CN106906641B - It is electromagnetically shielded inorganic ultra tiny conductive fiber of enhancing of grade and preparation method thereof - Google Patents

It is electromagnetically shielded inorganic ultra tiny conductive fiber of enhancing of grade and preparation method thereof Download PDF

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CN106906641B
CN106906641B CN201710091777.7A CN201710091777A CN106906641B CN 106906641 B CN106906641 B CN 106906641B CN 201710091777 A CN201710091777 A CN 201710091777A CN 106906641 B CN106906641 B CN 106906641B
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fiber
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CN106906641A (en
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杜英
杜宏伟
杜守成
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/73Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
    • D06M11/74Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Inorganic Fibers (AREA)
  • Paints Or Removers (AREA)
  • Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)

Abstract

The present invention relates to inorganic ultra tiny conductive fibers of enhancing of a kind of electromagnetic shielding grade and preparation method thereof.It selects natural high-quality inorganic fibrous nonmetallic ore as matrix, is processed into super-micro-fine fibres powder, is mixed with conductive black, ultra micro fine graphite powders, propane, auxiliary chemicals.Become partial size 0.5um~50um, draw ratio 2:1~100:1, pine ratio 0.1g/cm in fiber powder surface one layer of conductive film of secured carbonized graphiteization by pyrolytic, dehydrogenation, cyclisation, carbonization3~1.0g/cm3, 0.3 Ω of Ω .cm~10 cm of volume resistivity conductive fiber powder.With enhancing, wear-resisting, high temperature resistant, performance anti-aging, resistant to chemical etching, electric conductivity is constant, while having the characteristics that large specific surface area, light-weight, fiber overlap joint is intensive, conductivity is high, it can be compound with the industrial chemicals such as any resin.Especially suitable for producing the various invisible coatings of military equipment, antistatic, the demanding product of electromagnetic shielding performance;It is also applied for aerospace, high-speed rail automobile, electronic apparatus, plastic, rubber, chemical building material field.

