CN104179003A - Preparation method of carbon nanosphere-carbon fiber multi-scale reinforcement - Google Patents
Preparation method of carbon nanosphere-carbon fiber multi-scale reinforcement Download PDFInfo
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Abstract
The invention discloses a preparation method of a carbon nanosphere-carbon fiber multi-scale reinforcement used for a composite material and having excellent interface adhesion performance. The preparation method comprises the following steps: firstly, uniformly dispersing short chopped carbon fibers into methylcellulose aqueous solution; and with a carbohydrate solution serving as a precursor, performing two steps of hydrothermal reactions, and then growing a layer of carbon nanospheres with controllable particle sizes of 10 to 500nm on site on the surfaces of carbon fibers, thereby obtaining the carbon nanosphere-carbon fiber multi-scale reinforcement. By virtue of the hydrothermal synthesis process with low cost, environmental friendliness, low energy consumption and rapidness, the carbon nanosphere-carbon fiber multi-scale reinforcement is obtained on the premise that no carbon fiber is lost. The carbon nanosphere-carbon fiber multi-scale reinforcement has the advantages of high surface activity, multiple chemical functional groups, good adhesion to a matrix, and the like; the composite material prepared by the multi-scale reinforcement has the advantage that the interlaminar shear strength is enhanced by 35%-45%.
Description
Technical field
The present invention relates to field of nanometer technology, specifically a kind of preparation method of Nano carbon balls-carbon fiber multi-scale reinforcing body.
Background technology
Carbon fiber has the excellent properties such as lightweight, high-strength, Gao Mo, endurance and thermal coefficient of expansion be little, has become one of current most important composite material reinforcement body, and has obtained application in fields such as space flight, aviation and sports equipments.But because carbon fiber surface inertia is large, surface can be low, chemical functional group is few and with the shortcoming such as base bonding property is poor, while making carbon fiber be applied to composite, in interface, there is more defect.Therefore, make carbon fibre composite interlaminar strength low, limited the extensive use in fields such as Aero-Space.
At present, multiple dimensioned carbon reinforcement has been applied in (Metal Substrate, ceramic base, Polymers and C-base composte material) in advanced composite material more and more owing to having had the excellent properties of carbon nano-structured material and traditional fibre reinforcement.Result of study show multiple dimensioned carbon reinforcement can reinforced composite in interface adhesion and interface mechanical strength between matrix and reinforcement.But the existing preparation method of multi-scale reinforcing body only limits to adopt chemical vapor deposition (CVD), electrophoretic deposition (EPD) and chemical graft (CG) to prepare nano structural material at carbon fiber surface.Although these preparation methods can, effectively at carbon fiber surface deposit carbon nano structural material, in preparation process, need to use high temperature and severe chemical treatment, so limited practical application above.Compare the methods such as CVD, EPD and CG, hydrothermal synthesis method is a kind of low cost, environmental friendliness, low energy consumption and preparation method fast.Through domestic and foreign literature retrieval, have not yet to see report and adopt gentle hydrothermal synthesis method to prepare Nano carbon balls-carbon fiber multi-scale reinforcing body.
Summary of the invention
The object of the invention is in order to solve above-mentioned problems of the prior art, and a kind of preparation method of Nano carbon balls-carbon fiber multi-scale reinforcing body of the interface adhesion excellence for composite is provided.
