CN104803696A - High-strength carbon fiber enhanced silicon nitride ceramic matrix composite and preparation method thereof - Google Patents
High-strength carbon fiber enhanced silicon nitride ceramic matrix composite and preparation method thereof Download PDFInfo
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- CN104803696A CN104803696A CN201510169814.2A CN201510169814A CN104803696A CN 104803696 A CN104803696 A CN 104803696A CN 201510169814 A CN201510169814 A CN 201510169814A CN 104803696 A CN104803696 A CN 104803696A
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Abstract
The invention discloses high-strength carbon fiber enhanced silicon nitride ceramic matrix composite and a preparation method thereof. The high-strength carbon fiber enhanced silicon nitride ceramic matrix composite is characterized by being prepared from raw materials in parts by weight as follows: 5-7 parts of germanium oxide, 10-13 parts of modified high-elastic carbon fiber, 50-70 parts of silicon nitride, 3-5 parts of chromium powder, 5-7 parts of methacrylic acid, 0.02-0.04 parts of dicumyl peroxide, 0.4-0.6 parts of 3-amino propyl trimethoxy silane, 8-10 parts of mica powder, 1-3 parts of ammonium polyacrylate, 2-3 parts of bone glue, 20-30 parts of ethyl alcohol and 40-60 parts of deionized water. With modified high-strength carbon fiber as an enhancing phase, the high-strength carbon fiber enhanced silicon nitride ceramic matrix composite has the advantages of excellent oxidation resistance, improvement of ceramic toughness and strength, high-temperature and low-temperature resistance, good thermal conductivity and small expansion coefficient; the added germanium dioxide and chromium powder can be compacted on the ceramic surface, the high-strength carbon fiber enhanced silicon nitride ceramic matrix composite is watertight and gas-tight, surface defects are reduced, the use hardness and the ceramic surface glossiness can be improved, and accordingly, beauty is formed.
Description
Technical field
the present invention relates to a kind of high-strength carbon fibre and strengthen silicon Nitride Ceramic Matrix Composites and preparation method thereof, belong to technical field of ceramic production.
Background technology
It is very high and extremely high temperature resistant that silicon nitride ceramics has high intensity, and its intensity does not decline at the high temperature of 1200 ° of C, can not be melt into melt body after being heated, simultaneously, its resistance to chemical corrosion is excellent, the mineral acid that ability is nearly all and less than 30% caustic soda soln, the also a lot of organic acid corrosion of ability.The deadly defect of stupalith is fragility, under external force, produce stress concentration at material surface or internal tiny crack tip, crack propagation forms surface energy with consumed energy, thus the propagation rate of crackle is extremely rapid, often just makes stupalith suffer catastrophic destruction in moment.Theoretical according to matrix material, when crack propagation runs into fiber, absorb energy by the disengaging of fiber and basal body interface, relax stress concentration; When few fibers fracture occurs under tension stress effect and extracts from matrix, also larger energy will be absorbed.Therefore, FRCMC is a kind of approach of effective solution stupalith fragility.
It is high that high-elastic carbon fiber has intensity, Young's modulus is high, density is little, specific tenacity is high, ability surpasses high and low temperature, acid-alkali-corrosive-resisting is good, thermal expansivity is little, thermal conductivity is large, can the advantage that not easily bursts of resistance to rapid heat cycle, but the shortcoming of high-elastic carbon fiber is easily oxidized under strong acid effect, with can there is metallic carbide, carburizing and galvanic corrosion phenomenon during metal composite, so the present invention adopts gel-pickling process to carry out antioxidation treatment at carbon fiber surface, substantially increase the performance of high-elastic carbon fiber.Carbon fibre reinforced ceramics matrix material has obvious high and low temperature resistance, acid resistance, rub resistance, anti abrasive advantage, good biocompatibility, suitability is wide, and the wild phase as ceramic matrix can ensure the quality of product, can reduce costs again, have the advantage that other materials is incomparable.
Summary of the invention
The object of this invention is to provide a kind of high-strength carbon fibre and strengthen silicon Nitride Ceramic Matrix Composites and preparation method thereof.
In order to realize object of the present invention, the present invention is by following scheme implementation:
A kind of high-strength carbon fibre strengthens silicon Nitride Ceramic Matrix Composites and preparation method thereof, is made up: germanium oxide 5-7, the high-elastic carbon fiber 10-13 of modification, silicon nitride 50-70, chromium powder 3-5, methacrylic acid 5-7, dicumyl peroxide 0.02-0.04,3-aminopropyl trimethoxysilane 0.4-0.6, mica powder 8-10, ammonium polyacrylate 1-3, gelatine 2-3, ethanol 20-30, deionized water 40-60 of the raw material of following weight part;
The preparation method of described modified high-strength carbon fiber is: high-strength carbon fibre is soaked 1-2 hour in nitric acid, uses distilled water flushing 2-3 time, dry for standby after taking out, the ethanol mixing of the tetrabutyl titanate of 10-15 weight part and 150-180 weight part is added in the flask with magnetic stirring apparatus, by the deionized water of 2-3 weight part, the hydrochloric acid of 0.2-0.4 weight part and the ethanol of 2-5 weight part fully mix, slowly be added drop-wise in flask, add the silver oxide powder of 2-4 weight part again, stir 30-40 minute, high-strength carbon fibre for subsequent use is added in gel under vacuum tightness is 0.09-0.1MPa, floods 1-2 hour, dry under 70-80 ° of C after taking-up, repeatable operation like this 2-3 time, last under the protection of high-purity argon gas under 500-600 ° of C pyroreaction 1-2 hour.
