CN103602041B - A kind of preparation method improving the microstructure containing hole composite material bore edges abrasion resistance properties and contain hole composite material in order - Google Patents

A kind of preparation method improving the microstructure containing hole composite material bore edges abrasion resistance properties and contain hole composite material in order Download PDF

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CN103602041B
CN103602041B CN201310572198.6A CN201310572198A CN103602041B CN 103602041 B CN103602041 B CN 103602041B CN 201310572198 A CN201310572198 A CN 201310572198A CN 103602041 B CN103602041 B CN 103602041B
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composite material
carbon nanotube
hole composite
preparation
ratio
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CN103602041A (en
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矫维成
王荣国
刘文博
牛越
杨帆
郑莉
郝立峰
徐忠海
赫晓东
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Harbin Institute of Technology
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Harbin Institute of Technology
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Abstract

Improve the preparation method that the microstructure containing hole composite material bore edges abrasion resistance properties contains hole composite material in order, the present invention relates to a kind of preparation method containing hole composite material.The present invention will solve existing apertures composite-material abrasive to damage poor performance and the low problem of mechanical property, and preparation method of the present invention is as follows: one, carbon nanotube acidifying process; Two, the preparation of the carbon nanotube of surface magnetism particle modification; Three, the preparation of the orderly apertures carbon nano tube/epoxy resin composite material of microstructure.Prepared by present embodiment contains hole composite material, compare traditional bore edges reinforcement, quality is light, abrasion resistance properties improves about 77%, thus the work-ing life effectively extended containing hole composite material, and carbon nanotube is Orienting ordered arrangement in the epoxy, the resistance to air loss of this arrangement meeting reinforced composite in order, can be applied to the enhancing design of perforate matrix material.

Description

A kind of preparation method improving the microstructure containing hole composite material bore edges abrasion resistance properties and contain hole composite material in order
Technical field
The present invention relates to a kind of preparation method containing hole composite material.
Background technology
At present, take carbon-fibre composite as the excellent properties that the advanced material of representative has high-strength light because of it, be widely used in the field such as Aeronautics and Astronautics, naval vessel.Owing to being linked and packed, checking, connecting up, keeping in repair, the needs such as conduit, composite structure often will open many holes.But composite structure is very responsive to damage, especially open-celled structure, under the load effects such as stretching, compression, shearing, easily produces tiny crack and causes structure deteriorate, have a strong impact on work-ing life.The enhancing design of matrix material open-celled structure, enjoys the concern of researchist always.
Summary of the invention
The present invention will solve existing apertures composite-material abrasive to damage poor performance and the low problem of mechanical property, thus provides a kind of and improve microstructure containing hole composite material bore edges abrasion resistance properties in order containing the preparation method of hole composite material.
A kind of microstructure improved containing hole composite material bore edges abrasion resistance properties of the present invention is carried out according to the following steps containing the preparation method of hole composite material in order:
One, carbon nanotube acidifying process: by dense HNO 3with dense H 2sO 4at room temperature Homogeneous phase mixing, then carbon nanotube is added, and under temperature is 50 ~ 70 DEG C and rotating speed is the condition of 1200r/min ~ 1500r/min, stir 4h ~ 6h, supersound process 2h ~ 4h under ultrasonic frequency is 80Hz ~ 100Hz again, obtain acid solidliquid mixture, then the acid solidliquid mixture deionized water obtained being diluted to pH value is 0.8 ~ 1.2, then suction filtration is carried out, filtrate is discarded after suction filtration, and use deionized water wash solid matter, carry out suction filtration and washing again, until the filtrate pH value after suction filtration is 6.8 ~ 7.2, obtain solid matter, be dry 20h ~ 24h under the condition of 80 DEG C ~ 100 DEG C in temperature by the solid matter obtained, obtain the carbon nanotube after acidifying, dense HNO described in step one 3with dense H 2sO 4volume ratio be 1:(2 ~ 4), the quality of the carbon nanotube described in step one and dense HNO 3volume ratio be 1g:(6 ~ 9) mL,
Two, the preparation of the carbon nanotube of surface magnetism particle modification: the carbon nanotube after the acidifying 1. step one obtained puts into strong aqua, supersound process 1h ~ 3h under ultrasonic frequency is 80Hz ~ 100Hz, obtains carbon nanotube/ammoniacal liquor suspension, 2. be 10 in vacuum tightness -3pa ~ 1.5 × 10 -3under the condition of Pa by Iron trichloride hexahydrate and ferrous chloride hydrate dissolution in deionized water, Fe is obtained 3+/ Fe 2+mixing solutions, 3. be 10 in vacuum tightness -3pa ~ 1.5 × 10 -32. the Fe will obtained under the condition of Pa 3+/ Fe 2+mixing solutions joins 1. in the carbon nanotube/ammoniacal liquor suspension obtained, and obtains mixing solutions after mixing, and is then 10 in vacuum tightness -3pa ~ 1.5 × 10 -3under the condition of Pa, first Viscotrol C being warming up to temperature is 60 ~ 80 DEG C, then the mixing solutions obtained is joined in Viscotrol C, 3h ~ 5h is stirred again under temperature is 80 ~ 90 DEG C and rotating speed is 150r/min ~ 200r/min, complete reaction, obtain the carbon nano-tube solution that surface magnetism particle is modified, by carbon nano-tube solution centrifugal 4min ~ 6min under rotating speed is 11000r/min ~ 13000r/min that the surface magnetism particle obtained is modified, abandoning supernatant, and the solid matter obtained is purified, purify 2 ~ 4 dry 10h ~ 14h of final vacuum, obtain the carbon nanotube that surface magnetism particle is modified, purification processes described in step 2 is: first use absolute ethanol washing solid matter, then under ultrasonic frequency is 80Hz ~ 100Hz, processes 8min ~ 12min, then carries out magnetic resolution, step 2 1. described in the acidifying that obtains of step one after the quality of carbon nanotube be (3 ~ 5) mg:1mL with the ratio of the volume of strong aqua, step 2 2. described in Iron trichloride hexahydrate be (1 ~ 3) with the ratio of the amount of substance of ferrous chloride hydrate: 1, step 2 2. described in the amount of substance of Iron trichloride hexahydrate be 0.004mol:(4 ~ 6 with the ratio of the volume of deionized water) mL, step 2 3. described in carbon nanotube/ammoniacal liquor suspension of 1. obtaining of step 2 and the Fe that 2. obtains of step 2 3+/ Fe 2+the ratio of the volume of mixing solutions is (3 ~ 5): 1, step 2 3. described in mixing solutions be 1:(15 ~ 22 with the ratio of the volume of Viscotrol C),
Three, the preparation of the orderly apertures carbon nano tube/epoxy resin composite material of microstructure: the carbon nanotube that surface magnetism particle epoxy resin, dehydrated alcohol and step 2 3. obtained is modified mixes, then be the condition down cut 30min ~ 50min of 8000r/min ~ 10000r/min at rotating speed with high-speed shearing emulsion machine, add after quadrol mixes again, obtaining cured product, is then 10 at normal temperature and vacuum tightness -3pa ~ 10 -5under the condition of Pa, cured product being placed on magneticstrength is leave standstill 40min ~ 60min in the uniform magnetic field of 0.4T ~ 1T, then be dry 20h ~ 24h under the condition of 60 DEG C ~ 80 DEG C in temperature, obtain the orderly apertures carbon nano tube/epoxy resin composite material of microstructure; Epoxy resin wherein described in step 3 and the mass ratio of dehydrated alcohol are 100:(18 ~ 25); The mass ratio of the carbon nanotube that the surface magnetism particle that 3. epoxy resin described in step 3 and step 2 obtain is modified is 1000:(1 ~ 20); The mass ratio of the quadrol described in step 3 and epoxy resin is 1:(10 ~ 12).