The present invention is achieved through the following technical solutions:
A preparation method for Nano carbon balls-carbon fiber multi-scale reinforcing body, comprises the steps:
(1) first in acetone, the sizing agent of carbon fiber surface is removed, condition is soaking at room temperature 5～10h;
(2) after waiting to soak, carbon fiber is dried to 30～60min at 100～150 DEG C, be cut into afterwards the chopped carbon fiber that length is 3～4mm, then the chopped carbon fiber of 50～100mg is put into the polytetrafluoroethyllining lining of hydrothermal reaction kettle, then the methylated cellulose aqueous solution that is 0.4～1.0wt.% by 450mL mass concentration adds in polytetrafluoroethyllining lining, stirs 10～24h;
(3), after waiting to stir, start to carry out two step hydro-thermal reactions:
the first step: the sugar of 1.1～2.4g is joined in the mixed solution of the above-mentioned chopped carbon fiber stirring and methylated cellulose aqueous solution, after stirring 10～30min, seal, then the flat-temperature zone of reactor being put into air dry oven is warming up to 140～200 DEG C with 5～10 DEG C/min, constant temperature 1～5h afterwards, the complete reactor of opening after cooling of constant temperature, carries out second step hydro-thermal reaction;
second step: the sugar of 0.8～1.5g is joined in the product solution after first step hydro-thermal reaction, after stirring 10～30min, seal, and then the flat-temperature zone of reactor being put into air dry oven is warming up to 140～180 DEG C with 5～10 DEG C/min, constant temperature 5～10h afterwards, the complete reactor of opening after cooling of constant temperature, carries out post processing;
(4) the ultrasonic dispersion 10～30min of product solution step (3) being obtained, then at room temperature after ageing 5～10h, filters, separates, washs and be dried, and finally obtains described Nano carbon balls-carbon fiber multi-scale reinforcing body.
Further, described carbon fiber is polyacrylonitrile-based carbon fibre, asphalt base carbon fiber, viscose base carbon fibre; Described sugar is glucose, sucrose, starch.Carbon fiber can be selected any one in polyacrylonitrile-based carbon fibre, asphalt base carbon fiber, viscose base carbon fibre, and can prepare with a kind of sugar arbitrarily; Sugar can be selected any one in glucose, sucrose, starch, and in the time of first and second step hydro-thermal reaction, can select similar sugar, also can select inhomogeneity sugar.
First the present invention is dispersed in chopped carbon fiber in methylated cellulose aqueous solution, taking sugar juice as presoma, carry out again after two step hydro-thermal reactions, at carbon fiber surface growth in situ one deck Nano carbon balls, particle diameter is controlled, distribution of sizes is at 10～500nm, thereby prepares Nano carbon balls-carbon fiber multi-scale reinforcing body.The present invention using three kinds of different carbon matrix precursors as the carbon source of preparing Nano carbon balls, as glucose, sucrose, starch; Prepare taking three kinds of different presomas simultaneously to carbon fiber as matrix, as polyacrylonitrile-based carbon fibre, asphalt base carbon fiber (comprising isotropism and anisotropic asphalt base carbon fiber), viscose base carbon fibre.
By accompanying drawing in the present invention, as Fig. 2～10, can more clearly find out the modification of surface morphology of carbon fiber before and after two step hydrothermal treatment consists; Fig. 2 is the stereoscan photograph before polyacrylonitrile-based carbon fibre hydrothermal treatment consists, Fig. 3 is the stereoscan photograph before asphalt base carbon fiber hydrothermal treatment consists, Fig. 4 is the stereoscan photograph before viscose base carbon fibre hydrothermal treatment consists, can be found out by above three figure: the carbon fiber surface pattern difference preparing with three kinds of different presomas, but equal defects such as fluted, hole and fine cracks; Further, carbon fiber is after two step hydrothermal treatment consists, the carbon fiber surface preparing at three kinds of different presomas a large amount of closelypacked Nano carbon balls of all having grown, as shown in Fig. 5, Fig. 6 and Fig. 7, by size distribution statistical analysis, can show that Nano carbon balls distribution of sizes is at 10～500nm, as shown in Fig. 8, Fig. 9 and Figure 10.
Beneficial effect of the present invention is:
1) simple, with short production cycle, the instant effect of technique of the present invention, utilize low cost, environmental friendliness, low energy consumption, by the method for Hydrothermal Synthesis fast, do not losing under the prerequisite of carbon fiber,, distribution of sizes controlled at carbon fiber surface growth in situ one deck particle diameter be at the Nano carbon balls of 10～500nm, thereby obtain Nano carbon balls-carbon fiber multi-scale reinforcing body;
2) to have surface-activity large for Nano carbon balls-carbon fiber multi-scale reinforcing body of the present invention, and chemical functional group is many, and with the advantage such as base bonding property is good, the composite of preparing with this multi-scale reinforcing body, interlaminar shear strength has improved 35%～45%.
