CN105113213A - Method for preparation of antioxidant composite coating on carbon fiber surface - Google Patents
Method for preparation of antioxidant composite coating on carbon fiber surface Download PDFInfo
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Abstract
The invention relates to a method for preparation of an antioxidant composite coating on a carbon fiber surface. The antioxidant composite coating is an Al2O3-SiO2-TiO2 composite coating. The method is sol-gel method, which includes: composite sol preparation, carbon fiber surface activation treatment, coating, drying and heat treatment. The composite sol is prepared under room temperature, and the preparation process includes: firstly preparing a water-alcohol solution of tetraethyl orthosilicate and acetic acid into a mixed solution A, then pouring the mixed solution A into an alcohol solution of butyl titanate to prepare a mixed solution B, then under stirring, pouring an alcohol solution of aluminum nitrate nonahydrate into the mixed solution B to prepare a mixed solution C, finally adding an alcohol-water mixed solvent into the mixed solution C, and performing stirring to obtain the composite sol. With the ternary composite sol prepared by the method provided by the invention, a uniform and complete antioxidant coating with good adhesion and thickness within 3 micrometers can be prepared on the carbon fiber surface.
Description
Technical field
The present invention relates to a kind of method preparing anti-oxidation composite coating at carbon fiber surface, belong to technical field of inorganic nonmetallic materials.
Background technology
Carbon fiber (carbonfiber is called for short CF) is the tencel material of the high strength of a kind of phosphorus content more than 95%, high-modulus.Carbon fiber has many premium properties, as: axial strength and modulus high, density is low, higher than performance, without creep, superhigh temperature resistant under non-oxidizing atmosphere, fatigue durability is good, specific heat and electric conductivity are between nonmetal and metal, thermal coefficient of expansion is little and have anisotropy, good corrosion resistance, and X-ray transparent is good, electrical and thermal conductivity performance is good, and electromagnetic wave shielding is good.These characteristics make carbon fiber be used widely in the composite of matrix at materials such as pottery, resin, metal and even carbon.But carbon fiber antioxygenic property is poor, namely occurs in the air more than 400 DEG C that significantly weightless and intensity reduces phenomenon, cause the hydraulic performance decline of material.Moreover, because carbon fiber surface activity is lower, cause the wettability of carbon fiber and some matrix bad, the binding ability without surface-treated carbon fiber and matrix is poor, causes the performance of composite to reduce.
Research shows: preparing ORC at carbon fiber surface can effectively solve the problem, and in addition, selects suitable coating can also play the object of fiber surface modification, the adhesion of fortifying fibre and matrix material.At present, the preparation method of ORC is a lot, comprises chemical vapour deposition technique, physical vaporous deposition and sol-gel process etc.Vapour deposition process needs special gaseous phase deposition stove, and consersion unit is expensive; And sol-gel process to prepare coating not only simple, the even coating problem at each fiber surface in three-dimensional establishment inside and outside can be solved preferably simultaneously.Such as: on March 19th, 2014, Chinese invention patent CN103643481A discloses a kind of preparation method of carbon fiber surface aluminum oxide coating layer, take aluminum nitrate as raw material, adopt sol-gel process, through 75-95 DEG C of hydrolysis, insulation 1-2 hour, forms colloidal sol after the ageing of a period of time, then heat-treat at 1000 DEG C, obtain the α-Al at carbon fiber surface
2o
3oRC.But existing sol-gel process is when preparing colloidal sol, all needs to add thermal agitation and long-time pyrohydrolysis and aging, and there is the high problem of heat treatment temperature; In addition, when preparing the polynary colloidal sol of more than binary and binary, all the colloidal sol taking first to prepare one pack system, and then the one-component colloidal sol of preparation carried out mixing thus obtains polynary colloidal sol, this colloidal sol preparation method not only higher to equipment requirement, waste energy, preparation time is long, and high-temperature heat treatment also can cause Carbon Fiber Damage, reduce the performance of carbon fiber, do not meet energy-conserving and environment-protective requirement simultaneously yet, especially, easily there is crackle and obscission in prepared coating, affects its antioxygenic property.
