CN105198472A - Method for preparing silicon nitride layered ceramics reinforced by silicon nitride whiskers - Google Patents
Method for preparing silicon nitride layered ceramics reinforced by silicon nitride whiskers Download PDFInfo
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- CN105198472A CN105198472A CN201510621539.3A CN201510621539A CN105198472A CN 105198472 A CN105198472 A CN 105198472A CN 201510621539 A CN201510621539 A CN 201510621539A CN 105198472 A CN105198472 A CN 105198472A
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Abstract
The invention relates to a method for preparing silicon nitride layered ceramics reinforced by silicon nitride whiskers. The method includes preparing prefabricated parts of thin layers of the silicon nitride whiskers by the aid of tape casting processes, and preparing silicon nitride matrixes in the prefabricated parts by the aid of chemical vapor infiltration technologies to obtain silicon nitride composite materials reinforced by the silicon nitride whiskers; repeatedly carrying out repeated tape casting and chemical vapor infiltration technologies on two sides of each composite material which is used as a substrate until requirements on the thicknesses of the materials are met. The method has the advantages that whiskers of the whisker prefabricated parts prepared by the aid of the tape casting processes are uniformly dispersed, and accordingly reinforcement is high in volume fraction; the preparation temperatures can be lowered by the aid of the chemical vapor infiltration technologies as compared with sintering, accordingly, damage to the reinforcement can be reduced, sintering additives can be omitted, and influence of impurity phase can be reduced; the toughness of the silicon nitride layered ceramics can be improved owing to whisker toughening and layered compound toughening; the silicon nitride layered ceramics reinforced by the silicon nitride whiskers can be prepared by the aid of the method and are excellent in dielectric properties and mechanical properties.
Description
Technical field
The present invention relates to a kind of a kind of ceramic layered and preparation method thereof, particularly to strengthen silicon nitride ceramic layered and preparation method thereof for a kind of silicon nitride crystal whisker.
Background technology
High temperature wave-transparent material ensures that aerospace flight vehicle realizes the Multifunctional nursing material of the links such as communication, remote measurement, guidance, ignition under Working environment.Along with aeronautical and space technology and military scientific and technological development, the flight velocity of modern aerospace aircraft improves constantly, and Working environment more sophisticated, has higher requirement to high temperature wave-transparent material.High temperature wave-transparent material need have excellent dielectric properties, good thermotolerance, the row of resistance to environment and higher mechanical property.Silicon nitride (Si
3n
4) the ceramic first-selection being considered to high-performance high temperature wave-transparent material of future generation with its outstanding over-all properties, receive a large amount of concern and study with extensive.
Be disclose a kind of hot Wavetransparent Porous And Ceramic And Its Preparation Method in the Chinese patent of CN103274696A at application publication number, the method is by Homogeneous phase mixing such as silicon nitride, boron nitride, sintering aids, cold isostatic compaction after granulation, obtains porous ceramic film material after pressureless sintering.Be in the Chinese patent of CN102731098A, disclose a kind of silicon boron oxynitride fiber/silicon Nitride Ceramic Matrix Composites and preparation method thereof in application publication number, the method is by the silicon nitride of 80 ~ 90wt.%, the silicon boron oxynitride fiber of 3 ~ 10wt.% and the sintering aid of 3 ~ 10wt.%, through mixing, shaping, sintering, obtain the nitride silicon based composite material that silicon boron oxynitride fiber strengthens.
Above-mentioned research adopts traditional sintering process to prepare silicon nitride ceramics or nitride silicon based composite material, needs to add sintering aid, is unfavorable for the wave penetrate capability improving material; Preparation temperature is high; Reinforcement volume fraction is lower, and is easily damaged in moulding process, is unfavorable for the mechanical property improving material.
Summary of the invention
The technical problem solved
In order to avoid the deficiencies in the prior art part, the present invention proposes a kind of silicon nitride crystal whisker and strengthens the ceramic layered preparation method of silicon nitride, combines crystal whisker toughened and lamellar composite toughening mechanisms, the intensity of material and fracture toughness property are improved.Have employed the ceramic layered preparation technology of a kind of casting method in conjunction with CVI method, the designability of material is strong.