Method of the present invention adopts first carries out acidification by carbon nanotube, carbon nanotube after acidifying is put into strong aqua, prepare carbon nanotube/ammoniacal liquor suspension, then Iron trichloride hexahydrate and ferrous chloride hydrate are dissolved in deionized water under vacuum, prepare magnetic particle Fe 3+/ Fe 2+'smixing solutions, then by Fe 3+/ Fe 2+mixing solutions joins in carbon nanotube/ammoniacal liquor suspension, join after mixing in the Viscotrol C of preheating, again through centrifugal, purify and drying, obtain the carbon nanotube that surface magnetism particle is modified, finally by epoxy resin, the carbon nanotube that dehydrated alcohol and surface magnetism particle are modified mixes, sheared by high-speed shearing emulsion machine, solidify through quadrol again, then cured product is placed in uniform magnetic field and leaves standstill, again after drying, obtain the orderly apertures carbon nano tube/epoxy resin composite material of microstructure, prepared by the present invention contains hole composite material, compare traditional bore edges reinforcement, quality is light, abrasion resistance properties improves about 77%, thus the work-ing life effectively extended containing hole composite material, and carbon nanotube is Orienting ordered arrangement in the epoxy, the resistance to air loss of this arrangement meeting reinforced composite in order, the enhancing design of perforate matrix material can be applied to.
Accompanying drawing explanation
Fig. 1 is the arrangement schematic diagram of the orderly apertures carbon nano tube/epoxy resin composite material of microstructure that test one obtains; Wherein A is carbon nanotube, and B is epoxy resin, and C is magnet;
Fig. 2 is the friction and wear test graphic representation of the orderly apertures carbon nano tube/epoxy resin composite material of microstructure that test one obtains; Wherein a is pure epoxy resin, b be test one obtain the orderly apertures carbon nano tube/epoxy resin composite material of microstructure.
Embodiment
Embodiment one: a kind of microstructure improved containing hole composite material bore edges abrasion resistance properties of present embodiment is carried out according to the following steps containing the preparation method of hole composite material in order:
One, carbon nanotube acidifying process: by dense HNO 3with dense H 2sO 4at room temperature Homogeneous phase mixing, then carbon nanotube is added, and under temperature is 50 ~ 70 DEG C and rotating speed is the condition of 1200r/min ~ 1500r/min, stir 4h ~ 6h, supersound process 2h ~ 4h under ultrasonic frequency is 80Hz ~ 100Hz again, obtain acid solidliquid mixture, then the acid solidliquid mixture deionized water obtained being diluted to pH value is 0.8 ~ 1.2, then suction filtration is carried out, filtrate is discarded after suction filtration, and use deionized water wash solid matter, carry out suction filtration and washing again, until the filtrate pH value after suction filtration is 6.8 ~ 7.2, obtain solid matter, be dry 20h ~ 24h under the condition of 80 DEG C ~ 100 DEG C in temperature by the solid matter obtained, obtain the carbon nanotube after acidifying, dense HNO described in step one 3with dense H 2sO 4volume ratio be 1:(2 ~ 4), the quality of the carbon nanotube described in step one and dense HNO 3volume ratio be 1g:(6 ~ 9) mL,
Two, the preparation of the carbon nanotube of surface magnetism particle modification: the carbon nanotube after the acidifying 1. step one obtained puts into strong aqua, supersound process 1h ~ 3h under ultrasonic frequency is 80Hz ~ 100Hz, obtains carbon nanotube/ammoniacal liquor suspension, 2. be 10 in vacuum tightness -3pa ~ 1.5 × 10 -3under the condition of Pa by Iron trichloride hexahydrate and ferrous chloride hydrate dissolution in deionized water, Fe is obtained 3+/ Fe 2+mixing solutions, 3. be 10 in vacuum tightness -3pa ~ 1.5 × 10 -32. the Fe will obtained under the condition of Pa 3+/ Fe 2+mixing solutions joins 1. in the carbon nanotube/ammoniacal liquor suspension obtained, and obtains mixing solutions after mixing, and is then 10 in vacuum tightness -3pa ~ 1.5 × 10 -3under the condition of Pa, first Viscotrol C being