Description

It is electromagnetically shielded inorganic ultra tiny conductive fiber of enhancing of grade and preparation method thereof
Technical field
The present invention relates to conductive, antistatic, electromagnetic shielding material field more particularly to a kind of inorganic enhancings of electromagnetic shielding grade Ultra tiny conductive fiber and preparation method thereof.
Background technique
With the development of modern high technology, electromagnetism caused by the needs and electromagnetic wave of military equipment stealth technique is dry It disturbs (EMI) and electromagnetic compatibility (EMC) problem to get worse, not only electronic instrument, equipment is interfered and damaged, is influencing it just Often work, the serious international competitiveness for restricting China's electronic product and equipment, and pollute the environment, human health is endangered, In addition electromagnetic-wave leakage can also jeopardize the safety of national information safety and military vital strategic secrets.Therefore, environmentally protective, Gao Xing is explored Energy conduction, antistatic electromagnetic shielding stealth material, prevent electromagnetic interference caused by electromagnetic wave and electromagnetic compatibility problem, for mentioning The security reliability of high electronic product and equipment promotes international competitiveness, prevents the strike of electromagnetic pulse weapon, it is ensured that information is logical Letter system, network system, Transmission system, weapon platform etc. it is safe and smooth, particularly with R&D and production stealth military equipment have There is important meaning.
Conduction, antistatic, electromagnetic shielding material used in the country and the conduction of existing civilian electricity heating product at present Material uses the higher chopped carbon fiber of price mostly, or uses various metal powders, the chopped powder such as fine wire and silica Body and Organic Chemicals are combined.Since the powders such as silica itself are non-conductive, specific surface area is small, than great, makes With metal powder in the process, silk and Organic Chemicals easily occur chemical reaction and corrosion and ageing, and then cause conductivity, resist it is quiet Electricity, electromagnetic shielding effect decline.
Summary of the invention
To overcome above-mentioned the deficiencies in the prior art, the present invention provides a kind of inorganic ultra tiny conductions of enhancing of electromagnetic shielding grade Fiber and preparation method thereof.The present invention has enhancing, wear-resisting, high temperature resistant, property anti-aging, resistant to chemical etching, conductivity is constant Can, while having the characteristics that large specific surface area, light-weight, fiber overlap joint is intensive, conductivity is high, it can be former with any resin and chemical industry Expect it is compound, be suitable for aerospace, high-speed rail automobile, electronic apparatus, household electrical appliance, environment protection solar civil heating product, modeling Expect the fields such as rubber, chemical building material, is particularly suitable for the production various invisible coatings of military equipment, antistatic, electromagnetic wave shielding It can demanding product.
In order to achieve the above object, the present invention is implemented with the following technical solutions:
A kind of inorganic ultra tiny conductive fiber of enhancing of electromagnetic shielding grade, component weight percent proportion are as follows: natural excellent Super-micro-fine fibres powder 65%~95%, the conductive black 4%~45%, ultra micro microlith of matter inorganic fibrous nonmetallic ore processing Ink powder 1%~1.5%, dehydrogenating agent 0.1%~1.0%, carbon black disperser 0.5%~3%;The conductive fiber partial size 0.5um ~50um, draw ratio 2:1~100:1, Bulk Specific Gravity 0.1g/cm3~1.0g/cm3, 0.3 Ω of Ω cm~10 of volume resistivity cm。
A kind of preparation method of the ultra tiny conductive fiber of the inorganic enhancing of electromagnetic shielding grade, which is characterized in that specifically include as Lower step:
(1) superfine fibre powder is prepared, acicular wollastonite, fibrous sepiolite, ceramic fibre, basalt fibre etc. are selected Natural high-quality fusing point, as matrix, prepares partial size 0.5um~50um, major diameter in 1500 DEG C or more of inorganic fibrous nonmetallic ore Than the super-micro-fine fibres powder of 2:1~100:1, sedimentation value 30ml~150ml;
(2) conductive black, ultra micro fine graphite powders are mixed with dehydrogenating agent, carbon black disperser heating, and ultra tiny fibre is added Powder is tieed up, mixed fiber powder is packed into the storage bin of screw(-type) feeder;
(3) mixed fiber powder is delivered in gas-solid mixer by screw(-type) feeder, and with the propane of input with Inert gas is mixed with;
(4) by the graphite-pipe of mixture input high temperature furnace revolving burner, propane and dehydrogenating agent, carbon black disperser are in indifferent gas In 200 DEG C~1400 DEG C pyrolytics, dehydrogenation, cyclisation, carbonizations under body protection, and then by conductive black, ultra micro fine graphite powders, Even firm carbonized graphite forms one layer of conductive film on fiber powder surface;
(5) by the cooling purification of said mixture, finally it is prepared into the inorganic ultra tiny conductive fiber of enhancing of electromagnetic shielding grade.
Step (2) the super-micro-fine fibres powder weight is 65%~95% by percentage proportion, conductive black weight Amount is 4%~45% by percentage proportion, and ultra micro fine graphite powders weight is 1%~1.5% by percentage proportion, dehydrogenating agent weight It is 0.5%~3% that by percentage proportion, which be 0.1%~1.0%, carbon black disperser weight is matched by percentage.The step (3) The propane flow is measured in litres, and 20 liters~500 liters of flow per minute, inert gas flow is measured in litres, flow 30 per minute Rise~550 liters.
