1.76 6.6
4 1.09 5.8
5 1.56 21
6 1.77 9.9
The test data of 1-6 is it is found that the fiber reinforcement polytetrafluoroethylene (PTFE) of traditional handicraft processing is compound through the foregoing embodiment Fiber only has slight orientation in material, and the tensile strength and conductivity for showing as the test bars of different directions cutting have Difference;And the degree of orientation of Fiber In Composite Material prepared by the present invention is used to be substantially higher much, show as different directions cutting Test bars tensile strength and conductivity have apparent difference.The test data of 2-3 is it is found that pass through through the foregoing embodiment Reduce the amount of single charge to reduce increased thickness every time and the degree of orientation of fiber can be improved, but it is very few to feed every time, Increase obviously to upper bring difficulty is operated.
In addition to above embodiments, there are also following some embodiments by the present invention.
Embodiment 7
Polytetrafluoroethylene (PTFE) selects fine polytetrafluoroethylpowder powder, and fiber selects chopped carbon fiber, and carbon fiber percent by volume is 20%, after carbon fiber is using silane resin acceptor kh-550 processing, polytetrafluoroethylene powder and carbon fiber are uniformly mixed, by the present invention Technique mixture is added portionwise, every time be added after be forced into 10MPa, pressure maintaining 10 seconds, each feeding quantity made thick flake thickness degree Increase by 2 millimeters or so.Last time mixture is forced into 30MPa after adding, pressure maintaining 15 minutes, heat up and be sintered by established procedure, 3 hours finally are kept the temperature at 375 DEG C, is cooled down with furnace.Test bars, such as Fig. 1 are processed by different directions.
Embodiment 8
Polytetrafluoroethylene (PTFE) selects fine polytetrafluoroethylpowder powder, and fiber selects chopped carbon fiber, and carbon fiber percent by volume is 20%, after carbon fiber is using silane resin acceptor kh-550 processing, polytetrafluoroethylene powder and carbon fiber are uniformly mixed, by the present invention Technique mixture is added portionwise, every time be added after be forced into 10MPa, pressure maintaining 20 seconds, each feeding quantity made thick flake thickness degree Increase by 2 millimeters or so.Last time mixture is forced into 30MPa after adding, pressure maintaining 15 minutes, heat up and be sintered by established procedure, 3 hours finally are kept the temperature at 375 DEG C, is cooled down with furnace.Test bars, such as Fig. 1 are processed by different directions.
Embodiment 9
Polytetrafluoroethylene (PTFE) selects fine polytetrafluoroethylpowder powder, and fiber selects chopped carbon fiber, and carbon fiber percent by volume is 20%, after carbon fiber is using silane resin acceptor kh-550 processing, polytetrafluoroethylene powder and carbon fiber are uniformly mixed, by the present invention Technique mixture is added portionwise, every time be added after be forced into 10MPa, pressure maintaining 30 seconds, each feeding quantity made thick flake thickness degree Increase by 2 millimeters or so.Last time mixture is forced into 30MPa after adding, pressure maintaining 15 minutes, heat up and be sintered by established procedure, 3 hours finally are kept the temperature at 375 DEG C, is cooled down with furnace.Test bars, such as Fig. 1 are processed by different directions.
Embodiment 10
Polytetrafluoroethylene (PTFE) selects fine polytetrafluoroethylpowder powder, and fiber selects chopped carbon fiber, and carbon fiber percent by volume is 20%, after carbon fiber is using silane resin acceptor kh-550 processing, polytetrafluoroethylene powder and carbon fiber are uniformly mixed, by the present invention Technique mixture is added portionwise, every time be added after be forced into 10MPa, pressure maintaining 10 seconds, each feeding quantity made thick flake thickness degree Increase by 2 millimeters or so.Last time mixture is forced into 30MPa after adding, pressure maintaining 20 minutes, heat up and be sintered by established procedure, 3 hours finally are kept the temperature at 375 DEG C, is cooled down with furnace.Test bars, such as Fig. 1 are processed by different directions.
Embodiment 11
Polytetrafluoroethylene (PTFE) selects fine polytetrafluoroethylpowder powder, and fiber selects the carbon steel fiber that is chopped, carbon steel fiber percent by volume It is 25%, after carbon steel fiber is using alkali cleaning, pickling, silane resin acceptor kh-550 processing, polytetrafluoroethylene powder and carbon steel fiber is mixed It closes uniformly, mixture is added portionwise by technique of the invention, 10MPa is forced into after being added every time, pressure maintaining 10 seconds, is fed every time Amount is so that thick flake thickness degree increases by 2 millimeters or so.Last time mixture is forced into 30MPa after adding, and pressure maintaining 15 minutes, by regulation Temperature programming sintering, finally keeps the temperature 3 hours at 375 DEG C, cools down with furnace.Test bars, such as Fig. 1 are processed by different directions.
Embodiment 12
Polytetrafluoroethylene (PTFE) selects fine polytetrafluoroethylpowder powder, and fiber selects the aramid fiber that is chopped, aramid fiber percent by volume It is 20%, polytetrafluoroethylene powder and aramid fiber is uniformly mixed, mixture is added portionwise by technique of the invention, adds every time 10MPa is forced into after entering, pressure maintaining 10 seconds, each feeding quantity made thick flake thickness degree increase by 2 millimeters or so.Last time mixture adds It is forced into 30MPa after complete, pressure maintaining 15 minutes, heats up and is sintered by established procedure, finally keep the temperature 3 hours at 375 DEG C, cool down with furnace. Test bars, such as Fig. 1 are processed by different directions.
The technical means disclosed in the embodiments of the present invention is not limited to the technical means disclosed in the above technical means, and further includes Technical solution consisting of any combination of the above technical features.