Brief description of the drawings
Fig. 1 is preparation method's of the present invention flow chart.
Fig. 2 is polyacrylonitrile carbon fiber surface topography map.
Fig. 3 is asphalt base carbon fiber surface topography map.
Fig. 4 is viscose base carbon fibre surface topography map.
Fig. 5 is the distribution shape appearance figure of Nano carbon balls in Nano carbon balls-polyacrylonitrile carbon fiber multi-scale reinforcing body of preparing of the present invention.
Fig. 6 is the particle diameter distribution map of Nano carbon balls in Nano carbon balls-polyacrylonitrile carbon fiber multi-scale reinforcing body of preparing of the present invention.
Fig. 7 is the distribution shape appearance figure of Nano carbon balls in Nano carbon balls-asphalt base carbon fiber multi-scale reinforcing body of preparing of the present invention.
Fig. 8 is the particle diameter distribution map of Nano carbon balls in Nano carbon balls-asphalt base carbon fiber multi-scale reinforcing body of preparing of the present invention.
Fig. 9 is the distribution shape appearance figure of Nano carbon balls in Nano carbon balls-viscose base carbon fibre multi-scale reinforcing body of preparing of the present invention.
Figure 10 is the particle diameter distribution map of Nano carbon balls in Nano carbon balls-viscose base carbon fibre multi-scale reinforcing body of preparing of the present invention.
Detailed description of the invention
Embodiment 1
A preparation method for Nano carbon balls-carbon fiber multi-scale reinforcing body, comprises the steps:
(1) first in acetone, the sizing agent of carbon fiber surface is removed, condition is soaking at room temperature 5h;
(2) after waiting to soak, carbon fiber is dried to 60min at 120 DEG C, be cut into afterwards the chopped carbon fiber that length is 3～4mm, then the chopped carbon fiber of 60mg is put into the polytetrafluoroethyllining lining of hydrothermal reaction kettle, then the methylated cellulose aqueous solution that is 0.8wt.% by 450mL mass concentration adds in polytetrafluoroethyllining lining, stirs 10h;
(3), after waiting to stir, start to carry out two step hydro-thermal reactions:
the first step: the sugar of 1.5g is joined in the mixed solution of the above-mentioned chopped carbon fiber stirring and methylated cellulose aqueous solution, after stirring 10min, seal, then the flat-temperature zone of reactor being put into air dry oven is warming up to 180 DEG C with 5 DEG C/min, constant temperature 5h afterwards, the complete reactor of opening after cooling of constant temperature, carries out second step hydro-thermal reaction;
second step: the sugar of 0.8g is joined in the product solution after first step hydro-thermal reaction, stir after 30min and seal, and then the flat-temperature zone of reactor being put into air dry oven is warming up to 155 DEG C with 8 DEG C/min, constant temperature 5h afterwards, the complete reactor of opening after cooling of constant temperature, carries out post processing;
(4) the ultrasonic dispersion of product solution 25min step (3) being obtained, then at room temperature after ageing 10h, filters, separates, washs and be dried, and finally obtains described Nano carbon balls-carbon fiber multi-scale reinforcing body.
Further, described carbon fiber is polyacrylonitrile-based carbon fibre, and the sugar of first and second step hydro-thermal reaction is glucose.
