CN112143986A - Preparation method of directionally-distributed prestressed carbon fiber reinforced aluminum matrix composite - Google Patents
Preparation method of directionally-distributed prestressed carbon fiber reinforced aluminum matrix composite Download PDFInfo
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- C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
- C22C47/08—Making alloys containing metallic or non-metallic fibres or filaments by contacting the fibres or filaments with molten metal, e.g. by infiltrating the fibres or filaments placed in a mould
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- C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
- C22C47/02—Pretreatment of the fibres or filaments
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- C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
- C22C49/02—Alloys containing metallic or non-metallic fibres or filaments characterised by the matrix material
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- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/06—Electrolytic production, recovery or refining of metals by electrolysis of melts of aluminium
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Abstract
The invention relates to the field of aluminum alloy preparation, and discloses a preparation method of a directionally-distributed prestressed carbon fiber reinforced aluminum matrix composite, which comprises the following steps: (1) applying pretension to the carbon fibers arranged in the same direction, and fixing the carbon fibers by using a mold to obtain the carbon fibers arranged in a directional manner; (2) pouring a water solution of a surfactant into the mold, fully soaking, and drying to obtain the carbon fiber coated with the surfactant; (3) and pouring aluminum liquid into the mold, and cooling after ultrasonic oscillation to obtain the carbon fiber reinforced aluminum matrix composite. According to the preparation method, the surfactant is coated outside the carbon fibers, so that the compatibility between the carbon fibers and an aluminum matrix can be effectively improved, and the mechanical property and the heat conduction property of the composite material are improved.
Description
Technical Field
The invention relates to the field of aluminum alloy preparation, in particular to a preparation method of a directionally distributed prestressed carbon fiber reinforced aluminum matrix composite.
Background
The aluminum-based composite material is a common metal-based composite material, has the advantages of small density, light weight, good plasticity, easy processing and good high-temperature performance, has good physical and mechanical properties compared with other materials, and is very suitable for preparing high-thermal-conductivity and high-mechanical-strength materials for power systems. Carbon Fiber Reinforced Aluminum Matrix Composites (Cf/Al Composites for short) are a general name of composite materials in which Carbon fibers are used as a reinforcement and Aluminum or Aluminum alloy is used as a Matrix, have the advantages of good wear resistance, low thermal expansion coefficient, excellent electrical and thermal conductivity and the like, and are widely applied to the fields of aerospace, automobiles, electronic instruments, civil appliances and the like.
The combination mode and structure of the Cf/Al interface play an important role in load transfer between the matrix and the carbon fiber in the composite material. The carbon fiber of the reinforcement has a plurality of excellent performances, but the performances can be fully utilized only by the good combination of the carbon fiber and the aluminum matrix, and the carbon fiber and the aluminum matrix can be completely wetted only at 1000 ℃, but at the temperature, the oxidation reaction of the carbon fiber is strong, and the damage is very serious. On the other hand, the interface reaction progresses at high temperature, and interface bonding is improved, but Al is formed4N3The thermal conductivity is low (140W/m.K), and large interface thermal resistance is caused. The problem of poor interface identity influences the mechanical property and the heat-conducting property of the carbon fiber reinforced aluminum matrix composite.
Chinese patent publication No. CN108866457B discloses a method for preparing a continuous carbon fiber reinforced aluminum matrix composite, comprising the following steps: (1) plating copper on the surface of the monofilament of the carbon fiber to obtain a prepreg; (2) immersing the prepreg in an organic adhesive for 5-10 s, taking out, repeatedly vibrating the prepreg adhered with the organic adhesive in aluminum powder to obtain a primary impregnating material with the surface of the carbon fiber monofilament uniformly adhered with the aluminum powder, and curing the organic adhesive on the primary impregnating material to obtain a carbon fiber primary material; (3) immersing the carbon fiber primary material into the organic adhesive again for 5-10 s, taking out, then repeatedly vibrating in aluminum powder to obtain secondary immersion material with the surface of the carbon fiber monofilament uniformly adhered with the aluminum powder, and curing the organic adhesive on the secondary immersion material to obtain a carbon fiber secondary material; (4) repeating the step (3), and adhering multiple layers of aluminum powder to obtain a carbon fiber composite material with the diameter of 0.5-1 mm; (5) and putting a plurality of layers of the carbon fiber composite material in parallel in a hot-pressing die of a vacuum hot-pressing sintering furnace, and performing vacuum hot-pressing sintering to obtain the carbon fiber reinforced aluminum-based composite material. The method improves the interface wettability between aluminum and carbon fibers by plating copper on the surface of the carbon fibers, but compared with a Cf/Al composite material, the copper has lower thermal conductivity (401W/m.K) and can influence the thermal conductivity of the composite material. Therefore, a simple and efficient method for improving the compatibility of the Cf/Al interface to obtain the aluminum matrix composite with high thermal conductivity and high mechanical property is still lacking at present.