A kind of high-strength carbon fibre of the present invention strengthens silicon Nitride Ceramic Matrix Composites and preparation method thereof, is made up of following concrete steps:
(1) silicon nitride, mica powder are added in ball mill, ask as ball-milling medium using aluminum oxide, material ball ratio is 1:2, again methacrylic acid, dicumyl peroxide are added in the mixing solutions of ethanol and deionized water, adding after dissolving after gelatine, ammonium polyacrylate and modified high-strength carbon fiber stir is added in ball mill, ball milling 20-40 minute;
(2) slurry that ball milling obtains is vacuumized, take out and within 2-5 minute, add 3-aminopropyl trimethoxysilane in backward slurry and continue to stir, then slurry to be injected into after in laminated glass mould in vacuum drying oven dry 1-2 hour under 60-80 ° of C;
(3) by the wet base demoulding at room temperature seasoning 1-2 days in step (2), then at 95-100 ° of C temperature, humidity is dry 1-2 days under the condition of 60-70%, remaining one-tenth is distributed into plasma spraying powder conveyer in billet surface spraying evenly;
(4) by the base substrate of step (3) at room temperature with the ramp to 200 of 3-5 ° of C/min ° C, again with the ramp to 600 of 1-2 ° of C/min ° C, constant temperature keeps being positioned in vacuum sintering furnace after 1-2 hour, sinters 3-4 hour, can obtain at the temperature of 1400-1600 ° of C.
Advantage of the present invention is: the present invention adopts modified high-strength carbon fiber as wild phase, have excellent anti-oxidant, strengthen ceramics toughness, intensity, high-low temperature resistant, thermal conductivity is good and the coefficient of expansion is little advantage, the germanium dioxide added and chromium powder can in ceramic surface densifications, waterproof gentle, reduce surface imperfection, and can improve and use hardness and improve ceramic surface glossiness, form aesthetic feeling.
specific embodiments
Below by specific examples, the present invention is described in detail.
A kind of high-strength carbon fibre strengthens silicon Nitride Ceramic Matrix Composites and preparation method thereof, is made up: germanium oxide 6, the high-elastic carbon fiber 12 of modification, silicon nitride 70, chromium powder 4, methacrylic acid 6, dicumyl peroxide 0.04,3-aminopropyl trimethoxysilane 0.6, mica powder 9, ammonium polyacrylate 3, gelatine 3, ethanol 30, deionized water 60 of the raw material of following weight part (kilogram);
The preparation method of described modified high-strength carbon fiber is: high-strength carbon fibre is soaked 2 hours in nitric acid, uses distilled water flushing 3 times, dry for standby after taking out; The ethanol mixing of the tetrabutyl titanate of 15 weight parts and 180 weight parts is added in the flask with magnetic stirring apparatus; the hydrochloric acid of the deionized water of 3 weight parts, 0.4 weight part and the ethanol of 5 weight parts are fully mixed; slowly be added drop-wise in flask; add the silver oxide powder of 4 weight parts again; stir 40 minutes; high-strength carbon fibre for subsequent use is added in gel and floods 1 hour under vacuum tightness is 0.09MPa; dry under 80 ° of C after taking-up; repeatable operation like this 3 times, finally under the protection of high-purity argon gas under 600 ° of C pyroreaction 2 hours.
A kind of high-strength carbon fibre of the present invention strengthens silicon Nitride Ceramic Matrix Composites and preparation method thereof, is made up of following concrete steps:
(1) silicon nitride, mica powder are added in ball mill, ask as ball-milling medium using aluminum oxide, material ball ratio is 1:2, again methacrylic acid, dicumyl peroxide are added in the mixing solutions of ethanol and deionized water, adding after dissolving after gelatine, ammonium polyacrylate and modified high-strength carbon fiber stir is added in ball mill, ball milling 40 minutes;
(2) slurry that ball milling obtains is vacuumized, take out and within 4 minutes, add 3-aminopropyl trimethoxysilane in backward slurry and continue to stir, then slurry to be injected into after in laminated glass mould in vacuum drying oven under 80 ° of C dry 2 hours;
(3) by the wet base demoulding at room temperature seasoning in step (2) 2 days, then at 100 ° of C temperature, humidity under the condition of 60% dry 2 days, is distributed into plasma spraying powder conveyer in billet surface spraying evenly by remaining one-tenth;
(4) by the base substrate of step (3) at room temperature with the ramp to 200 of 3 ° of C/min ° C, again with the ramp to 600 of 1 ° of C/min ° C, constant temperature is positioned in vacuum sintering furnace after keeping 2 hours, sinters 4 hours, can obtain at the temperature of 1600 ° of C.