warming up to temperature is 60 ~ 80 DEG C, then the mixing solutions obtained is joined in Viscotrol C, 3h ~ 5h is stirred again under temperature is 80 ~ 90 DEG C and rotating speed is 150r/min ~ 200r/min, complete reaction, obtain the carbon nano-tube solution that surface magnetism particle is modified, by carbon nano-tube solution centrifugal 4min ~ 6min under rotating speed is 11000r/min ~ 13000r/min that the surface magnetism particle obtained is modified, abandoning supernatant, and the solid matter obtained is purified, purify 2 ~ 4 dry 10h ~ 14h of final vacuum, obtain the carbon nanotube that surface magnetism particle is modified, purification processes described in step 2 is: first use absolute ethanol washing solid matter, then under ultrasonic frequency is 80Hz ~ 100Hz, processes 8min ~ 12min, then carries out magnetic resolution, step 2 1. described in the acidifying that obtains of step one after the quality of carbon nanotube be (3 ~ 5) mg:1mL with the ratio of the volume of strong aqua, step 2 2. described in Iron trichloride hexahydrate be (1 ~ 3) with the ratio of the amount of substance of ferrous chloride hydrate: 1, step 2 2. described in the amount of substance of Iron trichloride hexahydrate be 0.004mol:(4 ~ 6 with the ratio of the volume of deionized water) mL, step 2 3. described in carbon nanotube/ammoniacal liquor suspension of 1. obtaining of step 2 and the Fe that 2. obtains of step 2 3+/ Fe 2+the ratio of the volume of mixing solutions is (3 ~ 5): 1, step 2 3. described in mixing solutions be 1:(15 ~ 22 with the ratio of the volume of Viscotrol C),
Three, the preparation of the orderly apertures carbon nano tube/epoxy resin composite material of microstructure: the carbon nanotube that surface magnetism particle epoxy resin, dehydrated alcohol and step 2 3. obtained is modified mixes, then be the condition down cut 30min ~ 50min of 8000r/min ~ 10000r/min at rotating speed with high-speed shearing emulsion machine, add after quadrol mixes again, obtaining cured product, is then 10 at normal temperature and vacuum tightness -3pa ~ 10 -5under the condition of Pa, cured product being placed on magneticstrength is leave standstill 40min ~ 60min in the uniform magnetic field of 0.4T ~ 1T, then be dry 20h ~ 24h under the condition of 60 DEG C ~ 80 DEG C in temperature, obtain the orderly apertures carbon nano tube/epoxy resin composite material of microstructure; Epoxy resin wherein described in step 3 and the mass ratio of dehydrated alcohol are 100:(18 ~ 25); The mass ratio of the carbon nanotube that the surface magnetism particle that 3. epoxy resin described in step 3 and step 2 obtain is modified is 1000:(1 ~ 20); The mass ratio of the quadrol described in step 3 and epoxy resin is 1:(10 ~ 12).
The method of present embodiment adopts first carries out acidification by carbon nanotube, carbon nanotube after acidifying is put into strong aqua, prepare carbon nanotube/ammoniacal liquor suspension, then Iron trichloride hexahydrate and ferrous chloride hydrate are dissolved in deionized water under vacuum, prepare magnetic particle Fe 3+/ Fe 2+'smixing solutions, then by Fe 3+/ Fe 2+mixing solutions joins in carbon nanotube/ammoniacal liquor suspension, join after mixing in the Viscotrol C of preheating, again through centrifugal, purify and drying, obtain the carbon nanotube that surface magnetism particle is modified, finally by epoxy resin, the carbon nanotube that dehydrated alcohol and surface magnetism particle are modified mixes, sheared by high-speed shearing emulsion machine, solidify through quadrol again, then cured product is placed in uniform magnetic field and leaves standstill, again after drying, obtain the orderly apertures carbon nano tube/epoxy resin composite material of microstructure, prepared by present embodiment contains hole composite material, compare traditional bore edges reinforcement, quality is light, abrasion resistance properties improves about 77%, thus the work-ing life effectively extended containing hole composite material, and carbon nanotube is Orienting ordered arrangement in the epoxy, the resistance to air loss of this arrangement meeting reinforced composite in order, the enhancing design of perforate matrix material can be applied to.