Disclosure of Invention
In order to solve the technical problem, the invention provides a preparation method of a directionally distributed prestressed carbon fiber reinforced aluminum matrix composite. The method can effectively improve the compatibility between the carbon fiber and the aluminum matrix and improve the mechanical property and the heat-conducting property of the composite material.
The specific technical scheme of the invention is as follows:
a preparation method of a directionally distributed prestressed carbon fiber reinforced aluminum matrix composite material comprises the following steps:
(1) applying pretension to the carbon fibers arranged in the same direction, and fixing the carbon fibers by using a mold to obtain the carbon fibers arranged in a directional manner;
(2) pouring a water solution of a surfactant into the mold, fully soaking, and drying to obtain the carbon fiber coated with the surfactant;
(3) and pouring aluminum liquid into the mold, and cooling after ultrasonic oscillation to obtain the carbon fiber reinforced aluminum matrix composite.
According to the invention, the surface of the carbon fiber is coated with the surfactant and then mixed with the aluminum liquid, so that the interfacial tension between the carbon fiber and the aluminum liquid can be reduced, the interfacial wettability is improved, and the interfacial bonding between the carbon fiber and the aluminum matrix is improved; meanwhile, after the aluminum liquid is poured, the diffusion of the aluminum liquid on the surface of the carbon fiber is promoted through ultrasonic vibration, and the Cf/Al interface combination can be further promoted. The improvement of the Cf/Al interface combination can effectively transfer load from the aluminum matrix to the carbon fiber and prevent the carbon fiber and the aluminum matrix from being stripped when being pulled, thereby improving the tensile property of the carbon fiber reinforced aluminum matrix composite material, and the improvement of the interface combination can also reduce the interface thermal resistance and improve the heat conducting property of the composite material.
In addition, the carbon fibers are directionally distributed by applying the pretension, so that the longitudinal tensile strength of the composite material can be effectively improved; and because the heat conduction of the carbon fibers has obvious anisotropy, the axial heat conductivity is very high, and the radial heat conductivity is very low, the advantage of one-dimensional high heat conductivity can be exerted by directionally distributing the carbon fibers, and the longitudinal heat conductivity of the composite material is improved.
Preferably, in the step (1), the pretension is 10 to 100N.
Preferably, in the step (2), the surfactant is at least one of stearic acid, sodium dodecylbenzenesulfonate, lecithin and alkyl glucoside.
Preferably, in the step (2), the mass fraction of the aqueous solution of the surfactant is 5 to 50 wt.%.
Preferably, in the step (2), the soaking time is 30-120 min.
Preferably, in the step (3), the time of the ultrasonic oscillation is 10-60 min.
Preferably, in step (1), the carbon fiber is a sheath-core structure carbon fiber comprising a core and a sheath; the core is carbon fiber, and the skin is aluminum/carbon composite material.
According to the invention, the carbon fiber is designed into a skin-core structure, and the aluminum/carbon composite material skin is combined with the aluminum matrix, so that the compatibility between the carbon fiber and the aluminum matrix can be improved, and the Cf/Al interface combination is improved, thereby improving the tensile strength and the thermal conductivity of the composite material; the carbon content in the carbon fiber can be improved through the carbon fiber core part, so that the reinforcing effect of the carbon fiber on the composite material can be better exerted.
Further, the diameter of the core part is 3-5 μm; the thickness of the skin layer is 1-2 mu m.
Further, the preparation method of the skin-core structure carbon fiber comprises the following steps:
(A) carrying out melt spinning on the asphalt to prepare carbon fiber precursor;
(B) pre-oxidizing carbon fiber precursors at 200-400 ℃ in an air atmosphere;
(C) impregnating the carbon fiber precursor with a mixed solution of aluminum sol and molten asphalt to obtain carbon fibers coated with the aluminum sol and the molten asphalt; the mass ratio of the aluminum sol to the molten asphalt is 1: 3-5;
(D) pre-oxidizing the carbon fiber subjected to the dipping treatment at 200-400 ℃ in an air atmosphere;
(E) carbonizing the carbon fiber subjected to preoxidation treatment at 800-1200 ℃ in a nitrogen atmosphere;
(F) laying the carbonized carbon fiber on the bottom of an electrolytic tank as a cathode, taking a carbon material as an anode and taking molten cryolite as electrolyte to carry out electrolysis; and after the electrolysis is finished, taking out the carbon fiber, and cooling to obtain the carbon fiber with the skin-core structure.
