CN103059514A - Preparation method of magnetic lyophoby type carbon nano tube base nanochannel damping plate and damper - Google Patents
Preparation method of magnetic lyophoby type carbon nano tube base nanochannel damping plate and damper Download PDFInfo
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- CN103059514A CN103059514A CN2012105492075A CN201210549207A CN103059514A CN 103059514 A CN103059514 A CN 103059514A CN 2012105492075 A CN2012105492075 A CN 2012105492075A CN 201210549207 A CN201210549207 A CN 201210549207A CN 103059514 A CN103059514 A CN 103059514A
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Abstract
The invention relates to a preparation method of a magnetic lyophoby type carbon nano tube base nanochannel damping plate and a damper. The damping plate is formed by compounding surface grafting dodecafluoroheptyl-propyl-trimethoxylsilane and ferroferric oxide nano particles, a multiwalled carbon nanotube with an inner diameter of 20-30nm and epoxide resin under a qualitative magnetic field at high temperature and high pressure. The damper comprises an upper cylinder, a lower cylinder body and two connecting steel tubes, and further comprises the damping plate; the magnetic lyophoby type carbon nano tube base nanochannel damping plate is fixed inside the upper cylinder body; the lower cylinder body is a dual-outlet piston cylinder; and ethanediol is filled inside the upper and the lower cylinder bodies and the two connecting steel tubes. A carbon nano tube base nanofluid damper developed in the invention has the advantages of being small in volume, light in weight, high in energy dissipation, low in cost and the like, and can be used as novel passive energy dissipation damper for vibration control in the fields of military affairs, aero-space, engineering machinery, civil engineering and the like.
Description
Technical field
Patent of the present invention relates to a kind of magnetization lyophoby type carbon nanotube-based nanochannel damping fin preparation method and deoscillator.
Background technology
Since the nineties in 20th century, the researchist begins exploration nano material technology is applied to field of heat transfer.Nineteen ninety-five, the people such as Choi of U.S. Argonne National Laboratory have proposed a brand-new concept---nano-fluid first.Nano-fluid refers to nanoparticulate dispersed be prepared into novel heat exchange medium even, stable, high heat conduction in water, alcohol, wet goods tradition heat transferring medium.
Calendar year 2001, the people such as Hummer utilize molecular dynamics at first to study the motion conditions of water molecules in Single Walled Carbon Nanotube, are hydrophobic materials although find carbon nanotube itself, and water molecule energy automatically flows into and passes through carbon nanotube.After reducing the Van der Waals force between tube wall and water molecules, water molecules can not enter and pass through carbon nanotube.
Cambre ' waits the people to adopt Raman spectrum directly to observe the characteristics of motion of water molecules in the carbon pipe.They adopt the method for experiment to observe the strand flow phenomenon of water molecules in pipe with small pipe diameter carbon pipe first, have confirmed thus the people's such as Hummer theoretical investigation.
The people such as Gojny apply the coercive method, and have prepared the matrix material of double-walled carbon nano-tube and resin.Find by research, because carbon pipe and carbon black have obtained uniform dispersion in resin base, so that the mechanical property of this matrix material is greatly improved.
The people such as Song are compound under magneticaction with carbon nanotube and ferroferric oxide nano granules, prepared a kind of electrochemical sensing platform.Than the ordinary hydrogen electrode, this new magnetic carbon tube base electrode has stronger electro catalytic activity.This matrix material is for electrochemical induction and prepare the carbon nanotube base electrode new method is provided.
The people such as Abdalla have studied under the strong magnetic field action, the relation between the technique-structure of multi-walled carbon nano-tubes and resin composite materials-character.They adopt under high-intensity magnetic field, and behind multi-walled carbon nano-tubes grafting magnetic group, the method that is dispersed in the resin prepares matrix material.Research finds that align direction along the carbon pipe, the mechanical property of matrix material has obtained raising in various degree.Even if the carbon pipe is fully not directed, this composite materials property and heat-conductive characteristic still have part to improve.
Theoretical and experimental study by the foreign scholar as can be known, the characteristics of motion and the Conversion of energy relation of fluid in the nanoscale scope also thoroughly do not studied unclear, and both at home and abroad research and the application of magnetizing the carbon nanotube based composites also is in the starting stage, and lacks correlative study and application that fluid moves in the carbon pipe based composites of functionalization.