In the present embodiment, the performance index result of pottery is as follows:
Ultimate compression strength (MPa): >=1000;
Fracture toughness property (Mpa/m
1/2):>=6.5;
Young's modulus (GPa): >=300;
Flexural strength (MPa): >=720;
Thermal expansivity (10
-6/ K):>=3.2.
Claims (2)
1. a high-strength carbon fibre strengthens silicon Nitride Ceramic Matrix Composites and preparation method thereof, it is characterized in that, be made up of the raw material of following weight part: germanium oxide 5-7, the high-elastic carbon fiber 10-13 of modification, silicon nitride 50-70, chromium powder 3-5, methacrylic acid 5-7, dicumyl peroxide 0.02-0.04,3-aminopropyl trimethoxysilane 0.4-0.6, mica powder 8-10, ammonium polyacrylate 1-3, gelatine 2-3, ethanol 20-30, deionized water 40-60;
The preparation method of described modified high-strength carbon fiber is: high-strength carbon fibre is soaked 1-2 hour in nitric acid, uses distilled water flushing 2-3 time, dry for standby after taking out, the ethanol mixing of the tetrabutyl titanate of 10-15 weight part and 150-180 weight part is added in the flask with magnetic stirring apparatus, by the deionized water of 2-3 weight part, the hydrochloric acid of 0.2-0.4 weight part and the ethanol of 2-5 weight part fully mix, slowly be added drop-wise in flask, add the silver oxide powder of 2-4 weight part again, stir 30-40 minute, high-strength carbon fibre for subsequent use is added in gel under vacuum tightness is 0.09-0.1MPa, floods 1-2 hour, dry under 70-80 ° of C after taking-up, repeatable operation like this 2-3 time, last under the protection of high-purity argon gas under 500-600 ° of C pyroreaction 1-2 hour.
2. according to claims 1, a kind of high-strength carbon fibre strengthens silicon Nitride Ceramic Matrix Composites and preparation method thereof, it is characterized in that, is made up of following concrete steps:
(1) silicon nitride, mica powder are added in ball mill, ask as ball-milling medium using aluminum oxide, material ball ratio is 1:2, again methacrylic acid, dicumyl peroxide are added in the mixing solutions of ethanol and deionized water, adding after dissolving after gelatine, ammonium polyacrylate and modified high-strength carbon fiber stir is added in ball mill, ball milling 20-40 minute;
(2) slurry that ball milling obtains is vacuumized, take out and within 2-5 minute, add 3-aminopropyl trimethoxysilane in backward slurry and continue to stir, then slurry to be injected into after in laminated glass mould in vacuum drying oven dry 1-2 hour under 60-80 ° of C;
(3) by the wet base demoulding at room temperature seasoning 1-2 days in step (2), then at 95-100 ° of C temperature, humidity is dry 1-2 days under the condition of 60-70%, remaining one-tenth is distributed into plasma spraying powder conveyer in billet surface spraying evenly;
(4) by the base substrate of step (3) at room temperature with the ramp to 200 of 3-5 ° of C/min ° C, again with the ramp to 600 of 1-2 ° of C/min ° C, constant temperature keeps being positioned in vacuum sintering furnace after 1-2 hour, sinters 3-4 hour, can obtain at the temperature of 1400-1600 ° of C.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105174969A (en) * | 2015-09-23 | 2015-12-23 | 杨洋 | High-hardness silicon nitride ceramic and preparing method thereof |
| CN106747546A (en) * | 2016-12-04 | 2017-05-31 | 淄博精诚专利信息咨询有限公司 | A kind of high-strength and high ductility ceramic composite and its application |
| CN110395989A (en) * | 2019-07-25 | 2019-11-01 | 国网河南省电力公司方城县供电公司 | A kind of silicon nitride circuit baseplate material and preparation method thereof |
-
2015
- 2015-04-13 CN CN201510169814.2A patent/CN104803696A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 王晓艳等: "Csf/Si3N4复合材料的力学性能和微波介电性能研究", 《稀有金属材料与工程》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105174969A (en) * | 2015-09-23 | 2015-12-23 | 杨洋 | High-hardness silicon nitride ceramic and preparing method thereof |
| CN106747546A (en) * | 2016-12-04 | 2017-05-31 | 淄博精诚专利信息咨询有限公司 | A kind of high-strength and high ductility ceramic composite and its application |
| CN110395989A (en) * | 2019-07-25 | 2019-11-01 | 国网河南省电力公司方城县供电公司 | A kind of silicon nitride circuit baseplate material and preparation method thereof |
| CN110395989B (en) * | 2019-07-25 | 2022-04-05 | 国网河南省电力公司方城县供电公司 | Silicon nitride circuit substrate material and preparation method thereof |
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Application publication date: 20150729 |