Technical scheme
Silicon nitride crystal whisker strengthens the ceramic layered preparation method of silicon nitride, it is characterized in that step is as follows:
Step 1, prepare silicon nitride crystal whisker thin layer precast body:
Step a1: be the silicon nitride crystal whisker of 30 ~ 50% by massfraction, the solvent of 40 ~ 60%, the dispersion agent triethyl phosphate of 2 ~ 4% carry out ball milling 12 ~ 24h, then binding agent polyvinyl butyral acetal, the softening agent of 2 ~ 4%, the defoamer of 2 ~ 4% that massfraction is 3 ~ 5% is added, continue ball milling 12 ~ 24h, froth in vacuum 10min, obtains whisker slurry; Described solvent is dehydrated alcohol and 2-butanone 1:1 mixed preparing by volume; Described softening agent is glycerol and dioctyl phthalate (DOP) 1:1 mixed preparing by volume; Described defoamer is propyl carbinol and ethylene glycol 1:1 mixed preparing by volume;
Step a2: whisker slurry is carried out curtain coating, after dry under room temperature, the demoulding obtains silicon nitride crystal whisker precast body thin layer;
Step 2, employing CVI method prepare silicon nitride matrix in silicon nitride crystal whisker film precast body, complete the preparation of single-layer silicon nitride silicon whisker reinforcement silicon nitride ceramics: depositing operation is: take silicon tetrachloride as silicon source, ammonia is nitrogenous source, hydrogen is carrier gas, argon gas is diluent gas, depositing temperature is 800 ~ 1000 DEG C, and depositing time is 20 ~ 40h.The flow of described silicon tetrachloride is 0.8 ~ 1.2L/min, and the flow of ammonia is 0.5 ~ 0.7L/min, and the flow of hydrogen is 0.8 ~ 1.2L/min, and the flow of argon gas is 0.8 ~ 1.2L/min.
It is substrate that the silicon nitride crystal whisker obtained with step 2 strengthens silicon nitride ceramics sheet, and repeating step a2, prepares whisker preform thin layer at substrate front and back; Repeating step 2 again, cvd nitride silicon substrate in the whisker preform thin layer that step 3 obtains; Repeatedly repeat this process, repeatedly carry out curtain coating and depositing operation, until ceramic layered thickness satisfies the demands.
Described ball milling carries out in ball grinder.
Curtain coating in described step a2 adopts casting machine, and the front scraper height of adjustment casting machine is 0.2 ~ 0.8mm, and rear scraper height is 0.4 ~ 1.2mm, and passing speed belt speed is 0.2 ~ 1m/min.
Described repeatedly multiplicity is 3 ~ 10 times.
Silicon nitride crystal whisker diameter in described step 1 is 0.1 ~ 5 μm, and length is 3 ~ 20 μm.
The gauge control of the silicon nitride crystal whisker precast body thin layer of the curtain coating in described step a2 is between 200 μm ~ 500 μm.
Beneficial effect
A kind of silicon nitride crystal whisker that the present invention proposes strengthens silicon nitride stratiform ceramic preparation.Use casting method to prepare silicon nitride crystal whisker thin layer precast body, then use chemical vapor infiltration technique to prepare silicon nitride matrix in precast body, obtain silicon nitride crystal whisker and strengthen silicon nitride composite material.Take matrix material as substrate, repeat curtain coating and chemical vapor deposition method in its both sides, until material thickness reaches requirement.The whisker preform whisker using casting method to prepare is uniformly dispersed, and reinforcement volume fraction is high.Chemical vapor deposition method can reduce preparation temperature compared to sintering, reduces the injury to reinforcement, and does not need to use sintering aid, decreases the impact of impurity phase.Meanwhile, the crystal whisker toughened and toughness reinforcing toughness improving silicon nitride ceramics of lamellar composite.The silicon nitride crystal whisker enhancing silicon nitride that the present invention can prepare dielectric properties and excellent in mechanical performance is ceramic layered.
The invention has the beneficial effects as follows: material consists of silicon nitride crystal whisker and the standby silicon nitride matrix of CVI legal system, do not need in preparation process to introduce sintering aid, the impact of impurity can be reduced.Adopt casting method to prepare whisker preform, whisker is evenly distributed, and whisker is higher.Adopt CVI legal system for silicon nitride matrix, compared with sintering, preparation temperature is low, and whisker is combined with basal body interface well, and the damage suffered by whisker is less.Crystal whisker toughened and stratiform are met toughness reinforcing combining, is conducive to the intensity and the fracture toughness property that improve material.Can find out more than comprehensive, the silicon nitride crystal whisker flexible silicon nitride that the present invention can prepare mechanical property and dielectric properties excellence is ceramic layered.
Accompanying drawing explanation
Fig. 1 is that silicon nitride crystal whisker strengthens the ceramic layered preparation method's schema of silicon nitride
Fig. 2 is the scanning electron microscopic picture that in embodiment 1, silicon nitride crystal whisker strengthens the ceramic polished fracture of silicon nitride stratiform
Fig. 3 is that in embodiment 1, silicon nitride crystal whisker strengthens the ceramic layered X-ray diffraction interpretation of result curve of silicon nitride
Embodiment
Now in conjunction with the embodiments, the invention will be further described for accompanying drawing:
Embodiment 1:
(1) by the silicon nitride crystal whisker of length-to-diameter ratio 5 ~ 10, solvent (dehydrated alcohol and 2-butanone, volume ratio is 1:1), dispersion agent (triethyl phosphate) adds in ball grinder, wherein silicon nitride crystal whisker, solvent, the massfraction of dispersion agent is respectively 35%, 55%, 2%, after low speed ball milling 12h, the binding agent (polyvinyl butyral acetal) that massfraction is 3% is added in ball grinder, massfraction is softening agent (glycerol and the dioctyl phthalate (DOP) of 3%, volume ratio is 1:1), massfraction is defoamer (propyl carbinol and the ethylene glycol of 2%, volume ratio is 1:1), ball milling 12h, obtain uniform and stable silicon nitride crystal whisker slurry, seal up for safekeeping stand-by.