Summary of the invention
For the problems referred to above that prior art exists, the object of this invention is to provide a kind of method preparing anti-oxidation composite coating at carbon fiber surface, not only meet energy-conserving and environment-protective requirement, and make prepared coating uniform complete and adhesive force good.
For achieving the above object, the technical solution used in the present invention is as follows:
Prepare a method for anti-oxidation composite coating at carbon fiber surface, described anti-oxidation composite coating is Al
2o
3-SiO
2-TiO
2composite coating, described method is sol-gel process, comprising: the preparation of complex sol, to the surface activation process of carbon fiber, coating, dry and heat treatment; It is characterized in that, the preparation of described complex sol comprises the steps:
A) water-alcohol solution of ethyl orthosilicate and acetic acid are at room temperature stirred to it to mix, obtain mixed solution A;
B) mixed solution A obtained is poured in the alcoholic solution of butyl titanate, be at room temperature stirred to it and mix, obtain mixed solution B;
C) under agitation, in mixed solution B, pour the alcoholic solution of ANN aluminium nitrate nonahydrate fast into, be at room temperature stirred to it and mix, obtain mixed solution C;
D) in mixed solution C, add alcohol water mixed solvent, be at room temperature stirred to and obtain described complex sol.
Preferably, step a) described in water-alcohol solution be formed by ethanol and water, the mol ratio of ethyl orthosilicate and second alcohol and water is followed successively by (3.5 ~ 4.5): (15.5 ~ 16.5): (10 ~ 12).
Preferably, step a) described in acetic acid and the mol ratio of ethyl orthosilicate be 1:1.
Preferably, step b) described in the alcoholic solution of butyl titanate be 1:(7 ~ 10 in molar ratio by butyl titanate and ethanol) formed.
Preferably, step c) described in the alcoholic solution of ANN aluminium nitrate nonahydrate be 1:(32 ~ 43 in molar ratio by ANN aluminium nitrate nonahydrate and ethanol) formed.
Preferably, the molal quantity of the water in described complex sol is 2.8 ~ 3.2 times of molal quantity sum of ethyl orthosilicate, butyl titanate, ANN aluminium nitrate nonahydrate.
Preferably, the concentration of described complex sol is 0.3 ~ 0.6mol/L.
Preferably, the mol ratio of the Al:Si:Ti in described complex sol is (0.5 ~ 3): 4:(0.5 ~ 1.5).
Preferably, comprise the steps: carbon fiber to be placed in tube furnace to the surface activation process of carbon fiber, at 380 ~ 420 DEG C, be incubated 30 ~ 40 minutes, to remove the epoxide-resin glue of carbon fiber surface; Carbon fiber after glue is placed in red fuming nitric acid (RFNA) dipping 30 ~ 120 minutes, then adopts deionized water or distilled water to clean at least 3 times to carbon fiber; 2 ~ 4 hours are incubated again at 70 ~ 80 DEG C.
Preferably, described coating refers to the carbon fiber ultrasonic immersing after surface activation process in described complex sol 15 ~ 120 minutes.
Preferably, described drying refers at room temperature dry 18 ~ 24 hours.
Preferably, described heat treatment refers to and carbon fiber is placed in tube furnace, is heated to 550 ~ 750 DEG C under inert gas shielding, is then incubated 1 ~ 2 hour.
As further preferred version, described inert gas is nitrogen or helium, economically considers preferred nitrogen.
As further preferred version, be heated to 550 ~ 750 DEG C with the heating rate of 0.5 ~ 2 DEG C/min.
Preferably, described carbon fiber select in carbon fiber bundle, carbon cloth, three-dimensional carbon fiber preform one or more.
Room temperature of the present invention refers to that indoor temperature is 20 ~ 25 DEG C.