Embodiment two: present embodiment and embodiment one are unlike the dense HNO described in step one 3with dense H 2sO 4volume ratio be 1:3; The quality of the carbon nanotube described in step one and dense HNO 3volume ratio be 1g:8mL.Other step is identical with embodiment one with parameter.
Embodiment three: present embodiment and embodiment one or two unlike: step 2 1. described in the acidifying that obtains of step one after the quality of carbon nanotube be 4mg:1mL with the ratio of the volume of strong aqua.Other step is identical with embodiment one or two with parameter.
Embodiment four: one of present embodiment and embodiment one to three unlike: step 2 2. described in Iron trichloride hexahydrate be 2:1 with the ratio of the amount of substance of ferrous chloride hydrate.Other step is identical with one of parameter and embodiment one to three.
Embodiment five: one of present embodiment and embodiment one to four unlike: step 2 2. described in the amount of substance of Iron trichloride hexahydrate be 0.004mol:5mL with the ratio of the volume of deionized water.Other step is identical with one of parameter and embodiment one to four.
Embodiment six: one of present embodiment and embodiment one to five unlike: step 2 3. described in carbon nanotube/ammoniacal liquor suspension of 1. obtaining of step 2 and the Fe that 2. obtains of step 2 3+/ Fe 2+the ratio of the volume of mixing solutions is 4:1.Other step is identical with one of parameter and embodiment one to five.
Embodiment seven: one of present embodiment and embodiment one to six unlike: step 2 3. described in mixing solutions be 1:(15 ~ 20 with the ratio of the volume of Viscotrol C).Other step is identical with one of parameter and embodiment one to six.
Embodiment eight: one of present embodiment and embodiment one to seven unlike: the mass ratio of the epoxy resin described in step 3 and dehydrated alcohol is 5:1.Other step is identical with one of parameter and embodiment one to seven.
Embodiment nine: one of present embodiment and embodiment one to eight unlike: the mass ratio of the carbon nanotube that the surface magnetism particle that 3. epoxy resin described in step 3 and step 2 obtain is modified is 1000:(3 ~ 20).Other step is identical with one of parameter and embodiment one to eight.
Embodiment ten: one of present embodiment and embodiment one to nine unlike: the mass ratio of the quadrol described in step 3 and epoxy resin is 1:11.Other step is identical with one of parameter and embodiment one to nine.
