CN101407433A - Preparation of carbon/carbon composite material molybdenum disilicide outer coating - Google Patents
Preparation of carbon/carbon composite material molybdenum disilicide outer coating Download PDFInfo
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- CN101407433A CN101407433A CNA2008102321355A CN200810232135A CN101407433A CN 101407433 A CN101407433 A CN 101407433A CN A2008102321355 A CNA2008102321355 A CN A2008102321355A CN 200810232135 A CN200810232135 A CN 200810232135A CN 101407433 A CN101407433 A CN 101407433A
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Abstract
The invention relates to a preparation method of a carbon/carbon composite material molybdenum disilicide external coating, which comprises the following steps: the ball-milled molybdenum disilicide powder and isopropanol are mixed in a supersonic generator and vibrated; suspending liquid A is obtained after magnetic stirring; iodine is added to the suspending liquid A and vibrated in the supersonic generator; solution B is obtained after magnetic stirring; the solution B is poured into a hydro-thermal reaction kettle; a carbon/carbon composite material sample with a SiC internal coating is clamped on a cathode clamp inside the hydro-thermal kettle; the hydro-thermal kettle is put in an oven; after the hydrothermal electrophoresis is finished, the sample is cooled to room temperature; and the sample is taken out and dried to obtain the final product, i.e., the carbon/carbon composite material with the protection of the molybdenum disilicide external coating and a carborundum internal coating. The adoption of the hydrothermal electrophoresis precipitation method can prepare the external coating with uniform thickness and without penetrating crackles and millipores. As the reaction is finished in the hydro-thermal kettle once without post heat treatment and carried out at low temperature, the base material is not damaged, the obtained molybdenum disilicide external coating has small internal stress and compact and uniform structure.
Description
Technical field
The present invention relates to a kind of preparation method of molybdenum disilicide outer coating, be specifically related to a kind of preparation method of carbon/carbon composite material molybdenum disilicide outer coating.
Background technology
Carbon/carbon compound material (C/C) becomes the focus of people's research gradually in recent years.Because the carbon/carbon compound material thermal expansivity is low, density is low, anti-ablation, corrosion-resistant, frictional property good, the heat-conductivity conducting performance is good and advantages such as high strength, high-modulus, the characteristic that goes up not down with temperature rising mechanical property particularly, thereby it is widely used in Aeronautics and Astronautics and civilian industry field.Yet only under inert atmosphere or be lower than under 370 ℃ the condition and could keep, oxidation weight loss will make the mechanical property of carbon/carbon compound material obviously descend to its many above-mentioned character, thereby limit the range of application of carbon/carbon compound material widely.Therefore, solving carbon/carbon compound material high temperature oxidation protection question is the prerequisite that makes full use of its performance.
The preparation of high-temperature oxidation resistant coating is considered to one of effective way that solves the carbon/carbon compound material problem of oxidation.Studies show that single coating system is difficult to long-time effectively protection carbon/carbon compound material and avoids oxidation, and because the low characteristics of the carbon/carbon compound material coefficient of expansion can't directly be used most of high temperature materials as coated material.For addressing this problem, mostly adopt the method for introducing transition layer to alleviate the mismatch problems of coated material and carbon/carbon compound material thermal expansivity, prepare high temperature resistant external coating (EC) at excessive laminar surface then, to guarantee the high temperature protection effect of coating.The SiC coating is owing to generally use as transition layer with the good physical chemistry consistency of C/C matrix material.MoSi
2Have 1800 ℃ under the oxidizing atmosphere high-temperature stability and have high-temp plastic and good self-healing ability, make it to become the coating protection material under the high temperature oxidation atmosphere of being used for that receives much attention.Yet MoSi
2Up to 8.1 * 10
-6The thermal expansivity of/K extremely limits its practical application.In conjunction with SiC and MoSi
2Both advantages, the design's method have prepared compact structure and the good MoSi of matrix bond on the SiC-C/C matrices of composite material
2External coating (EC).