After the carbon fiber precursor is pre-oxidized (stabilized), a mixed layer of alumina sol and molten pitch is coated outside the precursor by a dip coating method. In the subsequent pre-oxidation process, polyacrylonitrile in the outer layer mixing layer undergoes a series of complex reactions and is converted into a pyridine ring trapezoidal structure which is thermally stable and has a semiconductor resistance value, and meanwhile, the outer layer aluminum sol is dried and solidified. After carbonization, the aluminum oxide on the outer layer is converted into aluminum by electrolysis, and the specific process is as follows: during electrolysis, the alumina of the outer layer of the carbon fiber and the AlF in the molten cryolite6 3-Reaction to Al2OF6 2-，Al2OF6 2-Entering into electrolyte to form pores outside the carbon fiber, AlF6 3-And reducing the cathode into aluminum, filling the aluminum liquid into pores of the outer layer of the carbon fiber, and cooling to obtain the carbon fiber with the core part of the carbon fiber and the skin-core structure with the skin layer of the aluminum/carbon composite material. During electrolysis, carbon dioxide is generated at the anode, and whether the electrolysis is finished can be judged according to whether bubbles emerge from the anode.
The reason why the aluminum sol is adopted instead of the simple aluminum in the step (B) is that the simple aluminum has a low melting point (660 ℃), and flows away due to melting during carbonization, and aluminum in the aluminum sol exists in the form of aluminum oxide, the melting point of the aluminum oxide reaches 2054 ℃, and the aluminum oxide can still exist stably during high-temperature carbonization. In addition, the porosity of the aluminum sol enables the aluminum sol to form a porous framework in the skin layer, so that the contact area of aluminum and the carbon material in the skin layer is increased, and the compatibility between carbon fibers and an aluminum matrix in the composite material is better improved.
Further, the leather layer sequentially comprises an inner layer, a middle layer and an outer layer from inside to outside, and the aluminum content of the inner layer, the middle layer and the outer layer is sequentially increased; the diameter of the core part is 3-5 mu m, and the thicknesses of the inner layer, the middle layer and the outer layer are all 1-2 mu m.
Further, the preparation method of the skin-core structure carbon fiber comprises the following steps:
(a) carrying out melt spinning on the asphalt to prepare carbon fiber precursor;
(b) pre-oxidizing carbon fiber precursors at 200-400 ℃ in an air atmosphere;
(c) impregnating the carbon fiber precursor with a mixed solution of aluminum sol and molten asphalt to obtain carbon fibers coated with a first layer of aluminum sol and molten asphalt; the mass ratio of the aluminum sol to the molten asphalt is 1: 4.5-6.5;
(d) pre-oxidizing the carbon fiber subjected to the dipping treatment in the step (c) at 200-400 ℃ in an air atmosphere;
(e) dipping the carbon fiber subjected to the pre-oxidation treatment in the step (d) by using a mixed solution of aluminum sol and molten asphalt to obtain a second layer of aluminum sol and molten asphalt-coated carbon fiber; the mass ratio of the aluminum sol to the molten asphalt is 1: 2-4.5;
(f) pre-oxidizing the carbon fiber subjected to the dipping treatment in the step (e) at 200-400 ℃ in an air atmosphere;
(g) dipping the carbon fiber subjected to the pre-oxidation treatment in the step (f) by using a mixed solution of aluminum sol and molten asphalt to obtain a carbon fiber coated with a third layer of aluminum sol and molten asphalt; the mass ratio of the aluminum sol to the molten asphalt is 1: 1-2;
(h) pre-oxidizing the carbon fiber subjected to the dipping treatment in the step (g) at 200-400 ℃ in an air atmosphere;
(i) carbonizing the carbon fiber subjected to the pre-oxidation treatment in the step (h) at 800-1200 ℃ in a nitrogen atmosphere;
(j) laying the carbonized carbon fiber on the bottom of an electrolytic tank as a cathode, taking a carbon material as an anode and taking molten cryolite as electrolyte to carry out electrolysis; and after the electrolysis is finished, taking out the carbon fiber, and cooling to obtain the carbon fiber with the skin-core structure.