Embodiment 2
A preparation method for Nano carbon balls-carbon fiber multi-scale reinforcing body, comprises the steps:
(1) first in acetone, the sizing agent of carbon fiber surface is removed, condition is soaking at room temperature 8h;
(2) after waiting to soak, carbon fiber is dried to 40min at 110 DEG C, be cut into afterwards the chopped carbon fiber that length is 3～4mm, then the chopped carbon fiber of 100mg is put into the polytetrafluoroethyllining lining of hydrothermal reaction kettle, then the methylated cellulose aqueous solution that is 1.0wt.% by 450mL mass concentration adds in polytetrafluoroethyllining lining, stirs 20h;
(3), after waiting to stir, start to carry out two step hydro-thermal reactions:
the first step: the sugar of 1.1～2.0g is joined in the mixed solution of the above-mentioned chopped carbon fiber stirring and methylated cellulose aqueous solution, after stirring 25min, seal, then the flat-temperature zone of reactor being put into air dry oven is warming up to 150 DEG C with 8 DEG C/min, constant temperature 2h afterwards, the complete reactor of opening after cooling of constant temperature, carries out second step hydro-thermal reaction;
second step: the sugar of 1.0g is joined in the product solution after first step hydro-thermal reaction, stir after 15min and seal, and then the flat-temperature zone of reactor being put into air dry oven is warming up to 140 DEG C with 6 DEG C/min, constant temperature 9h afterwards, the complete reactor of opening after cooling of constant temperature, carries out post processing;
(4) the ultrasonic dispersion of product solution 30min step (3) being obtained, then at room temperature after ageing 6h, filters, separates, washs and be dried, and finally obtains described Nano carbon balls-carbon fiber multi-scale reinforcing body.
Further, described carbon fiber is viscose base carbon fibre, and the sugar of first step hydro-thermal reaction is glucose, and the sugar of second step hydro-thermal reaction is sucrose.
Embodiment 3
A preparation method for Nano carbon balls-carbon fiber multi-scale reinforcing body, comprises the steps:
(1) first in acetone, the sizing agent of carbon fiber surface is removed, condition is soaking at room temperature 7h;
(2) after waiting to soak, carbon fiber is dried to 35min at 150 DEG C, be cut into afterwards the chopped carbon fiber that length is 3～4mm, then the chopped carbon fiber of 90mg is put into the polytetrafluoroethyllining lining of hydrothermal reaction kettle, then the methylated cellulose aqueous solution that is 0.5wt.% by 450mL mass concentration adds in polytetrafluoroethyllining lining, stirs 15h;
(3), after waiting to stir, start to carry out two step hydro-thermal reactions:
the first step: the sugar of 1.1g is joined in the mixed solution of the above-mentioned chopped carbon fiber stirring and methylated cellulose aqueous solution, after stirring 20min, seal, then the flat-temperature zone of reactor being put into air dry oven is warming up to 140 DEG C with 10 DEG C/min, constant temperature 4h afterwards, the complete reactor of opening after cooling of constant temperature, carries out second step hydro-thermal reaction;
second step: the sugar of 1.5g is joined in the product solution after first step hydro-thermal reaction, stir after 25min and seal, and then the flat-temperature zone of reactor being put into air dry oven is warming up to 170 DEG C with 9 DEG C/min, constant temperature 8h afterwards, the complete reactor of opening after cooling of constant temperature, carries out post processing;
(4) the ultrasonic dispersion of product solution 25min step (3) being obtained, then at room temperature after ageing 9h, filters, separates, washs and be dried, and finally obtains described Nano carbon balls-carbon fiber multi-scale reinforcing body.
Further, described carbon fiber is asphalt base carbon fiber, and the sugar of first step hydro-thermal reaction is starch, and the sugar of second step hydro-thermal reaction is sucrose.