Claims (6)

1. a kind of preparation method of the two-dimensional orientation anisotropic composite material of fibre filling polytetrafluoroethyland, which is characterized in that Include:
A. fiber is surface-treated;
B. treated fiber and polytetrafluoroethylene powder are uniformly mixed, and obtain the mixture of fiber and polytetrafluoroethylene (PTFE);
C. fiber and teflon mixture are subjected to cold moudling in a mold, repeatedly fed in batches, is fed every time After once pressurizeed, after for the last time adding material, pressure is added to the value of process stipulation, and keep pressure;
D. it is sintered in sintering furnace.
2. the preparation side of the two-dimensional orientation anisotropic composite material of fibre filling polytetrafluoroethyland described in accordance with the claim 1 Method, which is characterized in that fiber is staple fiber.
3. the system of the two-dimensional orientation anisotropic composite material of fibre filling polytetrafluoroethyland according to claim 1 or 2 Preparation Method, which is characterized in that fiber described in step b and polytetrafluoroethylene (PTFE) are that 5%-35% is mixed by the percent by volume of fiber Uniformly.
4. the system of the two-dimensional orientation anisotropic composite material of fibre filling polytetrafluoroethyland according to claim 1 or 2 Preparation Method, which is characterized in that each feeding quantity described in step c makes thick flake thickness degree after pressurization increase 2-5 millimeters.
5. the system of the two-dimensional orientation anisotropic composite material of fibre filling polytetrafluoroethyland according to claim 1 or 2 Preparation Method, which is characterized in that the pressure value pressurizeed after feeding every time described in step c is 5-8MPa, and the dwell time is not less than 5 Second.
6. the system of the two-dimensional orientation anisotropic composite material of fibre filling polytetrafluoroethyland according to claim 1 or 2 Preparation Method, which is characterized in that pressure process specified value described in step c is 15-40MPa, and the dwell time is not less than 10 minutes.
CN201710431537.7A 2017-06-09 2017-06-09 A kind of preparation method of the two-dimensional orientation anisotropic composite material of fibre filling polytetrafluoroethyland Expired - Fee Related CN107099107B (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0248446A3 (en) * 1986-06-06 1990-01-03 E.I. Du Pont De Nemours And Company Anisotropic, liquid crystalline, polytetrafluoroethylene and tetrafluoroethylene copolymer aqueous dispersions

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