Compared with prior art, the beneficial effects of the present invention are:
The present invention provides inorganic ultra tiny conductive fibers of enhancing of a kind of electromagnetic shielding grade and preparation method thereof.Present invention choosing It is processed with inorganic fibrous nonmetallic ore, partial size 0.5um~50um, draw ratio 2:1~100:1, sedimentation value 30ml~150ml Super-micro-fine fibres powder is matrix;The conductive fiber partial size 0.5um~50um, draw ratio 2:1~100:1, Bulk Specific Gravity 0.1g/ cm3~1.0g/cm3, 0.3 Ω of Ω cm~10 cm of volume resistivity.500 DEG C of high temperature are resistant to, are resistant to 1400 DEG C under anaerobic state High temperature.The present invention has enhancing, wear-resisting, high temperature resistant, performance anti-aging, resistant to chemical etching, conductivity is constant, while having ratio The features such as surface area is big, light-weight, fiber connection is intensive, conductivity is high, can be compound with any resin and industrial chemicals, is suitable for Aerospace, high-speed rail automobile, electronic apparatus, household electrical appliance, environment protection solar civil heating product, plastic, rubber, chemical industry are built The fields such as material are particularly suitable for the production various invisible coatings of military equipment, antistatic, the demanding production of electromagnetic shielding performance Product.
Specific embodiment
Specific embodiments of the present invention will be further explained below:
A kind of inorganic ultra tiny conductive fiber of enhancing of electromagnetic shielding grade, component weight percent proportion are as follows: natural excellent Super-micro-fine fibres powder 65%~95%, the conductive black 4%~45%, ultra micro microlith of matter inorganic fibrous nonmetallic ore processing Ink powder 1%~1.5%, dehydrogenating agent weight is matched by percentage is matched for 0.1%~1.0%, carbon black disperser weight by percentage Than being 0.5%~3%;The conductive fiber partial size 0.5um~50um, draw ratio 2:1~100:1, Bulk Specific Gravity 0.1g/cm3~ 1.0g/cm3, 0.3 Ω of Ω cm~10 cm of volume resistivity.
A kind of preparation method of the inorganic ultra tiny conductive fiber of enhancing of electromagnetic shielding grade, specifically comprises the following steps:
(1) superfine fibre powder is prepared, acicular wollastonite, fibrous sepiolite, ceramic fibre, basalt fibre etc. are selected Natural high-quality fusing point, as matrix, prepares partial size 0.5um~50um, major diameter in 1500 DEG C or more of inorganic fibrous nonmetallic ore Than the super-micro-fine fibres powder of 2:1~100:1, sedimentation value 30ml~150ml;
(2) conductive black, ultra micro fine graphite powders are mixed with dehydrogenating agent, carbon black disperser heating, and ultra tiny fibre is added Powder is tieed up, mixed fiber powder is packed into the storage bin of screw(-type) feeder;The super-micro-fine fibres powder weight presses hundred Score proportion is 65%~95%, and conductive black weight is 4%~45% by percentage proportion, and ultra micro fine graphite powders weight presses hundred Score proportion is 1%~1.5%, and dehydrogenating agent weight is that 0.1%~1.0%, carbon black disperser weight presses hundred by percentage proportion Score proportion is 0.5%~3%.
(3) mixed fiber powder is delivered in gas-solid mixer by screw(-type) feeder, and with input propane with it is lazy Property gas is mixed with;Propane flow is measured in litres, and 20 liters~500 liters of flow per minute, inert gas flow is measured in litres, often 30 liters~550 liters of flow of minute.
Gas-solid mixer shape be it is oblate, inner circle be equipped with mixing chamber, outer circle be equipped with multiple air inlets.Air inlet hole mouth with Mixing chamber communicates collar extension and connect with air inlet pipe.One end face of gas-solid mixer is fixedly connected with screw(-type) feeder discharging end housing, separately One end face and high temperature furnace rotation boiler tube feed end are tightly connected.Screw(-type) feeder discharge end axis is equipped with agitator arm, paddle Mixing chamber is formed in wheel insertion gas-solid mixer mixing chamber.
(4) enter and mix indoor mixed powder, propane, inert gas, high temperature furnace revolving burner is inputted after agitated mixing In graphite-pipe in pipe, special-purpose high temperature furnace is electric heating, and it is adjustable that rotation boiler tube by heat-resisting material is made revolving speed, is rotated in boiler tube Stud with high temperature resistant graphite-pipe.It rotates boiler tube feed end and gas-solid mixer discharge port is tightly connected, discharge end and dedicated cooling fill Set import sealed connection.
Propane and dehydrogenating agent, carbon black disperser under inert gas protection 200 DEG C~1400 DEG C pyrolytics, dehydrogenation, Cyclisation, carbonization, and then by conductive black, ultra micro fine graphite powders, uniformly firm carbonized graphite is formed on fiber powder surface One layer of conductive film;
(5) by the cooling purification of said mixture, finally it is prepared into the inorganic ultra tiny conductive fiber of enhancing of electromagnetic shielding grade.
Cooling device is vertical rectangular shape, circulating water, lower end water inlet upper end water outlet.Cooling device upper end is equipped with sealing Cover board, side are equipped with feed inlet.It rotates boiler tube discharge port insertion cooling device feed inlet to be tightly connected, feed inlet side, which is equipped with, to be seen Examine window.Lower end is equipped with discharge port, connect with purifying plant blast pipe.
Embodiment 1:
A kind of inorganic ultra tiny conductive fiber of enhancing of electromagnetic shielding grade, component weight percent proportion are as follows: natural excellent Matter inorganic fibrous nonmetallic ore processing super-micro-fine fibres powder 70%, conductive black 30%, ultra micro fine graphite powders 1.5%, Dehydrogenating agent 0.8%, carbon black disperser 2.5%;The conductive fiber partial size 10um, draw ratio 2:1~10:1, Bulk Specific Gravity 0.14g/ cm3, 1.4 Ω cm of volume resistivity, be resistant to 480 DEG C of high temperature, 1390 DEG C of high temperature are resistant under anaerobic state.
A kind of preparation method of the inorganic ultra tiny conductive fiber of enhancing of electromagnetic shielding grade, specifically comprises the following steps:
(1) prepare superfine fibre powder, select natural high-quality fusing point 1500 DEG C or more inorganic acicular wollastonite as Matrix prepares the super-micro-fine fibres powder of partial size 10um, draw ratio 2:1~10:1.
(2) conductive black, ultra micro fine graphite powders are mixed with dehydrogenating agent, carbon black disperser heating, and ultra tiny fibre is added Powder is tieed up, mixed fiber powder is packed into the storage bin of screw(-type) feeder;The super-micro-fine fibres powder weight presses hundred Score proportion is 70%, and conductive black weight is 30% by percentage proportion, and ultra micro fine graphite powders weight is by percentage proportion 1.5%, it is 2.5% that dehydrogenating agent weight, which is matched by percentage and matched for 0.8%, carbon black disperser weight by percentage,.
(3) mixed fiber powder is delivered in gas-solid mixer by screw(-type) feeder, and with input propane with it is lazy Property gas is mixed with;The propane flow is measured in litres, and 250 liters of flow per minute, inert gas flow is measured in litres, and every point 300 liters of clock flow.
(4) by the graphite-pipe of mixture input high temperature furnace revolving burner, propane and dehydrogenating agent, carbon black disperser are in indifferent gas In 200 DEG C~1400 DEG C pyrolytics, dehydrogenation, cyclisation, carbonizations under body protection, and then by conductive black, ultra micro fine graphite powders, Even firm carbonized graphite forms one layer of conductive film on fiber powder surface.
(5) by the cooling purification of said mixture, finally it is prepared into the inorganic ultra tiny conductive fiber of enhancing of electromagnetic shielding grade.
Embodiment 2:
A kind of inorganic ultra tiny conductive fiber of enhancing of electromagnetic shielding grade, component weight percent proportion are as follows: natural excellent Matter inorganic fibrous nonmetallic ore processing super-micro-fine fibres powder 80%, conductive black 20%, ultra micro fine graphite powders 0.5%, Dehydrogenating agent 0.3%, carbon black disperser 1.5%;The conductive fiber draw ratio 30:1, Bulk Specific Gravity 0.2g/cm3, volume resistivity 0.6 Ω cm is resistant to 490 DEG C of high temperature, 1400 DEG C of high temperature is resistant under anaerobic state.
A kind of preparation method of the inorganic ultra tiny conductive fiber of enhancing of electromagnetic shielding grade, specifically comprises the following steps:
(1) superfine fibre powder is prepared, natural inorganic fibrous nonmetallic ore of the high-quality fusing point at 1500 DEG C or more is selected Acicular wollastonite, the super-micro-fine fibres powder of the draw ratio 30:1 of processing, sedimentation value 90ml.
(2) conductive black, ultra micro fine graphite powders are mixed with dehydrogenating agent, carbon black disperser heating, and ultra tiny fibre is added Powder is tieed up, mixed fiber powder is packed into the storage bin of screw(-type) feeder;The super-micro-fine fibres powder weight presses hundred Score proportion is 80%, and conductive black weight is 20% by percentage proportion, and ultra micro fine graphite powders weight is by percentage proportion 0.5%, it is 1.5% that dehydrogenating agent weight, which is matched by percentage and matched for 0.3%, carbon black disperser weight by percentage,.
(3) mixed fiber powder is delivered in gas-solid mixer by screw(-type) feeder, and with input propane with it is lazy Property gas is mixed with;The propane flow is measured in litres, and 350 liters of flow per minute, inert gas flow is measured in litres, and every point 390 liters of clock flow.
(4) by the graphite-pipe of mixture input high temperature furnace revolving burner, propane and dehydrogenating agent, carbon black disperser are in indifferent gas In 200 DEG C~1400 DEG C pyrolytics, dehydrogenation, cyclisation, carbonizations under body protection, and then by conductive black, ultra micro fine graphite powders, Even firm carbonized graphite forms one layer of conductive film on fiber powder surface.
(5) by the cooling purification of said mixture, finally it is prepared into the inorganic ultra tiny conductive fiber of enhancing of electromagnetic shielding grade.
The present invention has enhancing, wear-resisting, high temperature resistant, performance anti-aging, resistant to chemical etching, conductivity is constant, has simultaneously There is the features such as large specific surface area, light-weight, fiber overlap joint is intensive, conductivity is high, can be compound with any resin and industrial chemicals, it fits For aerospace, high-speed rail automobile, electronic apparatus, household electrical appliance, environment protection solar civil heating product, plastic, rubber, change The fields such as work building materials are particularly suitable for producing various invisible coatings, antistatic, electromagnetic wave shielding performance requirement height in military equipment Product.
The above only lifts two specific embodiment of the invention, but scope of protection of the present invention is not limited thereto, appoints What those familiar with the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its sends out Bright design is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.