By repeating the steps of dipping and pre-oxidation, three layers of skins are wrapped outside the carbon fiber core, and the aluminum content from the inner layer to the outer layer is sequentially increased, the compatibility among the core, the skins and the aluminum matrix can be further improved through the gradient transition, the Cf/Al interface combination is improved, and the tensile strength and the thermal conductivity of the composite material are improved.
Preferably, in the step (F) or the step (j), the mass ratio of the cathode to the molten cryolite is 1:2 to 2.5.
Preferably, in the step (C) or the step (C) or the step (e) or the step (g), the impregnation time is 30 to 40 min.
Preferably, in the step (B), the step (D), the step (B), the step (D), the step (f) or the step (h), the pre-oxidation time is 30-40 min.
Preferably, in the step (E) or the step (i), the carbonization time is 3-6 h.
Preferably, in the step (F) or the step (j), the voltage of the electrolysis is 3.5 to 4.5V.
Compared with the prior art, the invention has the following advantages:
(1) by coating with a surfactant and ultrasonic vibration, the interface bonding between the carbon fiber and the aluminum matrix can be improved, and the tensile property and the heat conductivity of the composite material are improved;
(2) the carbon fibers are directionally distributed by applying the pretension, so that the longitudinal tensile property and the longitudinal thermal conductivity of the composite material can be improved;
(3) by adopting the carbon fiber with the skin-core structure, the compatibility between the carbon fiber and the aluminum matrix can be improved, and the tensile property and the thermal conductivity of the composite material are further improved.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples.
General examples
A preparation method of a directionally distributed prestressed carbon fiber reinforced aluminum matrix composite material comprises the following steps (as shown in figure 1):
(1) applying 10-100N pretension to a plurality of strands of carbon fibers arranged in the same direction, and fixing the carbon fibers by using a mold to obtain the carbon fibers arranged in a directional manner;
(2) pouring 5-50 wt.% of surfactant aqueous solution into a mold, soaking for 30-120 min, and drying to obtain the surfactant-coated carbon fiber; the surfactant is at least one of stearic acid, sodium dodecyl benzene sulfonate, lecithin and alkyl glucoside;
(3) and pouring aluminum liquid into the mold, oscillating for 10-60 min by using 500-1000W of ultrasonic waves, and cooling to obtain the carbon fiber reinforced aluminum matrix composite.
Optionally, in step (1), the carbon fiber is a sheath-core structure carbon fiber comprising a core and a skin; the core is made of carbon fiber, and the skin layer is made of aluminum/carbon composite material; the diameter of the core is 3-5 mu m, and the thickness of the skin layer is 1-2 mu m. The preparation method of the skin-core structure carbon fiber comprises the following steps:
(A) carrying out melt spinning on the asphalt to prepare carbon fiber precursor;
(B) pre-oxidizing carbon fiber precursors at 200-400 ℃ in an air atmosphere for 30-40 min;
(C) impregnating the carbon fiber precursor with a mixed solution of aluminum sol and molten asphalt for 30-40 min to obtain carbon fibers coated with the aluminum sol and the molten asphalt; the mass ratio of the aluminum sol to the molten asphalt is 1: 3-5;
(D) pre-oxidizing the carbon fiber subjected to the dipping treatment for 30-40 min at 200-400 ℃ in an air atmosphere;
(E) carbonizing the carbon fiber subjected to preoxidation treatment for 3-6 hours at 800-1200 ℃ in a nitrogen atmosphere;
(F) laying the carbonized carbon fibers at the bottom of an electrolytic tank as a cathode, taking a carbon material as an anode and molten cryolite as electrolyte, wherein the mass ratio of the cathode to the molten cryolite is 1: 2-2.5, and electrolyzing at a voltage of 3.5-4.5V; and after the electrolysis is finished, taking out the carbon fiber, and cooling to obtain the carbon fiber with the skin-core structure.