Summary of the invention
The object of the present invention is to provide and a kind ofly possess that volume is little, quality is light, energy dissipation capacity is strong, and by surface grafting ten difluoro heptyl propyl trimethoxy silicane and ferroferric oxide nano granules, internal diameter is the multi-walled carbon nano-tubes of 20-30nm and the nanoporous damping block that Resins, epoxy is composited under High Temperature High Pressure and directional magnetic field effect, and with the deoscillator of the supporting composition of ethylene glycol.
The technology used in the present invention is as follows:
A kind of preparation method of magnetizing the carbon nanotube-based nanochannel damping fin of lyophoby type is:
1) with the Ag internal diameter is 100 ℃ of dryings of multi-walled carbon nano-tubes vacuum of 20-30nm after 24 hours, mixes with the concentrated nitric acid of BmL68wt.% and 90 ℃ of high temperature refluxes 12 hours; After multi-walled carbon nano-tubes is washed till neutrality, mix in round-bottomed flask with dry toluene, add rapidly behind the C mL ten difluoro heptyl propyl trimethoxy silicanes mixed solution magnetic agitation and 90 ℃ of oil bath reflux 24 hours, reflux complete after with solution with the repeatedly 100 ℃ of vacuum-drying 12 hours after the washing and filtering 3 times of toluene and distilled water, with the multi-walled carbon nano-tubes of lyophoby and ferrous sulfate grain dissolution in volume ratio is 4: 1 distilled water and dehydrated alcohol mixed solution, the multi-walled carbon nano-tubes of lyophoby wherein, the solid-to-liquid ratio of ferrous sulfate particle and distilled water and dehydrated alcohol mixed solution is 1g: 10g: 250mL, supersound process 30 minutes, mechanical stirring 12 hours mixes solution; Then mixed-liquor return is heated to 90 ℃, slowly adding and ferrous sulfate mol ratio are 2: 1 sodium hydrate particle, 6 hours final vacuum dryings of 90 ℃ of lower mechanical stirring heating; Wherein said solid-to-liquid ratio A: B: C=1g: 100mL: 100mL;
2) will magnetize the multi-walled carbon nano-tubes of lyophoby and bisphenol A epoxide resin and trimethylhexamethylenediamine solidifying agent and join in the acetone, the multi-walled carbon nano-tubes of magnetization lyophoby: bisphenol A epoxide resin: trimethylhexamethylenediamine solidifying agent: the solid-to-liquid ratio in the acetone is 1g: 1g: 0.25g: 50mL; Normal temperature lower magnetic force stirred solution mixes it; The continuous volatilization of acetone, solution finally becomes sticky shape; Sticky thing is put into cylindrical die, and under the directional magnetic field effect of 1 tesla's intensity, with 10MPa pressure, the condition of 80 ℃ of temperature was solidified 6 hours; Damping block with curing molding is polished into the 5mm thin rounded flakes from two toward the centre respectively at last.
The present invention also has following feature:
1, the carbon nanotube-based nanochannel damping fin of a kind of magnetization lyophoby type for preparing by aforesaid preparation method.
2, a kind of high dynamic hydraulic sealed damper, comprise upper cylinder body, lower cylinder body and two joint steel pipes, it is characterized in that: also comprise the as mentioned above carbon nanotube-based nanochannel damping fin of a kind of magnetization lyophoby type, upper cylinder body inside is fixed with the carbon nanotube-based nanochannel damping fin of magnetization lyophoby type; Lower cylinder body goes out piston cylinder for two, and lower cylinder body is connected with the two ends of upper cylinder body by two joint steel pipes respectively and adopts the high pressure viton seal ring to seal, and ethylene glycol is equipped with in upper and lower cylinder body and two joint steel pipe inside; Operating pressure is 60MPa to the maximum; By two piston rods that go out piston cylinder are applied pulling force or pressure, make in the nano pore of ethylene glycol in damping fin continuously back and forth movement.
3, aforesaid a kind of high dynamic hydraulic sealed damper, its described ethylene glycol or be and the contact angle on the surface of the magnetization lyophoby type carbon nanotube-based nanochannel damping fin liquid greater than 100 °.
The carbon nanotube-based nano-fluid deoscillator of the present invention development possesses that volume is little, quality is light, energy dissipation capacity is strong, low cost and other advantages, can be used as novel passive energy-consumption damper for the vibration control in the fields such as military affairs, aerospace, engineering machinery and civil engineering work.