At present, good MoSi
2The relevant report of coating is also few, particularly with pure MoSi
2Report as external coating (EC) is more rare, and the preparation method mainly concentrates on entrapping method and molten slurry cladding process.Paying just to wait adopts entrapping method and slip cladding process to prepare MoSi respectively on the C/C matrices of composite material
2-SiC-Si and glass duplex coating system, complicated process of preparation [Fu Qian-Gang, LiHe-Jun
*, Li Ke-Zhi, Shi Xiao-Hong, Huang Min.Carbon.2006,44.].Once employing entrapping method such as mediate banyan had prepared MoSi
2/ SiC compound coating, wherein the SiC undercoat is a vesicular structure, MoSi
2External coating (EC) infiltration wherein inlay in conjunction with [once mediate banyan, Yang Zheng, Li Hejun, Zheng Changqing. aviation journal .1997,18,4.].Entrapping method prepares coating owing to the preparation temperature height, bigger stress, particularly SiC, the MoSi of the inner existence easily of coating
2And thermal expansivity exists than big-difference between the C/C matrices of composite material three, cause coating to occur the rimose phenomenon easily, and this method reaction mechanism complexity, all multifactor influential to reaction and diffusion, so the compactness of coating and homogeneity and coat-thickness are wayward.The molten slurry of employings such as Zhang Yu-Lei cladding process has prepared Si-Mo-Cr complex phase external coating (EC) on the SiC-C/C matrices of composite material, coating preparation needs repeatedly brushing repeatedly once not finish and sample needs later stage thermal treatment, otherwise be difficult to guarantee good combination [Zhang Yu-Lei, the Li He-Jun of coating and body material
*, Fu Qian-Gang, Yao Xi-Yuan, Li Ke-Zhi, Jiao Geng-Sheng.Carbon.2008,46.].Yan Zhi-Qiao etc. adopt the Si-Mo-SiC complex phase coating of chemical Vapor deposition process in conjunction with the preparation of molten slurry cladding process, chemical vapour deposition prepare coating experimental period long, temperature of reaction is higher, destroy C/C matrices of composite material performance easily, and the bonding force of coating and matrix a little less than, coating comes off easily under the influence of factors such as thermal stresses.This complex phase coating number of plies is too much, and complex structure greatly reduces preparation technology's repeatability, reliability [Yan Zhi-Qiao, Xiong Xiang
*, XiaoPeng, Chen Feng, Zhang Hong-Bo, Huang Bai-Yun.Carbon.2008,46.].
Summary of the invention
The objective of the invention is to overcome the shortcoming of above-mentioned prior art, provide a kind of not only preparation cost low, and simple to operate, preparation temperature is low, the cycle is short and do not need the preparation method of heat treated carbon/carbon composite material molybdenum disilicide outer coating of later stage.
For achieving the above object, the technical solution used in the present invention is:
1) selecting commercially available mean particle size is 180 purpose molybdenum disilicide powders, the Virahol of the iodine of purity 〉=99.7% and purity 〉=99.8% is a raw material: at first with molybdenum disilicide powder wet ball grinding 10-60h, the powder that takes by weighing behind the 1-10g ball milling adds in the Erlenmeyer flask, again the Virahol of 100-300ml is poured into and obtained suspension in the Erlenmeyer flask, after again suspension being put into 200-300W ultrasonic generator concussion 30-60min, on magnetic stirring apparatus, stir 12-24h and obtain suspending liquid A;
2) elemental iodine of adding 0.05-0.5g in suspending liquid A, the ultrasonic generator of putting into 200-300W shakes 30-60min, is placed on after the taking-up to stir 12-24h on the magnetic stirring apparatus, makes solution B;
3) above-mentioned solution B is poured in the hydrothermal reaction kettle, compactedness is controlled at 65-75%; To have then on the negative electrode folder of the internally coated carbon/carbon compound material sample holder of SiC in water heating kettle, water heating kettle will be put into baking oven; The positive and negative electrode of water heating kettle is received respectively on the corresponding the two poles of the earth of constant voltage power supply, hydrothermal temperature is controlled at 80-300 ℃ again, and electrophoresis time is controlled at 5-60min, and voltage of supply is controlled at 120-230V, and the hydro-thermal electrophoresis naturally cools to room temperature after finishing;
4) open water heating kettle, take out sample, put it into then in the electric drying oven with forced convection and descend dry 2-4h, promptly get the carbon/carbon compound material sample of final product molybdenum disilicide outer coating protection at 40-100 ℃.
The present invention adopts the water heat electrophoresis deposition method can prepare the thickness homogeneous and does not have through-wall crack and the external coating (EC) of micropore.Owing to be reflected in the water heating kettle and once finish, do not need later stage thermal treatment, and react and carry out at low temperatures, to the body material not damaged, little, the compact and uniform structure of gained molybdenum disilicide outer coating internal stress.And technology is simple, and is easy to operate, and raw material is easy to get, and the gained molybdenum disilicide outer coating is evenly fine and close and matrix bond is good, and reaction time is short, and cost is low; The molybdenum disilicide outer coating of preparation has in the oxygen atmosphere 1500 ℃ of static state and can effectively protect C/C matrix material 500 hours, the oxidative mass loss of sample only 0.8%.