Optionally, in step (1), the carbon fiber is a sheath-core structure carbon fiber comprising a core and a skin; the core is made of carbon fiber, and the skin layer is made of aluminum/carbon composite material; the cortex sequentially comprises an inner layer, a middle layer and an outer layer from inside to outside, and the aluminum content of the inner layer, the middle layer and the outer layer is sequentially increased; the diameter of the core part is 3-5 mu m, and the thicknesses of the inner layer, the middle layer and the outer layer are all 1-2 mu m. The preparation method of the skin-core structure carbon fiber comprises the following steps:
(a) carrying out melt spinning on the asphalt to prepare carbon fiber precursor;
(b) pre-oxidizing carbon fiber precursors at 200-400 ℃ in an air atmosphere for 30-40 min;
(c) impregnating the carbon fiber precursor with a mixed solution of aluminum sol and molten asphalt for 30-40 min to obtain carbon fibers coated with a first layer of aluminum sol and molten asphalt; the mass ratio of the aluminum sol to the molten asphalt is 1: 4.5-6.5;
(d) pre-oxidizing the carbon fiber subjected to the dipping treatment in the step (c) for 30-40 min at 200-400 ℃ in an air atmosphere;
(e) dipping the carbon fiber subjected to the pre-oxidation treatment in the step (d) by using a mixed solution of aluminum sol and molten asphalt for 30-40 min to obtain a second layer of aluminum sol and molten asphalt coated carbon fiber; the mass ratio of the aluminum sol to the molten asphalt is 1: 2-4.5;
(f) pre-oxidizing the carbon fiber subjected to the dipping treatment in the step (e) for 30-40 min at 200-400 ℃ in an air atmosphere;
(g) dipping the carbon fiber subjected to the pre-oxidation treatment in the step (f) by using a mixed solution of aluminum sol and molten asphalt to obtain a carbon fiber coated with a third layer of aluminum sol and molten asphalt; the mass ratio of the aluminum sol to the molten asphalt is 1: 1-2;
(h) pre-oxidizing the carbon fiber subjected to the dipping treatment in the step (g) at 200-400 ℃ in an air atmosphere;
(i) carbonizing the carbon fiber subjected to the pre-oxidation treatment in the step (e) for 3-6 hours at 800-1200 ℃ in a nitrogen atmosphere;
(j) laying the carbonized carbon fibers at the bottom of an electrolytic tank as a cathode, taking a carbon material as an anode and molten cryolite as electrolyte, wherein the mass ratio of the cathode to the molten cryolite is 1: 2-2.5, and electrolyzing at a voltage of 3.5-4.5V; and after no bubble emerges from the anode, taking out the carbon fiber, and cooling to obtain the carbon fiber with the skin-core structure.
Example 1
A preparation method of a directionally distributed prestressed carbon fiber reinforced aluminum matrix composite material comprises the following steps:
(1) applying 50N pretension to 10 strands of carbon fibers arranged in the same direction, and fixing the carbon fibers by using a mold to obtain the carbon fibers arranged in a directional manner;
(2) pouring 30 wt.% aqueous solution of stearic acid into the mold, soaking for 60min, and drying to obtain the carbon fiber coated with the surfactant;
(3) and pouring aluminum liquid into the mold, oscillating for 40min by using 800W ultrasonic wave, and cooling to obtain the carbon fiber reinforced aluminum matrix composite.
Example 2
The preparation was carried out according to the procedure of example 1, except that the magnitude of the pretension in the step (1) was 10N.
Example 3
The preparation was carried out according to the procedure of example 1, except that the magnitude of the pretension in the step (1) was 30N, as in example 1.
Example 4
The preparation was carried out according to the procedure of example 1, except that the magnitude of the pretension in the step (1) was 70N.
Example 5
Prepared according to the procedure of example 1, except that stearic acid in the step (2) is replaced with sodium dodecylbenzenesulfonate, as in example 1.
Example 6
Prepared according to the procedure of example 1, except that stearic acid in the step (2) is replaced with lecithin, as in example 1.
Example 7
Prepared according to the procedure of example 1, except that stearic acid in the step (2) is replaced with C16 alkyl glucoside, as in example 1.
Example 8
Prepared according to the procedure of example 1, differing from example 1 in that the mass fraction of the aqueous stearic acid solution in the step (2) is 10 wt.%.
Example 9
Prepared according to the procedure of example 1, differing from example 1 in that the mass fraction of the aqueous stearic acid solution in said step 2) is 20 wt.%.
Example 10
Prepared according to the procedure of example 1, differing from example 1 in that the mass fraction of the aqueous stearic acid solution in said step 2) is 40 wt.%.
Example 11
The preparation was carried out by following the procedure of example 1, differing from example 1 in that the time of ultrasonic oscillation in said step (3) was 20 min.
Example 12
The preparation was carried out by following the procedure of example 1, differing from example 1 in that the time of ultrasonic oscillation in said step (3) was 30 min.
Example 13
The preparation was carried out by following the procedure of example 1, differing from example 1 in that the time of ultrasonic oscillation in said step (3) was 50 min.