Description of drawings
Fig. 1 is carbon nanotube-based nano-fluid deoscillator power consumption hysteresis loop figure; Wherein (a) loading frequency is the 0.1Hz hysteresis loop; (b) loading frequency is the 0.5Hz hysteresis loop; (c) loading frequency is the 1Hz hysteresis loop;
Fig. 2 magnetizes lyophoby carbon nano tube TEM photo; (a) matrix material vertical view wherein; (b) along carbon pipe orientation direction matrix material sectional view;
Fig. 3 carbon nanotube base nano pore composite material SEM photo; (a) matrix material vertical view wherein; (b) along carbon pipe orientation direction matrix material sectional view;
Fig. 4 nano-fluid damper structure synoptic diagram.
Embodiment
For example patent of the present invention is described in more detail below in conjunction with accompanying drawing:
Embodiment 1: in conjunction with Fig. 1, the nano-fluid damping material that the present invention relates to is by surface grafting ten difluoro heptyl propyl trimethoxy silicane and ferroferric oxide nano granules, and internal diameter is multi-walled carbon nano-tubes based composites and the supporting composition of ethylene glycol of 20-30nm.The bonding situation of efficient and carbon pipe and the Resins, epoxy of this carbon nano pore composite material inner orientation nanochannel has directly determined the energy dissipation capacity of this damping material.The preparation of this nanoporous damping material mainly is divided into two steps:
1, be that 100 ℃ of dryings of multi-wall carbon nano-tube tube material vacuum of 20-30nm are after 24 hours with the 1g internal diameter, mix in the 500mL round-bottomed flask with the 50mL dry toluene, add fast behind the 10mL ten difluoro heptyl propyl trimethoxy silicanes mixed solution magnetic agitation and 90 ℃ of oil baths were refluxed 24 hours.Reflux complete after with solution with repeatedly washing and filtering and the 100 ℃ of vacuum-drying 12 hours of toluene and distilled water.With the 1g multi-walled carbon nano-tubes behind the surperficial lyophoby and 10g ferrous sulfate particle, be dissolved in the 250mL volume ratio and be in 4: 1 distilled water and the dehydrated alcohol mixed solution and supersound process 30 minutes, mechanical stirring 12 hours mixes solution.Then mixed-liquor return is heated to 90 ℃, slowly adding and ferrous sulfate mol ratio are 2: 1 sodium hydrate particle, 6 hours final vacuum dryings of 90 ℃ of lower mechanical stirring.
2,1g being magnetized the multi-walled carbon nano-tubes of lyophoby and 1g bisphenol A epoxide resin and 0.25g trimethylhexamethylenediamine solidifying agent joins in the 50mL acetone.Normal temperature lower magnetic force stirred solution mixes it.Because the continuous volatilization of acetone, solution finally becomes sticky shape.Sticky thing is put into cylindrical die, and under the directional magnetic field effect of about 1 tesla's intensity, with 10MPa pressure, the condition of 80 ℃ of temperature was solidified 6 hours.Damping block with curing molding is polished into the 5mm thin rounded flakes from two toward the centre respectively at last.
The liquid that forms nano-fluid power consumption material must satisfy with functionalization after the carbon nanotube principle that can not mutually infiltrate, can adopt the contact angle of measuring the carbon tube-surface of liquid after processing greater than 100 ° method.This patent all can form contact angle greater than 100 ° with magnetization lyophoby carbon nanotube powder through the high surface tension liquid of evidence ethylene glycol isopolarity, solid-liquid can not infiltrate mutually, can form the nano-fluid damping material with energy dissipation capacity with modified carbon nano-tube base nanochannel damping block.
Realize the energy dissipation capacity of this nano-fluid, need to force ethylene glycol liquid in the nanochannel of the matrix material of preparation, to flow, therefore need a kind of high dynamic hydraulic sealing resistance cylinders of design.The damping cavity of the present invention's design mainly is divided into two parts---and top is used for fixed carbon nanoporous damp composite material; The two rod piston/cylinders in bottom are used for holding and promote the ethylene glycol liquid-flow, and the upper and lower part cylinder body connects by steel pipe.The sealing of high pressure viton seal ring is all adopted in this resistance cylinders junction, and operating pressure is 60MPa to the maximum.Draw by deoscillator lower piston bar is applied, pressure, can force in the directed carbon pipe of ethylene glycol in matrix material continuously back and forth movement.