With following verification experimental verification beneficial effect of the present invention:
Test one, a kind of preparation method improving the microstructure containing hole composite material bore edges abrasion resistance properties and contain hole composite material in order, is characterized in that a kind of microstructure improved containing hole composite material bore edges abrasion resistance properties is carried out according to the following steps containing the preparation method of hole composite material in order:
One, carbon nanotube acidifying process: by dense for 10mL HNO 3h dense with 30mL 2sO 4at room temperature Homogeneous phase mixing, then 1.8g carbon nanotube is added, and under temperature is 70 DEG C and rotating speed is the condition of 1500r/min, stir 4h, supersound process 3h under ultrasonic frequency is 100Hz again, obtain acid solidliquid mixture, then the acid solidliquid mixture deionized water obtained being diluted to pH value is 1, then suction filtration is carried out, filtrate is discarded after suction filtration, and use deionized water wash solid matter, carry out suction filtration and washing again, until the filtrate pH value after suction filtration is 7, obtain solid matter, be dry 24h under the condition of 80 DEG C in temperature by the solid matter obtained, obtain the carbon nanotube after acidifying,
Two, the preparation of the carbon nanotube of surface magnetism particle modification: the carbon nanotube after the acidifying 1. 0.1g step one obtained puts into 30mL strong aqua, supersound process 1h under ultrasonic frequency is 80Hz, obtains carbon nanotube/ammoniacal liquor suspension; 2. be 10 in vacuum tightness -3under the condition of Pa by 5.4g Iron trichloride hexahydrate and 2g ferrous chloride hydrate dissolution in 5mL deionized water, obtain Fe 3+/ Fe 2+3. mixing solutions is 10 in vacuum tightness -3under the condition of Pa by 5mL 2. in the Fe that obtains 3+/ Fe 2+mixing solutions join 30mL 1. in carbon nanotube/ammoniacal liquor suspension of obtaining, obtaining mixing solutions after mixing, is then 10 in vacuum tightness -3under the condition of Pa, first 450mL Viscotrol C being warming up to temperature is 80 DEG C, then the mixing solutions obtained is joined in Viscotrol C, 3h is stirred again under temperature is 80 DEG C and rotating speed is 150r/min, complete reaction, obtain the carbon nano-tube solution that surface magnetism particle is modified, by carbon nano-tube solution centrifugal 5min under rotating speed is 11000r/min that the surface magnetism particle obtained is modified, abandoning supernatant, and the solid matter obtained is purified, purify 3 dry 10h of final vacuum, obtains the carbon nanotube that surface magnetism particle is modified; Purification processes described in step 2 is: first use absolute ethanol washing solid matter, then under ultrasonic frequency is 80Hz, processes 10min, then carries out magnetic resolution;
Three, the preparation of the orderly apertures carbon nano tube/epoxy resin composite material of microstructure: the carbon nanotube that surface magnetism particle 50g epoxy resin, 10mL dehydrated alcohol and 1.5g step 2 3. obtained is modified mixes, then be the condition down cut 30min of 10000r/min at rotating speed with high-speed shearing emulsion machine, add after 6g quadrol mixes again, obtaining cured product, is then 10 at normal temperature and vacuum tightness -3under the condition of Pa, cured product being placed on magneticstrength is leave standstill 60min in the uniform magnetic field of 0.4T, is then dry 24h under the condition of 80 DEG C in temperature, obtains the orderly apertures carbon nano tube/epoxy resin composite material of microstructure.
Fig. 1 is the arrangement schematic diagram of test one, and after the action of a magnetic field, carbon nanotube is Orienting ordered arrangement in the epoxy, successfully the obtained structurally ordered nano composite material of carbon nanotube reinforced epoxy, the resistance to air loss of this arrangement meeting reinforced composite in order.
Model is adopted to be that MVF-1A friction wear testing machine carries out friction and wear behavior detection to the orderly apertures carbon nano tube/epoxy resin composite material of microstructure that test one obtains, and by pure epoxy resin material as a control group, obtain friction and wear test graphic representation as shown in table 2; Wherein a is pure epoxy resin, b is the orderly apertures carbon nano tube/epoxy resin composite material of microstructure that test one obtains, and can be drawn the performance of friction and wear behavior far above pure epoxy resin of the orderly apertures carbon nano tube/epoxy resin composite material of microstructure by Fig. 2.