Compared with prior art, the present invention has following conspicuousness beneficial effect:
1, the preparation technology of complex sol of the present invention is simple, whole process is all at room temperature carried out, without the need to adding thermal agitation and mixing time in preparation process, digestion time are short, compared with prior art, total preparation time of colloidal sol at least shortens half, not only simple to operate, without the need to Special Equipment, and economize energy, be applicable to mass production;
2, the present invention adopts described tri compound colloidal sol, can obtain Al under comparatively low heat-treatment temperature (750 DEG C)
2o
3-SiO
2-TiO
2composite coating, not only reduces the requirement to equipment, economize energy, also avoid the damage of heat treatment on carbon fiber and the impact of performance of excessive temperature simultaneously, makes gained coating uniform complete and adhesive force good;
3, in addition, the present invention adopts acetic acid to prepare complex sol, not only safety and environmental protection, also overcomes technology prejudice in the past (in current bibliographical information, when preparing colloidal sol, think that the pH value of solution is larger, sol-hydrolysis speed is faster, adopt acid stronger hydrochloric acid or nitric acid, finally think that the effect of employing nitric acid is best, and acetic acid due to its acidity more weak, the degradation of colloidal sol can be made, hydrolysis prepare colloidal sol poor effect).
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the anti-oxidation composite coating at carbon fiber surface prepared by embodiment 1;
The energy spectrum analysis figure of the anti-oxidation composite coating at carbon fiber surface of Fig. 2 prepared by embodiment 1.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, technical solution of the present invention is described in further detail and completely.
Embodiment 1
Prepare a method for anti-oxidation composite coating at carbon fiber surface, comprise the steps:
(1) preparation of complex sol: precursor ethyl orthosilicate (CAS#78-10-4), butyl titanate (CAS#5593-70-4), ANN aluminium nitrate nonahydrate (CAS#7784-27-2) are prepared tri compound colloidal sol according to Al:Si:Ti=1.5:4:0.5 (mol ratio), is specially:
A) ethyl orthosilicate, acetic acid and distilled water are joined in ethanol successively, at room temperature stir 2 hours, obtain mixed solution A, wherein: ethyl orthosilicate: ethanol: acetic acid: distilled water=4:16:4:11 (mol ratio); According to butyl titanate: ethanol=1:8 (mol ratio), joins butyl titanate in ethanol, at room temperature stir and make it to mix, obtain the ethanolic solution of butyl titanate; According to ANN aluminium nitrate nonahydrate: ethanol=1:35 (mol ratio), joins ANN aluminium nitrate nonahydrate in ethanol, at room temperature stir and make it to mix, obtain the ethanolic solution of ANN aluminium nitrate nonahydrate; According to ethanol: distilled water=1:0.084 (mol ratio), mixes ethanol and distilled water, obtains alcohol water mixed solvent;
B) mixed solution A of 18.93 parts by mass is poured in the ethanolic solution of butyl titanate of 3.40 parts by mass, be at room temperature stirred to it and mix (about 2 ~ 15 seconds), obtain mixed solution B;
C) under agitation, in mixed solution B, pour the ethanolic solution of the ANN aluminium nitrate nonahydrate of 28.56 parts by mass fast into, be at room temperature stirred to it and mix (about 1 hour), obtain mixed solution C;
D) in mixed solution C, add the alcohol water mixed solvent of 49.11 parts by mass, at room temperature stir 40 minutes, leave standstill, namely obtain the complex sol that clear stablizes nothing precipitation, the concentration of described complex sol is 0.5mol/L;
(2) to the surface activation process of carbon fiber: carbon fiber is placed in tube furnace, at 400 DEG C, 35 minutes are incubated, to remove the epoxide-resin glue of carbon fiber surface; By except the impregnated carbon fiber after glue in red fuming nitric acid (RFNA) 90 minutes, then with the nitric acid of distilled water cleaning carbon fiber surface, repeatedly clean five times, at 75 DEG C, be incubated 2 hours after cleaning again (with the moisture that drying removing carbon fiber surface is residual), namely obtain the carbon fiber of surface activation process;
(3) coating and dry: the carbon fiber after step (2) surface activation process is immersed in complex sol prepared by step (1), ultrasonic immersing is after 90 minutes, at room temperature dry 24 hours;
(4) heat treatment: the carbon fiber that step (3) obtains is placed in tube furnace; with the heating rate of 1 DEG C/min in purity for 99.999%; flow is be heated to 750 DEG C under the nitrogen protection of 100mL/min; be incubated after 1 hour; naturally cool to room temperature, surface can be obtained and be coated with Al
2o
3-SiO
2-TiO
2the carbon fiber of anti-oxidation composite coating, the thickness of coating is about 0.75 μm.