In order to test the energy dissipation capacity of this nano-fluid deoscillator, the magnetization lyophoby carbon nano tube based composites prepared and ethylene glycol liquid are packed in the deoscillator as stated above, and get rid of all air in the chamber as far as possible.Adopt the Instron4505 universal testing machine to push away, draw damper rod, make liquid come and go the aligned carbon nanotube that flows through composite inner.Trier load to adopt just profound ripple displacement-control mode, adds that the unloading frequency is respectively 0.1,0.5,1Hz, and vibration amplitude is 5mm.
As can be seen from Figure 1, load the starting stage, ethylene glycol liquid can't enter in the aligned carbon nanotube of matrix material, and curve only is liquid compressibility.When hydraulic pressure in the cylinder reached liquid and enters in the carbon pipe required minimum pressure, glycol molecule overcame solid---and light-liquid interfacial tension begins to enter in the carbon nanotube.Along with the further rising of pressure, fluid molecule constantly enters from matrix material one end, and continuously outflows from the other end.When reverse loading, the mode of motion of liquid in carbon nanotube loads identical with forward.After once adding unloading, formed a similar oval-shaped hysteresis loop.As can be seen from Figure 1, along with the increase of loading frequency, the energy dissipation capacity of nano-fluid improves gradually.The damping force maximum value is increased to about 22.5kN of 1Hz from about 4kN of 0.1Hz, and this trend meets the relation of liquid capillary force and wicking rate in the duct.Can stablize coincidence behind the hysteresis loop of this matrix material circulation 5 circles among the figure, the energy dissipation capacity that this nano-fluid deoscillator is described is stable.In addition, all can have a slope over 10 slowly to increase curve before the forward and reverse loading of this damping material begins, this is because due to the inner remaining air pressurized of deoscillator.
Embodiment 2: in conjunction with Fig. 2, the present invention adopts projection electron microscope (TEM) to study the carbon nanotube microscopic pattern structure of surface magnetization lyophoby.From Fig. 2, can obviously find out, comparatively uniformly grafting of carbon nano tube surface ferroferric oxide nano granules, therefore particle diameter has guaranteed can realize the good effect that aligns under the directional magnetic field effect of carbon Guan Zaiyue 1 tesla about about 5-10nm.Because ten difluoro heptyl propyl trimethoxy silicane content of grafting are limited, can't find out from the TEM photo, can prove by methods analysts such as XPS, XRD.
Embodiment 3: in conjunction with Fig. 3, the present invention has adopted scanning electronic microscope (SEM) to study the carbon nanotube of surface magnetization lyophoby and the combining case of Resins, epoxy.Can find out that from Fig. 2 (a) under quantitative the action of a magnetic field, the carbon pipe aligns comparatively uniformly in Resins, epoxy inside, composite material surface has only exposed the opening of carbon pipe.Fig. 2 (b) is the sectional view along carbon pipe orientation direction matrix material.Can find out that from figure the carbon pipe aligns uniformly in Resins, epoxy inside, and carbon pipe and resin-bonded degree are better.When having guaranteed thus liquid by this matrix material, major part is to pass from the carbon pipe that aligns.When this matrix material must guarantee integral rigidity, reduce the situation that Resins, epoxy stops up carbon nanotube as far as possible.Therefore, need to seek the mass ratio of carbon pipe and Resins, epoxy by constantly experiment, and moulding process.Multi-walled carbon nano-tubes and 1g bisphenol A epoxide resin and the 0.25g ambient cure agent of the present invention by 1g being magnetized lyophoby joins in the 50mL acetone.Normal temperature lower magnetic force stirred solution mixes it.Because the continuous volatilization of acetone, solution finally becomes sticky shape.Sticky thing is put into cylindrical die, under the directional magnetic field effect of about 1 tesla's intensity, with 10MPa pressure, the condition of 80 ℃ of temperature was solidified 6 hours, finally prepare as shown in Figure 2 the not blocked carbon nanotube base nano pore composite material of survivable and most of inner carbon pipe under the high hydraulic pressure.
Embodiment 4: in conjunction with Fig. 4, the present invention is in order to realize the reciprocal continuous flow of fluid in the composite material nanometer duct, and a kind of high dynamic hydraulic of designing seals two rod deoscillators.Comprise upper cylinder body 1, lower cylinder body 2 and two joint steel pipes 5, also comprise the carbon nanotube-based nanochannel damping fin 3 of magnetization lyophoby type, upper cylinder body 1 inside is fixed with the carbon nanotube-based nanochannel damping fin 3 of magnetization lyophoby type; Lower cylinder body 2 goes out piston cylinder for two, and lower cylinder body 2 is connected with the two ends of upper cylinder body 1 by two joint steel pipes 5 respectively and adopts the high pressure viton seal ring to seal, and ethylene glycol 4 is equipped with in upper and lower cylinder body 1.2 and two joint steel pipe 5 inside; The operating pressure maximum can be to 60MPa; By two piston rods 6 that go out piston cylinder are applied pulling force or pressure, can make in the nano pore of ethylene glycol 4 in graphene-based nanometer sheet 3 continuously back and forth movement.