Description of drawings
Fig. 1 prepares molybdenum disilicide outer coating surface (XRD) collection of illustrative plates for the present invention, and wherein X-coordinate is diffraction angle 2 θ, and unit is °; Ordinate zou is a diffraction peak intensity, and unit is a.u.;
Fig. 2 for the present invention 120 ℃ of hydrothermal temperatures, electrophoretic deposition voltage 210V is field emission scanning electron microscope (FE-SEM) photo on preparation carbon/carbon composite material molybdenum disilicide outer coating surface down;
Fig. 3 for the present invention 120 ℃ of hydrothermal temperatures, electrophoretic deposition voltage 210V is section surface sweeping Electronic Speculum (SEM) photo of the silicified molybdenum coating of preparation down.
Embodiment
Below in conjunction with accompanying drawing the present invention is described in further detail.
Embodiment 1: selecting commercially available mean particle size is that the iodine of 180 purpose molybdenum disilicide powders, purity 〉=99.7% and the Virahol of purity 〉=99.8% are raw material: at first the molybdenum disilicide powder 1g behind the wet ball grinding 10h is added in the Erlenmeyer flask, again the Virahol of 250ml is poured into and obtained suspension in the Erlenmeyer flask, after again suspension being put into 300W ultrasonic generator concussion 30min, on magnetic stirring apparatus, stir 12h and obtain suspending liquid A; Add the elemental iodine of 0.05g in suspending liquid A, the ultrasonic generator of putting into 300W shakes 30min, is placed on after the taking-up to stir 12h on the magnetic stirring apparatus, makes solution B; Above-mentioned solution B is poured in the hydrothermal reaction kettle, and compactedness is controlled at 70%; To have then on the negative electrode folder of the internally coated carbon/carbon compound material sample holder of SiC in water heating kettle, water heating kettle will be put into baking oven; The positive and negative electrode of water heating kettle is received respectively on the corresponding the two poles of the earth of constant voltage power supply, hydrothermal temperature is controlled at 100 ℃ again, and electrophoresis time is controlled at 30min, and voltage of supply is controlled at 210V, and the hydro-thermal electrophoresis naturally cools to room temperature after finishing; Open water heating kettle, take out sample, put it into then in the electric drying oven with forced convection and descend dry 3h, promptly get the carbon/carbon compound material sample of final product molybdenum disilicide outer coating protection at 50 ℃.
Embodiment 2: selecting commercially available mean particle size is that the iodine of 180 purpose molybdenum disilicide powders, purity 〉=99.7% and the Virahol of purity 〉=99.8% are raw material: at first the molybdenum disilicide powder 2g behind the wet ball grinding 20h is added in the Erlenmeyer flask, again the Virahol of 200ml is poured into and obtained suspension in the Erlenmeyer flask, after again suspension being put into 250W ultrasonic generator concussion 50min, on magnetic stirring apparatus, stir 16h and obtain suspending liquid A; Add the elemental iodine of 0.2g in suspending liquid A, the ultrasonic generator of putting into 250W shakes 50min, is placed on after the taking-up to stir 16h on the magnetic stirring apparatus, makes solution B; Above-mentioned solution B is poured in the hydrothermal reaction kettle, and compactedness is controlled at 65%; To have then on the negative electrode folder of the internally coated carbon/carbon compound material sample holder of SiC in water heating kettle, water heating kettle will be put into baking oven; The positive and negative electrode of water heating kettle is received respectively on the corresponding the two poles of the earth of constant voltage power supply, hydrothermal temperature is controlled at 160 ℃ again, and electrophoresis time is controlled at 10min, and voltage of supply is controlled at 150V, and the hydro-thermal electrophoresis naturally cools to room temperature after finishing; Open water heating kettle, take out sample, put it into then in the electric drying oven with forced convection and descend dry 2h, promptly get the carbon/carbon compound material sample of final product molybdenum disilicide outer coating protection at 70 ℃.