The scanning electron microscope (SEM) photograph of the anti-oxidation composite coating at carbon fiber surface of Fig. 1 prepared by the present embodiment, as seen from Figure 1: prepared Al
2o
3-SiO
2-TiO
2anti-oxidation composite coating is evenly complete and adhesive force good.
The energy spectrum analysis figure of the anti-oxidation composite coating at carbon fiber surface of Fig. 2 prepared by the present embodiment, as seen from Figure 2: containing each element of Al, Si, Ti, O in coating, and the mol ratio (0.5:4:1.5) of Al, Si, Ti in the mol ratio of Al, Si, Ti and complex sol closely, illustrate: in colloidal sol preparation process of the present invention, there is no element loss, free from foreign meter in prepared complex sol, and also do not lose through follow-up heat treatment, this also illustrates that preparation method of the present invention all can not cause damage to carbon fiber and coating.
Embodiment 2
The difference of the present embodiment and embodiment 1 is only: " ultrasonic immersing 90 minutes " in step (3) replaced with " ultrasonic immersing 60 minutes ", all the other contents, with described in embodiment 1, finally obtain surface and are coated with Al
2o
3-SiO
2-TiO
2the carbon fiber of anti-oxidation composite coating, the thickness of coating is about 0.55 μm; Detect through ESEM, prepared Al
2o
3-SiO
2-TiO
2anti-oxidation composite coating is as shown in Figure 1: evenly complete and adhesive force good.
Embodiment 3
The difference of the present embodiment and embodiment 1 is only: " ultrasonic immersing 90 minutes " in step (3) replaced with " ultrasonic immersing 60 minutes ", and make carbon fiber repeatedly through twice coating and dry process, and " the 750 DEG C of insulations 1 hour " in step (4) are replaced with " 750 DEG C of insulations 1.5 hours ", all the other contents, with described in embodiment 1, finally obtain surface and are coated with Al
2o
3-SiO
2-TiO
2the carbon fiber of anti-oxidation composite coating, the thickness of coating is about 1.17 μm; Detect through ESEM, prepared Al
2o
3-SiO
2-TiO
2anti-oxidation composite coating is as shown in Figure 1: evenly complete and adhesive force good.
Embodiment 4
Prepare a method for anti-oxidation composite coating at carbon fiber surface, comprise the steps:
(1) preparation of complex sol: precursor ethyl orthosilicate (CAS#78-10-4), butyl titanate (CAS#5593-70-4), ANN aluminium nitrate nonahydrate (CAS#7784-27-2) are prepared tri compound colloidal sol according to Al:Si:Ti=0.5:4:1.5 (mol ratio), is specially:
A) ethyl orthosilicate, acetic acid and distilled water are joined in ethanol successively, at room temperature stir 2 hours, obtain mixed solution A, wherein: ethyl orthosilicate: ethanol: acetic acid: distilled water=4:16:4:11 (mol ratio); According to butyl titanate: ethanol=1:10 (mol ratio), joins butyl titanate in ethanol, at room temperature stir and make it to mix, obtain the ethanolic solution of butyl titanate; According to ANN aluminium nitrate nonahydrate: ethanol=1:40 (mol ratio), joins ANN aluminium nitrate nonahydrate in ethanol, at room temperature stir and make it to mix, obtain the ethanolic solution of ANN aluminium nitrate nonahydrate; According to ethanol: distilled water=1:0.052 (mol ratio), mixes ethanol and distilled water, obtains alcohol water mixed solvent;
B) mixed solution A of 15.97 parts by mass is poured in the ethanolic solution of butyl titanate of 9.71 parts by mass, be at room temperature stirred to it and mix (about 2 ~ 15 seconds), obtain mixed solution B;
C) under agitation, in mixed solution B, pour the ethanolic solution of the ANN aluminium nitrate nonahydrate of 8.96 parts by mass fast into, be at room temperature stirred to it and mix (about 1 hour), obtain mixed solution C;
D) in mixed solution C, add the alcohol water mixed solvent of 65.36 parts by mass, at room temperature stir 50 minutes, leave standstill, namely obtain the complex sol that clear stablizes nothing precipitation, the concentration of described complex sol is 0.4mol/L
(2) to the surface activation process of carbon fiber: carbon fiber is placed in tube furnace, at 420 DEG C, 30 minutes are incubated, to remove the epoxide-resin glue of carbon fiber surface; By except the impregnated carbon fiber after glue in red fuming nitric acid (RFNA) 80 minutes, then with the nitric acid of distilled water cleaning carbon fiber surface, repeatedly clean five times, at 80 DEG C, be incubated 2 hours after cleaning again (with the moisture that drying removing carbon fiber surface is residual), namely obtain the carbon fiber of surface activation process;
(3) coating and dry: the carbon fiber after step (2) surface activation process is immersed in complex sol prepared by step (1), ultrasonic immersing is after 60 minutes, at room temperature dry 20 hours;
(4) heat treatment: the carbon fiber that step (3) obtains is placed in tube furnace; with the heating rate of 2 DEG C/min in purity for 99.999%; flow is be heated to 750 DEG C under the nitrogen protection of 100mL/min; be incubated after 2 hours; naturally cool to room temperature, surface can be obtained and be coated with Al
2o
3-SiO
2-TiO
2the carbon fiber of anti-oxidation composite coating, the thickness of coating is about 0.43 μm; Detect through ESEM, prepared Al
2o
3-SiO
2-TiO
2anti-oxidation composite coating is as shown in Figure 1: evenly complete and adhesive force good.