Claims (4)
1. a preparation method of magnetizing the carbon nanotube-based nanochannel damping fin of lyophoby type is characterized in that, the method is:
1) with the Ag internal diameter is 100 ℃ of dryings of multi-walled carbon nano-tubes vacuum of 20-30nm after 24 hours, mixes with the concentrated nitric acid of B mL68wt.% and 90 ℃ of high temperature refluxes 12 hours; After multi-walled carbon nano-tubes is washed till neutrality, mix in round-bottomed flask with dry toluene, add rapidly behind the C mL ten difluoro heptyl propyl trimethoxy silicanes mixed solution magnetic agitation and 90 ℃ of oil bath reflux 24 hours, reflux complete after with solution with the repeatedly 100 ℃ of (vacuum-dryings 12 hours after the washing and filtering 3 times of toluene and distilled water, with the multi-walled carbon nano-tubes of lyophoby and ferrous sulfate grain dissolution in volume ratio is 4: 1 distilled water and dehydrated alcohol mixed solution, the multi-walled carbon nano-tubes of lyophoby wherein, the solid-to-liquid ratio of ferrous sulfate particle and distilled water and dehydrated alcohol mixed solution is 1g: 10g: 250mL, supersound process 30 minutes, mechanical stirring 12 hours mixes solution; Then mixed-liquor return is heated to 90 ℃, slowly adding and ferrous sulfate mol ratio are 2: 1 sodium hydrate particle, 6 hours final vacuum dryings of 90 ℃ of lower mechanical stirring heating;
Wherein said solid-to-liquid ratio A: B: C=1g: 100mL: 100mL;
2) will magnetize the multi-walled carbon nano-tubes of lyophoby and bisphenol A epoxide resin and trimethylhexamethylenediamine solidifying agent and join in the acetone, the multi-walled carbon nano-tubes of magnetization lyophoby: bisphenol A epoxide resin: trimethylhexamethylenediamine solidifying agent: the solid-to-liquid ratio in the acetone is 1g: 1g: 0.25g: 50mL; Normal temperature lower magnetic force stirred solution mixes it; The continuous volatilization of acetone, solution finally becomes sticky shape; Sticky thing is put into cylindrical die, and under the directional magnetic field effect of 1 tesla's intensity, with 10MPa pressure, the condition of 80 ℃ of temperature was solidified 6 hours; Damping block with curing molding is polished into the 5mm thin rounded flakes from two toward the centre respectively at last.
2. the carbon nanotube-based nanochannel damping fin of a kind of magnetization lyophoby type of a kind of preparation method's preparation of magnetizing the carbon nanotube-based nanochannel damping fin of lyophoby type as claimed in claim 1.
3. one kind high dynamic hydraulic sealed damper, comprise upper cylinder body, lower cylinder body and two joint steel pipes, it is characterized in that: also comprise the as claimed in claim 2 carbon nanotube-based nanochannel damping fin of a kind of magnetization lyophoby type, upper cylinder body inside is fixed with the carbon nanotube-based nanochannel damping fin of magnetization lyophoby type; Lower cylinder body goes out piston cylinder for two, and lower cylinder body is connected with the two ends of upper cylinder body by two joint steel pipes respectively and adopts the high pressure viton seal ring to seal, and ethylene glycol is equipped with in upper and lower cylinder body and two joint steel pipe inside; Operating pressure is 60MPa to the maximum; By two piston rods that go out piston cylinder are applied pulling force or pressure, make in the nano pore of ethylene glycol in damping fin continuously back and forth movement.
4. a kind of high dynamic hydraulic sealed damper according to claim 3 is characterized in that: described ethylene glycol or for the contact angle on the surface of the carbon nanotube-based nanochannel damping fin of the magnetization lyophoby type liquid greater than 100 °.
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| CN110410607A (en) * | 2019-08-07 | 2019-11-05 | 陈浩然 | A kind of environmental protection expansion bellow |
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