Claims (10)

1. improve the preparation method that the microstructure containing hole composite material bore edges abrasion resistance properties contains hole composite material in order, it is characterized in that a kind of microstructure improved containing hole composite material bore edges abrasion resistance properties is carried out according to the following steps containing the preparation method of hole composite material in order:
One, carbon nanotube acidifying process: by dense HNO 3with dense H 2sO 4at room temperature Homogeneous phase mixing, then carbon nanotube is added, and under temperature is 50 ~ 70 DEG C and rotating speed is the condition of 1200r/min ~ 1500r/min, stir 4h ~ 6h, supersound process 2h ~ 4h under ultrasonic frequency is 80Hz ~ 100Hz again, obtain acid solidliquid mixture, then the acid solidliquid mixture deionized water obtained being diluted to pH value is 0.8 ~ 1.2, then suction filtration is carried out, filtrate is discarded after suction filtration, and use deionized water wash solid matter, carry out suction filtration and washing again, until the filtrate pH value after suction filtration is 6.8 ~ 7.2, obtain solid matter, be dry 20h ~ 24h under the condition of 80 DEG C ~ 100 DEG C in temperature by the solid matter obtained, obtain the carbon nanotube after acidifying, dense HNO described in step one 3with dense H 2sO 4volume ratio be 1:(2 ~ 4), the quality of the carbon nanotube described in step one and dense HNO 3volume ratio be 1g:(6 ~ 9) mL,
Two, the preparation of the carbon nanotube of surface magnetism particle modification: the carbon nanotube after the acidifying 1. step one obtained puts into strong aqua, supersound process 1h ~ 3h under ultrasonic frequency is 80Hz ~ 100Hz, obtains carbon nanotube/ammoniacal liquor suspension, 2. be 10 in vacuum tightness -3pa ~ 1.5 × 10 -3under the condition of Pa by Iron trichloride hexahydrate and ferrous chloride hydrate dissolution in deionized water, Fe is obtained 3+/ Fe 2+mixing solutions, 3. be 10 in vacuum tightness -3pa ~ 1.5 × 10 -32. the Fe will obtained under the condition of Pa 3+/ Fe 2+mixing solutions joins 1. in the carbon nanotube/ammoniacal liquor suspension obtained, and obtains mixing solutions after mixing, and is then 10 in vacuum tightness -3pa ~ 1.5 × 10 -3under the condition of Pa, first Viscotrol C being warming up to temperature is 60 ~ 80 DEG C, then the mixing solutions obtained is joined in Viscotrol C, 3h ~ 5h is stirred again under temperature is 80 ~ 90 DEG C and rotating speed is 150r/min ~ 200r/min, complete reaction, obtain the carbon nano-tube solution that surface magnetism particle is modified, by carbon nano-tube solution centrifugal 4min ~ 6min under rotating speed is 11000r/min ~ 13000r/min that the surface magnetism particle obtained is modified, abandoning supernatant, and the solid matter obtained is purified, purify 2 ~ 4 dry 10h ~ 14h of final vacuum, obtain the carbon nanotube that surface magnetism particle is modified, purification processes described in step 2 is: first use absolute ethanol washing solid matter, then under ultrasonic frequency is 80Hz ~ 100Hz, processes 8min ~ 12min, then carries out magnetic resolution, step 2 1. described in the acidifying that obtains of step one after the quality of carbon nanotube be (3 ~ 5) mg:1mL with the ratio of the volume of strong aqua, step 2 2. described in Iron trichloride hexahydrate be (1 ~ 3) with the ratio of the amount of substance of ferrous chloride hydrate: 1, step 2 2. described in the amount of substance of Iron trichloride hexahydrate be 0.004mol:(4 ~ 6 with the ratio of the volume of deionized water) mL, step 2 3. described in carbon nanotube/ammoniacal liquor suspension of 1. obtaining of step 2 and the Fe that 2. obtains of step 2 3+/ Fe 2+the ratio of the volume of mixing solutions is (3 ~ 5): 1, step 2 3. described in mixing solutions be 1:(15 ~ 22 with the ratio of the volume of Viscotrol C),
Three, the preparation of the orderly apertures carbon nano tube/epoxy resin composite material of microstructure: the carbon nanotube that surface magnetism particle epoxy resin, dehydrated alcohol and step 2 3. obtained is modified mixes, then be the condition down cut 30min ~ 50min of 8000r/min ~ 10000r/min at rotating speed with high-speed shearing emulsion machine, add after quadrol mixes again, obtaining cured product, is then 10 at normal temperature and vacuum tightness -3pa ~ 10 -5under the condition of Pa, cured product being placed on magneticstrength is leave standstill 40min ~ 60min in the uniform magnetic field of 0.4T ~ 1T, then be dry 20h ~ 24h under the condition of 60 DEG C ~ 80 DEG C in temperature, obtain the orderly apertures carbon nano tube/epoxy resin composite material of microstructure; Epoxy resin wherein described in step 3 and the mass ratio of dehydrated alcohol are 100:(18 ~ 25); The mass ratio of the carbon nanotube that the surface magnetism particle that 3. epoxy resin described in step 3 and step 2 obtain is modified is 1000:(1 ~ 20); The mass ratio of the quadrol described in step 3 and epoxy resin is 1:(10 ~ 12).