Owing to containing many kinds of metal ions in the preparation system of multiple elements design colloidal sol, the hydrolysising condition of every metal ion species is different all separately, so that the stability of colloidal sol is difficult to control, and how to prepare the colloidal sol that clarification is uniform and stable, making it not have flocculate, is a difficult thing.
Prepare multiple elements design colloidal sol at present and usually adopt two kinds of methods: 1) single for difference colloidal sol is prepared shaping in advance, the more various colloidal sol configured is formed by different proportion Homogeneous phase mixing; There is the defects such as preparation time length, complex operation in the method; 2) precursor corresponding for component each in complex sol is added in a certain order, be mixed with colloidal sol through stirring after a while and pyrohydrolysis; This kind of direct high temperature is hydrolyzed precursor corresponding to each component simultaneously, although saved the time to a certain extent, the requirement of high-temperature operation to equipment is higher, causes energy waste simultaneously; And during high temperature, colloidal sol can become opaque, and the viscosity of colloidal sol can increase, and causes gel time to shorten, so that the bad stability of complex sol.
And the preparation technology of the multiple elements design colloidal sol that the present invention adopts, not only simple to operate, and whole process is all at room temperature carried out, without the need to adding thermal agitation, total preparation time of colloidal sol at least can shorten half relative to prior art, economize energy, is applicable to mass production; Especially, adopt tri compound colloidal sol of the present invention, Al can be obtained under comparatively low heat-treatment temperature (750 DEG C)
2o
3-SiO
2-TiO
2composite coating, not only reduces the requirement to equipment, economize energy, also avoid the damage of heat treatment on carbon fiber and the impact of performance of excessive temperature simultaneously, makes gained coating uniform complete and adhesive force good.In sum, adopt the inventive method can prepare a kind of uniform and stable tri compound colloidal sol, this colloidal sol is coated in carbon fiber surface, can obtains evenly complete and adhesive force good, the ORC of thickness within 3 μm.
Finally need described herein: be only part preferred embodiment of the present invention above, should be understood that, the present invention also has other embodiment, material mixture ratio in such as change above-described embodiment and parameter value etc., such as acidic catalyst selects nitric acid or hydrochloric acid, aluminium isopropoxide selected by aluminium salt, and alcoholic solvent selects methyl alcohol etc., and this is easy to realize to one skilled in the art.In a word; above content is only for being described in more detail technical scheme of the present invention; can not be interpreted as limiting the scope of the invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.
Claims (10)
1. prepare a method for anti-oxidation composite coating at carbon fiber surface, described anti-oxidation composite coating is Al
2o
3-SiO
2-TiO
2composite coating, described method is sol-gel process, comprising: the preparation of complex sol, to the surface activation process of carbon fiber, coating, dry and heat treatment; It is characterized in that, the preparation of described complex sol comprises the steps:
A) water-alcohol solution of ethyl orthosilicate and acetic acid are at room temperature stirred to it to mix, obtain mixed solution A;
B) mixed solution A obtained is poured in the alcoholic solution of butyl titanate, be at room temperature stirred to it and mix, obtain mixed solution B;
C) under agitation, in mixed solution B, pour the alcoholic solution of ANN aluminium nitrate nonahydrate fast into, be at room temperature stirred to it and mix, obtain mixed solution C;
D) in mixed solution C, add alcohol water mixed solvent, be at room temperature stirred to and obtain described complex sol.