Embodiment 3: selecting commercially available mean particle size is that the iodine of 180 purpose molybdenum disilicide powders, purity 〉=99.7% and the Virahol of purity 〉=99.8% are raw material: at first the molybdenum disilicide powder 5g behind the wet ball grinding 30h is added in the Erlenmeyer flask, again the Virahol of 150ml is poured into and obtained suspension in the Erlenmeyer flask, after again suspension being put into 230W ultrasonic generator concussion 40min, on magnetic stirring apparatus, stir 20h and obtain suspending liquid A; Add the elemental iodine of 0.1g in suspending liquid A, the ultrasonic generator of putting into 230W shakes 40min, is placed on after the taking-up to stir 20h on the magnetic stirring apparatus, makes solution B; Above-mentioned solution B is poured in the hydrothermal reaction kettle, and compactedness is controlled at 72%; To have then on the negative electrode folder of the internally coated carbon/carbon compound material sample holder of SiC in water heating kettle, water heating kettle will be put into baking oven; The positive and negative electrode of water heating kettle is received respectively on the corresponding the two poles of the earth of constant voltage power supply, hydrothermal temperature is controlled at 200 ℃ again, and electrophoresis time is controlled at 40min, and voltage of supply is controlled at 180V, and the hydro-thermal electrophoresis naturally cools to room temperature after finishing; Open water heating kettle, take out sample, put it into then in the electric drying oven with forced convection and descend dry 4h, promptly get the carbon/carbon compound material sample of final product molybdenum disilicide outer coating protection at 80 ℃.
Embodiment 4: selecting commercially available mean particle size is that the iodine of 180 purpose molybdenum disilicide powders, purity 〉=99.7% and the Virahol of purity 〉=99.8% are raw material: at first the molybdenum disilicide powder 8g behind the wet ball grinding 40h is added in the Erlenmeyer flask, again the Virahol of 100ml is poured into and obtained suspension in the Erlenmeyer flask, after again suspension being put into 200W ultrasonic generator concussion 35min, on magnetic stirring apparatus, stir 14h and obtain suspending liquid A; Add the elemental iodine of 0.3g in suspending liquid A, the ultrasonic generator of putting into 200W shakes 35min, is placed on after the taking-up to stir 14h on the magnetic stirring apparatus, makes solution B; Above-mentioned solution B is poured in the hydrothermal reaction kettle, and compactedness is controlled at 75%; To have then on the negative electrode folder of the internally coated carbon/carbon compound material sample holder of SiC in water heating kettle, water heating kettle will be put into baking oven; The positive and negative electrode of water heating kettle is received respectively on the corresponding the two poles of the earth of constant voltage power supply, hydrothermal temperature is controlled at 300 ℃ again, and electrophoresis time is controlled at 5min, and voltage of supply is controlled at 120V, and the hydro-thermal electrophoresis naturally cools to room temperature after finishing; Open water heating kettle, take out sample, put it into then in the electric drying oven with forced convection and descend dry 2h, promptly get the carbon/carbon compound material sample of final product molybdenum disilicide outer coating protection at 40 ℃.
Embodiment 5: selecting commercially available mean particle size is that the iodine of 180 purpose molybdenum disilicide powders, purity 〉=99.7% and the Virahol of purity 〉=99.8% are raw material: at first the molybdenum disilicide powder 7g behind the wet ball grinding 50h is added in the Erlenmeyer flask, again the Virahol of 270ml is poured into and obtained suspension in the Erlenmeyer flask, after again suspension being put into 250W ultrasonic generator concussion 60min, on magnetic stirring apparatus, stir 24h and obtain suspending liquid A; Add the elemental iodine of 0.4g in suspending liquid A, the ultrasonic generator of putting into 250W shakes 60min, is placed on after the taking-up to stir 24h on the magnetic stirring apparatus, makes solution B; Above-mentioned solution B is poured in the hydrothermal reaction kettle, and compactedness is controlled at 69%; To have then on the negative electrode folder of the internally coated carbon/carbon compound material sample holder of SiC in water heating kettle, water heating kettle will be put into baking oven; The positive and negative electrode of water heating kettle is received respectively on the corresponding the two poles of the earth of constant voltage power supply, hydrothermal temperature is controlled at 240 ℃ again, and electrophoresis time is controlled at 50min, and voltage of supply is controlled at 230V, and the hydro-thermal electrophoresis naturally cools to room temperature after finishing; Open water heating kettle, take out sample, put it into then in the electric drying oven with forced convection and descend dry 3h, promptly get the carbon/carbon compound material sample of final product molybdenum disilicide outer coating protection at 90 ℃.