2. a kind of preparation method improving the microstructure containing hole composite material bore edges abrasion resistance properties and contain hole composite material in order according to claim 1, is characterized in that the dense HNO described in step one 3with dense H 2sO 4volume ratio be 1:3; The quality of the carbon nanotube described in step one and dense HNO 3volume ratio be 1g:8mL.
3. a kind of preparation method improving the microstructure containing hole composite material bore edges abrasion resistance properties and contain hole composite material in order according to claim 1 and 2, is characterized in that the quality of carbon nanotube after the acidifying that the step one described in step 2 1. obtains is 4mg:1mL with the ratio of the volume of strong aqua.
4. a kind of preparation method improving the microstructure containing hole composite material bore edges abrasion resistance properties and contain hole composite material in order according to claim 3, is characterized in that the Iron trichloride hexahydrate described in step 2 is 2. 2:1 with the ratio of the amount of substance of ferrous chloride hydrate.
5. a kind of preparation method improving the microstructure containing hole composite material bore edges abrasion resistance properties and contain hole composite material in order according to claim 3, is characterized in that the amount of substance of Iron trichloride hexahydrate described in step 2 is 2. 0.004mol:5mL with the ratio of the volume of deionized water.
6. a kind of preparation method improving the microstructure containing hole composite material bore edges abrasion resistance properties and contain hole composite material in order according to claim 3, is characterized in that carbon nanotube/ammoniacal liquor suspension that 1. step 2 described in step 2 3. obtains and the Fe that 2. step 2 obtains 3+/ Fe 2+the ratio of the volume of mixing solutions is 4:1.
7. a kind of preparation method improving the microstructure containing hole composite material bore edges abrasion resistance properties and contain hole composite material in order according to claim 3, is characterized in that the mixing solutions described in step 2 is 3. 1:(15 ~ 20 with the ratio of the volume of Viscotrol C).
8. a kind of preparation method improving the microstructure containing hole composite material bore edges abrasion resistance properties and contain hole composite material in order according to claim 3, is characterized in that the mass ratio of the epoxy resin described in step 3 and dehydrated alcohol is 5:1.
9. a kind of preparation method improving the microstructure containing hole composite material bore edges abrasion resistance properties and contain hole composite material in order according to claim 3, is characterized in that the mass ratio of the carbon nanotube that the surface magnetism particle that 3. epoxy resin described in step 3 and step 2 obtain is modified is 1000:(3 ~ 20).
10. a kind of preparation method improving the microstructure containing hole composite material bore edges abrasion resistance properties and contain hole composite material in order according to claim 3, is characterized in that the mass ratio of the quadrol described in step 3 and epoxy resin is 1:11.
CN201310572198.6A 2013-11-15 2013-11-15 A kind of preparation method improving the microstructure containing hole composite material bore edges abrasion resistance properties and contain hole composite material in order Expired - Fee Related CN103602041B (en)

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CN105111723B (en) * 2015-09-28 2017-08-25 哈尔滨工业大学 A kind of preparation method of the orderly magnetic boron nitride nanosheet/compound polyurethane material of surface micro-structure
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