2. the method for claim 1, it is characterized in that: step a) described in water-alcohol solution be formed by ethanol and water, the mol ratio of ethyl orthosilicate and second alcohol and water is followed successively by (3.5 ~ 4.5): (15.5 ~ 16.5): (10 ~ 12), step a) described in acetic acid and the mol ratio of ethyl orthosilicate be 1:1.
3. the method for claim 1, is characterized in that: step b) described in the alcoholic solution of butyl titanate be 1:(7 ~ 10 in molar ratio by butyl titanate and ethanol) formed.
4. the method for claim 1, is characterized in that: step c) described in the alcoholic solution of ANN aluminium nitrate nonahydrate be 1:(32 ~ 43 in molar ratio by ANN aluminium nitrate nonahydrate and ethanol) formed.
5. the method for claim 1, is characterized in that: the molal quantity of the water in described complex sol is 2.8 ~ 3.2 times of molal quantity sum of ethyl orthosilicate, butyl titanate, ANN aluminium nitrate nonahydrate.
6. the method for claim 1, is characterized in that: the concentration of described complex sol is 0.3 ~ 0.6mol/L, and the mol ratio of the Al:Si:Ti in described complex sol is (0.5 ~ 3): 4:(0.5 ~ 1.5).
7. the method for claim 1, is characterized in that, comprises the steps: carbon fiber to be placed in tube furnace to the surface activation process of carbon fiber, is incubated 30 ~ 40 minutes, to remove the epoxide-resin glue of carbon fiber surface at 380 ~ 420 DEG C; Carbon fiber after glue is placed in red fuming nitric acid (RFNA) dipping 30 ~ 120 minutes, then adopts deionized water or distilled water to clean at least 3 times to carbon fiber; 2 ~ 4 hours are incubated again at 70 ~ 80 DEG C.
8. the method for claim 1, is characterized in that: described coating refers to the carbon fiber ultrasonic immersing after surface activation process in described complex sol 15 ~ 120 minutes.
9. the method for claim 1, is characterized in that: described drying refers at room temperature dry 18 ~ 24 hours.
10. the method for claim 1, is characterized in that: described heat treatment refers to and carbon fiber is placed in tube furnace, is heated to 550 ~ 750 DEG C under inert gas shielding, is then incubated 1 ~ 2 hour.
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| CN110176581A (en) * | 2019-04-26 | 2019-08-27 | 广东邦普循环科技有限公司 | The anode material of lithium battery and its preparation method and purposes of a kind of alcohol system titanium Aluminum sol cladding |
| CN110318254A (en) * | 2019-08-11 | 2019-10-11 | 西南石油大学 | A kind of carbon fiber surface HfB2The preparation method of coating |
| CN110318253A (en) * | 2019-08-11 | 2019-10-11 | 西南石油大学 | A kind of preparation method of carbon fiber surface modification anti-oxidation composite coating |
| CN110318254B (en) * | 2019-08-11 | 2021-12-03 | 西南石油大学 | HfB on surface of carbon fiber2Method for producing a coating |
| CN110438589A (en) * | 2019-08-15 | 2019-11-12 | 南京林业大学 | A kind of high heat conducting nano carbon fiber production method |
| CN111250124A (en) * | 2020-02-28 | 2020-06-09 | 松山湖材料实验室 | Preparation method of carrier with composite coating |
| CN111617706A (en) * | 2020-05-28 | 2020-09-04 | 中国科学院化学研究所 | Al (aluminum)2O3-B2O3-SiO2Composite sol, core-shell structure active carbon fiber and preparation method thereof |
| CN111617706B (en) * | 2020-05-28 | 2021-03-12 | 中国科学院化学研究所 | Al (aluminum)2O3-B2O3-SiO2Composite sol, core-shell structure active carbon fiber and preparation method thereof |
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