Example 14
The carbon fiber is prepared according to the steps of example 1, and is different from example 1 in that the carbon fiber in the step (1) adopts a skin-core structure carbon fiber, and the preparation method comprises the following steps:
(A) carrying out melt spinning on the asphalt to prepare carbon fiber precursor;
(B) pre-oxidizing carbon fiber precursors for 35min at 300 ℃ in an air atmosphere;
(C) impregnating the carbon fiber precursor with a mixed solution of aluminum sol and molten asphalt for 35min to obtain carbon fibers coated with the aluminum sol and the molten asphalt; the mass ratio of the aluminum sol to the molten asphalt is 1: 4;
(D) pre-oxidizing the carbon fiber subjected to the dipping treatment at 300 ℃ for 35min in an air atmosphere;
(E) carbonizing the carbon fiber subjected to preoxidation treatment for 5 hours at 1000 ℃ in a nitrogen atmosphere;
(F) laying the carbonized carbon fiber at the bottom of an electrolytic tank as a cathode, taking graphite as an anode and molten cryolite as electrolyte, wherein the mass ratio of the cathode to the molten cryolite is 1:2, and electrolyzing at 4V; and after no bubble emerges from the anode, taking out the carbon fiber, and cooling to obtain the carbon fiber with the skin-core structure.
The core diameter of the prepared carbon fiber with the skin-core structure is 5 mu m, and the skin thickness is 1.5 +/-0.5 mu m.
Example 15
The carbon fiber is prepared according to the steps of example 1, and is different from example 1 in that the carbon fiber in the step (1) adopts a skin-core structure carbon fiber, and the preparation method comprises the following steps:
(a) carrying out melt spinning on the asphalt to prepare carbon fiber precursor;
(b) pre-oxidizing carbon fiber precursors for 35min at 300 ℃ in an air atmosphere;
(c) impregnating the carbon fiber precursor with a mixed solution of alumina sol and molten asphalt for 35min to obtain carbon fibers coated with a first layer of alumina sol and molten asphalt; the mass ratio of the aluminum sol to the molten asphalt is 1: 5.5;
(d) pre-oxidizing the carbon fiber subjected to the dipping treatment in the step (c) for 35min at 300 ℃ in an air atmosphere;
(e) dipping the carbon fiber subjected to the pre-oxidation treatment in the step (d) by using a mixed solution of aluminum sol and molten asphalt, wherein the dipping time is 35min, and obtaining carbon fiber coated with a second layer of aluminum sol and molten asphalt; the mass ratio of the aluminum sol to the molten asphalt is 1: 3;
(f) pre-oxidizing the carbon fiber subjected to the dipping treatment in the step (e) for 35min at 200-400 ℃ in an air atmosphere;
(g) dipping the carbon fiber subjected to the pre-oxidation treatment in the step (f) for 35min by using a mixed solution of aluminum sol and molten asphalt to obtain a carbon fiber coated with a third layer of aluminum sol and molten asphalt; the mass ratio of the aluminum sol to the molten asphalt is 1: 1.5;
(h) pre-oxidizing the carbon fiber subjected to the dipping treatment in the step (g) at 300 ℃ in an air atmosphere;
(i) carbonizing the carbon fiber subjected to the pre-oxidation treatment in the step (e) for 5 hours at 1000 ℃ in a nitrogen atmosphere;
(j) laying the carbonized carbon fiber at the bottom of an electrolytic tank as a cathode, taking graphite as an anode and molten cryolite as electrolyte, wherein the mass ratio of the cathode to the molten cryolite is 1:2, and electrolyzing at 4V; and after no bubble emerges from the anode, taking out the carbon fiber, and cooling to obtain the carbon fiber with the skin-core structure.
The core diameter of the prepared skin-core structure carbon fiber is 3 μm, and the thicknesses of the inner layer, the middle layer and the outer layer of the skin layer are 1.5 +/-0.5 μm.
Comparative example 1
The preparation was carried out by following the procedure of example 1, differing from example 1 in that step (2) was not carried out.
The longitudinal tensile strength and the longitudinal thermal conductivity of the carbon fiber reinforced aluminum matrix composite materials prepared in the examples 1 to 15 and the comparative example 1 are tested, and the test results are shown in table 1.