Embodiment 6: selecting commercially available mean particle size is that the iodine of 180 purpose molybdenum disilicide powders, purity 〉=99.7% and the Virahol of purity 〉=99.8% are raw material: at first the molybdenum disilicide powder 10g behind the wet ball grinding 60h is added in the Erlenmeyer flask, again the Virahol of 300ml is poured into and obtained suspension in the Erlenmeyer flask, after again suspension being put into 280W ultrasonic generator concussion 55min, on magnetic stirring apparatus, stir 22h and obtain suspending liquid A; Add the elemental iodine of 0.5g in suspending liquid A, the ultrasonic generator of putting into 280W shakes 55min, is placed on after the taking-up to stir 22h on the magnetic stirring apparatus, makes solution B; Above-mentioned solution B is poured in the hydrothermal reaction kettle, and compactedness is controlled at 73%; To have then on the negative electrode folder of the internally coated carbon/carbon compound material sample holder of SiC in water heating kettle, water heating kettle will be put into baking oven; The positive and negative electrode of water heating kettle is received respectively on the corresponding the two poles of the earth of constant voltage power supply, hydrothermal temperature is controlled at 80 ℃ again, and electrophoresis time is controlled at 60min, and voltage of supply is controlled at 200V, and the hydro-thermal electrophoresis naturally cools to room temperature after finishing; Open water heating kettle, take out sample, put it into then in the electric drying oven with forced convection and descend dry 4h, promptly get the carbon/carbon compound material sample of final product molybdenum disilicide outer coating protection at 100 ℃.
With Japanese D/max2000PC x-ray diffractometer analytic sample of science, discovery coating gained collection of illustrative plates is molybdenum disilicide diffraction peak (Fig. 1) with the silicified molybdenum coating sample of the present invention preparation.This sample is observed with the field emission JSM-6700F type scanning electronic microscope (Fig. 2) that Japanese JEOL company produces, and from the photo pattern of prepared coatingsurface as can be seen: uniform surface, densification do not have tiny crack to produce.Sample is observed (Fig. 3) with the FEI-QUANTA400 type surface sweeping electron microscope that Dutch FEI Co. produces, find to have prepared fine and close thickness evenly and do not have a molybdenum disilicide outer coating of penetrating crack.
Claims (1)
1, a kind of preparation method of carbon/carbon composite material molybdenum disilicide outer coating is characterized in that:
1) selecting commercially available mean particle size is 180 purpose molybdenum disilicide powders, the Virahol of the iodine of purity 〉=99.7% and purity 〉=99.8% is a raw material: at first with molybdenum disilicide powder wet ball grinding 10-60h, the powder that takes by weighing behind the 1-10g ball milling adds in the Erlenmeyer flask, again the Virahol of 100-300ml is poured into and obtained suspension in the Erlenmeyer flask, after again suspension being put into 200-300W ultrasonic generator concussion 30-60min, on magnetic stirring apparatus, stir 12-24h and obtain suspending liquid A;
2) elemental iodine of adding 0.05-0.5g in suspending liquid A, the ultrasonic generator of putting into 200-300W shakes 30-60min, is placed on after the taking-up to stir 12-24h on the magnetic stirring apparatus, makes solution B;
3) above-mentioned solution B is poured in the hydrothermal reaction kettle, compactedness is controlled at 65-75%; To have then on the negative electrode folder of the internally coated carbon/carbon compound material sample holder of SiC in water heating kettle, water heating kettle will be put into baking oven; The positive and negative electrode of water heating kettle is received respectively on the corresponding the two poles of the earth of constant voltage power supply, hydrothermal temperature is controlled at 80-300 ℃ again, and electrophoresis time is controlled at 5-60min, and voltage of supply is controlled at 120-230V, and the hydro-thermal electrophoresis naturally cools to room temperature after finishing;
4) open water heating kettle, take out sample, put it into then in the electric drying oven with forced convection and descend dry 2-4h, promptly get the carbon/carbon compound material sample of final product molybdenum disilicide outer coating protection at 40-100 ℃.
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| CN101838836A (en) * | 2010-05-25 | 2010-09-22 | 陕西科技大学 | Method for preparing carbon/carbon composite mullite and molybdenum disilicide composite outer coating |
| CN101844936A (en) * | 2010-05-25 | 2010-09-29 | 陕西科技大学 | Method for preparing C/C composite material nanometer silicon carbide-mullite-molybdenum disilicide composite external coating |
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| CN102674901B (en) * | 2012-05-15 | 2014-01-29 | 陕西科技大学 | Preparation method of carbon/carbon material C-AlPO4-mullite-MoSi2 composite outer coating layer |
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| CN105198500A (en) * | 2015-08-28 | 2015-12-30 | 陕西科技大学 | Preparation method of sheet-shaped C/C-MoSi2 composite |
| CN105198500B (en) * | 2015-08-28 | 2017-06-13 | 陕西科技大学 | A kind of laminar C/C MoSi2The preparation method of composite |
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| CN114716268B (en) * | 2022-04-02 | 2022-11-29 | 陕西科技大学 | Preparation of Glass-MoSi on surface of carbon/carbon composite material 2 @Y 2 O 3 Method for preparing-SiC oxidation-resistant coating |
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