Embodiment 4
A preparation method for Nano carbon balls-carbon fiber multi-scale reinforcing body, comprises the steps:
(1) first in acetone, the sizing agent of carbon fiber surface is removed, condition is soaking at room temperature 10h;
(2) after waiting to soak, carbon fiber is dried to 50min at 100 DEG C, be cut into afterwards the chopped carbon fiber that length is 3～4mm, then the chopped carbon fiber of 70mg is put into the polytetrafluoroethyllining lining of hydrothermal reaction kettle, then the methylated cellulose aqueous solution that is 0.4wt.% by 450mL mass concentration adds in polytetrafluoroethyllining lining, stirs 24h;
(3), after waiting to stir, start to carry out two step hydro-thermal reactions:
the first step: the sugar of 2.4g is joined in the mixed solution of the above-mentioned chopped carbon fiber stirring and methylated cellulose aqueous solution, after stirring 30min, seal, then the flat-temperature zone of reactor being put into air dry oven is warming up to 200 DEG C with 9 DEG C/min, constant temperature 3h afterwards, the complete reactor of opening after cooling of constant temperature, carries out second step hydro-thermal reaction;
second step: the sugar of 0.9g is joined in the product solution after first step hydro-thermal reaction, stir after 20min and seal, and then the flat-temperature zone of reactor being put into air dry oven is warming up to 150 DEG C with 5 DEG C/min, constant temperature 10h afterwards, the complete reactor of opening after cooling of constant temperature, carries out post processing;
(4) the ultrasonic dispersion of product solution 10min step (3) being obtained, then at room temperature after ageing 5h, filters, separates, washs and be dried, and finally obtains described Nano carbon balls-carbon fiber multi-scale reinforcing body.
Further, described carbon fiber is asphalt base carbon fiber, and the sugar of first and second step hydro-thermal reaction is starch.
Embodiment 5
A preparation method for Nano carbon balls-carbon fiber multi-scale reinforcing body, comprises the steps:
(1) first in acetone, the sizing agent of carbon fiber surface is removed, condition is soaking at room temperature 9h;
(2) after waiting to soak, carbon fiber is dried to 30min at 130 DEG C, be cut into afterwards the chopped carbon fiber that length is 3～4mm, then the chopped carbon fiber of 50mg is put into the polytetrafluoroethyllining lining of hydrothermal reaction kettle, then the methylated cellulose aqueous solution that is 0.9wt.% by 450mL mass concentration adds in polytetrafluoroethyllining lining, stirs 13h;
(3), after waiting to stir, start to carry out two step hydro-thermal reactions:
the first step: the sugar of 1.8g is joined in the mixed solution of the above-mentioned chopped carbon fiber stirring and methylated cellulose aqueous solution, after stirring 15min, seal, then the flat-temperature zone of reactor being put into air dry oven is warming up to 190 DEG C with 7 DEG C/min, constant temperature 1h afterwards, the complete reactor of opening after cooling of constant temperature, carries out second step hydro-thermal reaction;
second step: the sugar of 1.4g is joined in the product solution after first step hydro-thermal reaction, stir after 10min and seal, and then the flat-temperature zone of reactor being put into air dry oven is warming up to 180 DEG C with 10 DEG C/min, constant temperature 6h afterwards, the complete reactor of opening after cooling of constant temperature, carries out post processing;
(4) the ultrasonic dispersion of product solution 20min step (3) being obtained, then at room temperature after ageing 7h, filters, separates, washs and be dried, and finally obtains described Nano carbon balls-carbon fiber multi-scale reinforcing body.
Further, described carbon fiber is polyacrylonitrile-based carbon fibre, and the sugar of first and second step hydro-thermal reaction is sucrose.
Embodiment 6
A preparation method for Nano carbon balls-carbon fiber multi-scale reinforcing body, comprises the steps:
(1) first in acetone, the sizing agent of carbon fiber surface is removed, condition is soaking at room temperature 6h;
(2) after waiting to soak, carbon fiber is dried to 55min at 140 DEG C, be cut into afterwards the chopped carbon fiber that length is 3～4mm, then the chopped carbon fiber of 80mg is put into the polytetrafluoroethyllining lining of hydrothermal reaction kettle, then the methylated cellulose aqueous solution that is 0.7wt.% by 450mL mass concentration adds in polytetrafluoroethyllining lining, stirs 18h;
(3), after waiting to stir, start to carry out two step hydro-thermal reactions:
the first step: the sugar of 2.2g is joined in the mixed solution of the above-mentioned chopped carbon fiber stirring and methylated cellulose aqueous solution, after stirring 20min, seal, then the flat-temperature zone of reactor being put into air dry oven is warming up to 160 DEG C with 6 DEG C/min, constant temperature 3h afterwards, the complete reactor of opening after cooling of constant temperature, carries out second step hydro-thermal reaction;
second step: the sugar of 1.2g is joined in the product solution after first step hydro-thermal reaction, stir after 15min and seal, and then the flat-temperature zone of reactor being put into air dry oven is warming up to 160 DEG C with 7 DEG C/min, constant temperature 7h afterwards, the complete reactor of opening after cooling of constant temperature, carries out post processing;
(4) the ultrasonic dispersion of product solution 15min step (3) being obtained, then at room temperature after ageing 8h, filters, separates, washs and be dried, and finally obtains described Nano carbon balls-carbon fiber multi-scale reinforcing body.