Claims (2)

1. a kind of inorganic ultra tiny conductive fiber of enhancing of electromagnetic shielding grade, which is characterized in that its component weight percent proportion Are as follows: the super-micro-fine fibres powder 65%~95% of natural inorganic fiber shape nonmetallic ore processing, surpasses conductive black 4%~45% Fine graphitic powder 1%~1.5%, dehydrogenating agent 0.1%~1.0%, carbon black disperser 0.5%~3.0%;The conductive fiber grain Diameter 0.5um~50um, draw ratio 2:1~100:1, Bulk Specific Gravity 0.1g/cm3~1.0g/cm3, 0.3 Ω cm of volume resistivity~ 10Ω·cm;
The preparation method of the inorganic ultra tiny conductive fiber of enhancing of the electromagnetic shielding grade, specifically comprises the following steps:
(1) it prepares superfine fibre powder, selects acicular wollastonite, fibrous sepiolite, ceramic fibre, one in basalt fibre Kind or it is several, natural fusing point in 1500 DEG C or more of inorganic fibrous nonmetallic ore as matrix, prepare partial size 0.5um~ The super-micro-fine fibres powder of 50um, draw ratio 2:1~100:1, sedimentation value 30ml~150ml;
(2) conductive black, ultra micro fine graphite powders are mixed with dehydrogenating agent, carbon black disperser heating, and super-micro-fine fibres powder is added Mixed fiber powder is packed into the storage bin of screw(-type) feeder by body;
Super-micro-fine fibres powder weight is 65%~95% by percentage proportion, and conductive black weight is 4% by percentage proportion ~45%, ultra micro fine graphite powders weight is 1%~1.5% by percentage proportion, and dehydrogenating agent weight is 0.1% by percentage proportion ~1.0%, carbon black disperser weight is 0.5%~3.0% by percentage proportion;
(3) mixed fiber powder is delivered in gas-solid mixer by screw(-type) feeder, and with the propane of input, indifferent gas Body mixing;
(4) by the graphite-pipe of mixture input high temperature furnace revolving burner, propane and dehydrogenating agent, carbon black disperser are protected in inert gas In 200 DEG C~1400 DEG C pyrolytics, dehydrogenation, cyclisation, carbonizations under shield, and then by conductive black, ultra micro fine graphite powders, uniform jail Solid carbonized graphite on fiber powder surface, form one layer of conductive film;
(5) by the cooling purification of said mixture, finally it is prepared into the inorganic ultra tiny conductive fiber of enhancing of electromagnetic shielding grade.
2. a kind of preparation method of the inorganic ultra tiny conductive fiber of enhancing of electromagnetic shielding grade according to claim 1, special Sign is that propane flow is measured in litres in the step (3), and 20 liters~500 liters of flow per minute, inert gas flow is in litres Amount, 30 liters~550 liters of flow per minute.
CN201710091777.7A 2017-02-21 2017-02-21 It is electromagnetically shielded inorganic ultra tiny conductive fiber of enhancing of grade and preparation method thereof Expired - Fee Related CN106906641B (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1461364A (en) * 2000-09-21 2003-12-10 美利肯公司 Temp. dependent electrically resistive yarn
CN103966844A (en) * 2014-05-23 2014-08-06 青岛大学 Preparation method of graphene electroconductive composite fiber

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103554530A (en) * 2013-10-11 2014-02-05 中国航空工业集团公司北京航空材料研究院 Electric conductive continuous fiber-reinforced fabric or prepreg and electric conductive treatment method

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1461364A (en) * 2000-09-21 2003-12-10 美利肯公司 Temp. dependent electrically resistive yarn
CN103966844A (en) * 2014-05-23 2014-08-06 青岛大学 Preparation method of graphene electroconductive composite fiber

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