TABLE 1 mechanical and thermal conductivity of the products of examples 1-15 and comparative example 1
| Sample (I) | Longitudinal tensile strength (MPa) | Longitudinal thermal conductivity (W/m. K) |
| Example 1 | 725 | 810 |
| Example 2 | 532 | 734 |
| Example 3 | 614 | 776 |
| Example 4 | 632 | 763 |
| Example 5 | 639 | 753 |
| Example 6 | 652 | 687 |
| Example 7 | 638 | 768 |
| Example 8 | 614 | 736 |
| Example 9 | 678 | 721 |
| Example 10 | 638 | 790 |
| Example 11 | 634 | 765 |
| Example 12 | 685 | 775 |
| Example 13 | 573 | 689 |
| Example 14 | 831 | 900 |
| Example 15 | 890 | 963 |
| Comparative example 1 | 456 | 593 |
Example 1 on the basis of comparative example 1, carbon fibers are soaked by a surfactant and then mixed with aluminum liquid, so that the tensile strength and the thermal conductivity of the prepared composite material are obviously increased, because: the carbon fibers are coated by the surfactant, so that the interfacial tension between the carbon fibers and the aluminum liquid can be reduced, the interfacial wettability is improved, the interfacial bonding between the carbon fibers and the aluminum matrix is improved, the load can be effectively transferred from the aluminum matrix to the carbon fibers, and the carbon fibers and the aluminum matrix are prevented from being peeled off when being pulled, so that the tensile property of the carbon fiber reinforced aluminum matrix composite material is improved, and the improvement of the interfacial bonding can also reduce the interfacial thermal resistance and improve the heat conducting property of the composite material.
In examples 2 to 13, one of the magnitude of the pretension, the type of the surfactant, the mass fraction of the surfactant aqueous solution, and the time of ultrasonic oscillation is changed on the basis of example 1, and the test results of the composite materials prepared in comparative examples 1 to 13 show that the longitudinal thermal conductivity of the aluminum alloy obtained by adopting the process parameters in example 1 can reach 810W/m.k, the tensile strength can reach 725MPa, and the results are all superior to those of other examples. Therefore, the process parameters of example 1 can be selected as the optimum choice.
Example 14 on the basis of example 1, using carbon fiber of a sheath-core structure, the core of which is carbon fiber and the sheath of which is aluminum/carbon composite, the tensile strength and thermal conductivity of the resulting composite are significantly increased because: the skin layer is used as a transition layer between the carbon fiber and the aluminum matrix, so that the compatibility between the carbon fiber and the aluminum matrix can be improved, the Cf/Al interface combination is improved, and the tensile strength and the thermal conductivity of the composite material are improved.
Example 15 on the basis of example 14, the skin layers are designed to be three layers, the aluminum content is increased from inside to outside, and the tensile strength and the thermal conductivity of the prepared composite material are obviously increased because: the compatibility among the core part, the skin layer and the aluminum matrix can be further improved through gradient transition among the carbon fiber core part, the skin layer inner layer, the middle layer, the outer layer and the aluminum matrix, and Cf/Al interface combination is improved, so that the tensile strength and the thermal conductivity of the composite material are improved.
The raw materials and equipment used in the invention are common raw materials and equipment in the field if not specified; the methods used in the present invention are conventional in the art unless otherwise specified.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, alterations and equivalents of the above embodiments according to the technical spirit of the present invention are still within the protection scope of the technical solution of the present invention.
Claims (10)
1. The preparation method of the directionally distributed prestressed carbon fiber reinforced aluminum matrix composite is characterized by comprising the following steps of:
(1) applying pretension to the carbon fibers arranged in the same direction, and fixing the carbon fibers by using a mold to obtain the carbon fibers arranged in a directional manner;
(2) pouring a water solution of a surfactant into the mold, fully soaking, and drying to obtain the carbon fiber coated with the surfactant;
(3) and pouring aluminum liquid into the mold, and cooling after ultrasonic oscillation to obtain the carbon fiber reinforced aluminum matrix composite.
2. The method for preparing the directionally distributed prestressed carbon fiber reinforced aluminum matrix composite material as claimed in claim 1, wherein in the step (1), the pretension is 10-100N.
3. The method for preparing the directionally distributed prestressed carbon fiber reinforced aluminum matrix composite material as claimed in claim 1, wherein:
in the step (2), the surfactant is at least one of stearic acid, sodium dodecyl benzene sulfonate, lecithin and alkyl glucoside; and/or
In the step (2), the mass fraction of the aqueous solution of the surfactant is 5-50 wt.%.
4. The method for preparing the directionally distributed prestressed carbon fiber reinforced aluminum matrix composite material as claimed in claim 1, wherein in the step (2), the soaking time is 30-120 min.