Further, described carbon fiber is viscose base carbon fibre, and the sugar of first step hydro-thermal reaction is glucose, and the sugar of second step hydro-thermal reaction is starch.
Claims (2)
1. a preparation method for Nano carbon balls-carbon fiber multi-scale reinforcing body, is characterized in that, comprises the steps:
(1) first in acetone, the sizing agent of carbon fiber surface is removed, condition is soaking at room temperature 5～10h;
(2) after waiting to soak, carbon fiber is dried to 30～60min at 100～150 DEG C, be cut into afterwards the chopped carbon fiber that length is 3～4mm, then the chopped carbon fiber of 50～100mg is put into the polytetrafluoroethyllining lining of hydrothermal reaction kettle, then the methylated cellulose aqueous solution that is 0.4～1.0wt.% by 450mL mass concentration adds in polytetrafluoroethyllining lining, stirs 10～24h;
(3), after waiting to stir, start to carry out two step hydro-thermal reactions:
the first step: the sugar of 1.1～2.4g is joined in the mixed solution of the above-mentioned chopped carbon fiber stirring and methylated cellulose aqueous solution, after stirring 10～30min, seal, then the flat-temperature zone of reactor being put into air dry oven is warming up to 140～200 DEG C with 5～10 DEG C/min, constant temperature 1～5h afterwards, the complete reactor of opening after cooling of constant temperature, carries out second step hydro-thermal reaction;
second step: the sugar of 0.8～1.5g is joined in the product solution after first step hydro-thermal reaction, after stirring 10～30min, seal, and then the flat-temperature zone of reactor being put into air dry oven is warming up to 140～180 DEG C with 5～10 DEG C/min, constant temperature 5～10h afterwards, the complete reactor of opening after cooling of constant temperature, carries out post processing;
(4) the ultrasonic dispersion 10～30min of product solution step (3) being obtained, then at room temperature after ageing 5～10h, filters, separates, washs and be dried, and finally obtains described Nano carbon balls-carbon fiber multi-scale reinforcing body.
2. the preparation method of Nano carbon balls-carbon fiber multi-scale reinforcing body according to claim 1, is characterized in that: described carbon fiber is polyacrylonitrile-based carbon fibre, asphalt base carbon fiber, viscose base carbon fibre; Described sugar is glucose, sucrose, starch.
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| CN104805682A (en) * | 2015-04-17 | 2015-07-29 | 浙江冶金环境保护设计研究有限公司 | Carbon fiber material applied to electro-Fenton system and preparation method of carbon fiber material |
| CN110284321A (en) * | 2019-06-27 | 2019-09-27 | 陕西科技大学 | A kind of glucose modified polyimide fiber and preparation method thereof |
| CN110528271A (en) * | 2019-07-29 | 2019-12-03 | 惠州学院 | A kind of preparation method and applications of char sucrose modified carbon fiber |
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| CN110528271B (en) * | 2019-07-29 | 2021-09-03 | 惠州学院 | Preparation method and application of sucrose carbonization modified carbon fiber |
| CN114575148A (en) * | 2022-04-29 | 2022-06-03 | 中北大学 | Simplified preparation method of graphene conductive fiber cloth and broadband electromagnetic wave absorption composite material thereof |
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| CN117447222A (en) * | 2023-12-26 | 2024-01-26 | 富优特(山东)新材料科技有限公司 | Preparation method of carbon fiber reinforced carbon-based composite material |
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