5. The method for preparing the directionally distributed prestressed carbon fiber reinforced aluminum matrix composite material as claimed in claim 1, wherein in the step (3), the power of the ultrasonic oscillation is 500-1000W, and the time is 10-60 min.
6. The method for preparing an directionally distributed prestressed carbon fiber reinforced aluminum matrix composite as claimed in claim 1, wherein in step (1), said carbon fibers are skin-core structured carbon fibers comprising a core portion and a skin layer; the core is carbon fiber, and the skin is aluminum/carbon composite material.
7. The method for preparing the directionally distributed prestressed carbon fiber reinforced aluminum matrix composite material as claimed in claim 6, wherein the diameter of said core portion is 3-5 μm; the thickness of the skin layer is 1-2 mu m.
8. The method for preparing the directionally distributed prestressed carbon fiber reinforced aluminum matrix composite material as claimed in claim 7, wherein the method for preparing the carbon fiber with the skin-core structure comprises the following steps:
(A) carrying out melt spinning on the asphalt to prepare carbon fiber precursor;
(B) pre-oxidizing carbon fiber precursors at 200-400 ℃ in an air atmosphere;
(C) impregnating the carbon fiber precursor with a mixed solution of aluminum sol and molten asphalt to obtain carbon fibers coated with the aluminum sol and the molten asphalt; the mass ratio of the aluminum sol to the molten asphalt is 1: 3-5;
(D) pre-oxidizing the carbon fiber subjected to the dipping treatment at 200-400 ℃ in an air atmosphere;
(E) carbonizing the carbon fiber subjected to preoxidation treatment at 800-1200 ℃ in a nitrogen atmosphere;
(F) laying the carbonized carbon fiber on the bottom of an electrolytic tank as a cathode, taking a carbon material as an anode and taking molten cryolite as electrolyte to carry out electrolysis; and after the electrolysis is finished, taking out the carbon fiber, and cooling to obtain the carbon fiber with the skin-core structure.
9. The method for preparing the directionally distributed prestressed carbon fiber reinforced aluminum-based composite material as claimed in claim 6, wherein the skin layer comprises an inner layer, a middle layer and an outer layer in sequence from inside to outside, and the aluminum content of the inner layer, the middle layer and the outer layer is increased in sequence; the diameter of the core part is 3-5 mu m, and the thicknesses of the inner layer, the middle layer and the outer layer are all 1-2 mu m.
10. The method for preparing the directionally distributed prestressed carbon fiber reinforced aluminum matrix composite material as claimed in claim 9, wherein the method for preparing the carbon fiber with the skin-core structure comprises the following steps:
(a) carrying out melt spinning on the asphalt to prepare carbon fiber precursor;
(b) pre-oxidizing carbon fiber precursors at 200-400 ℃ in an air atmosphere;
(c) impregnating the carbon fiber precursor with a mixed solution of aluminum sol and molten asphalt to obtain carbon fibers coated with a first layer of aluminum sol and molten asphalt; the mass ratio of the aluminum sol to the molten asphalt is 1: 4.5-6.5;
(d) pre-oxidizing the carbon fiber subjected to the dipping treatment in the step (c) at 200-400 ℃ in an air atmosphere;
(e) dipping the carbon fiber subjected to the pre-oxidation treatment in the step (d) by using a mixed solution of aluminum sol and molten asphalt to obtain a second layer of aluminum sol and molten asphalt-coated carbon fiber; the mass ratio of the aluminum sol to the molten asphalt is 1: 2-4.5;
(f) pre-oxidizing the carbon fiber subjected to the dipping treatment in the step (e) at 200-400 ℃ in an air atmosphere;
(g) dipping the carbon fiber subjected to the pre-oxidation treatment in the step (f) by using a mixed solution of aluminum sol and molten asphalt to obtain a carbon fiber coated with a third layer of aluminum sol and molten asphalt; the mass ratio of the aluminum sol to the molten asphalt is 1: 1-2;
(h) pre-oxidizing the carbon fiber subjected to the dipping treatment in the step (g) at 200-400 ℃ in an air atmosphere;
(i) carbonizing the carbon fiber subjected to the pre-oxidation treatment in the step (h) at 800-1200 ℃ in a nitrogen atmosphere;
(j) laying the carbonized carbon fiber on the bottom of an electrolytic tank as a cathode, taking a carbon material as an anode and taking molten cryolite as electrolyte to carry out electrolysis; and after the electrolysis is finished, taking out the carbon fiber, and cooling to obtain the carbon fiber with the skin-core structure.
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