(2) casting method prepares whisker preform thin layer: the front scraper height of the two scraper casting machine of adjustment is 0.6mm, and rear scraper height is 0.8mm, is poured into by silicon nitride crystal whisker slurry in casting machine slurry tank, and biography speed belt speed is set to 0.8m/min and carries out curtain coating.After dry under curtain coating thin layer room temperature, the demoulding is for subsequent use.Gained thickness of thin layer is 300 μm, and whisker is 30%
(3) CVI method is adopted to prepare silicon nitride matrix in silicon nitride crystal whisker film precast body.Depositing operation is: take silicon tetrachloride as silicon source, and ammonia is nitrogenous source, and hydrogen is carrier gas, and argon gas is diluent gas, and depositing temperature is 800 ~ 1000 DEG C, and depositing time is 20 ~ 40h.The flow of described silicon tetrachloride is 0.8 ~ 1.2L/min, and the flow of ammonia is 0.5 ~ 0.7L/min, and the flow of hydrogen is 0.8 ~ 1.2L/min, and the flow of argon gas is 0.8 ~ 1.2L/min.
(4) after CVI, obtain the bilateral curtain coating that silicon nitride crystal whisker strengthens silicon nitride ceramics, prepare silicon nitride crystal whisker thin layer precast body, gained precast body thickness is 300 μm, and whisker is 30%
(5) repeat (3) and (4), until material thickness reaches 3mm, obtain silicon nitride crystal whisker enhancing silicon nitride ceramic layered.
Embodiment 2:
(1) by the silicon nitride crystal whisker of length-to-diameter ratio 5 ~ 10, solvent (dehydrated alcohol and 2-butanone, volume ratio is 1:1), dispersion agent (triethyl phosphate) adds in ball grinder, wherein silicon nitride crystal whisker, solvent, the massfraction of dispersion agent is respectively 50%, 40%, 2%, after low speed ball milling 12h, the binding agent (polyvinyl butyral acetal) that massfraction is 3% is added in ball grinder, massfraction is softening agent (glycerol and the dioctyl phthalate (DOP) of 3%, volume ratio is 1:1), massfraction is defoamer (propyl carbinol and the ethylene glycol of 2%, volume ratio is 1:1), ball milling 12h, obtain uniform and stable silicon nitride crystal whisker slurry, seal up for safekeeping stand-by.
(2) casting method prepares whisker preform thin layer: the front scraper height of the two scraper casting machine of adjustment is 0.6mm, and rear scraper height is 0.8mm, is poured into by silicon nitride crystal whisker slurry in casting machine slurry tank, and biography speed belt speed is set to 0.8m/min and carries out curtain coating.After dry under curtain coating thin layer room temperature, the demoulding is for subsequent use.Gained thickness of thin layer is 350 μm, and whisker is 40%
(3) CVI method is adopted to prepare silicon nitride matrix in silicon nitride crystal whisker film precast body.Depositing operation is: take silicon tetrachloride as silicon source, and ammonia is nitrogenous source, and hydrogen is carrier gas, and argon gas is diluent gas, and depositing temperature is 800 ~ 1000 DEG C, and depositing time is 20 ~ 40h.The flow of described silicon tetrachloride is 0.8 ~ 1.2L/min, and the flow of ammonia is 0.5 ~ 0.7L/min, and the flow of hydrogen is 0.8 ~ 1.2L/min, and the flow of argon gas is 0.8 ~ 1.2L/min.
(4) after CVI, obtain the bilateral curtain coating that silicon nitride crystal whisker strengthens silicon nitride ceramics, prepare silicon nitride crystal whisker thin layer precast body, gained precast body thickness is 350 μm, and whisker is 40%
(5) repeat (3) and (4), until material thickness reaches 3mm, obtain silicon nitride crystal whisker enhancing silicon nitride ceramic layered.
Claims (7)
1. silicon nitride crystal whisker strengthens the ceramic layered preparation method of silicon nitride, it is characterized in that step is as follows:
Step 1, prepare silicon nitride crystal whisker thin layer precast body:
Step a1: be the silicon nitride crystal whisker of 30 ~ 50% by massfraction, the solvent of 40 ~ 60%, the dispersion agent triethyl phosphate of 2 ~ 4% carry out ball milling 12 ~ 24h, then binding agent polyvinyl butyral acetal, the softening agent of 2 ~ 4%, the defoamer of 2 ~ 4% that massfraction is 3 ~ 5% is added, continue ball milling 12 ~ 24h, froth in vacuum 10min, obtains whisker slurry; Described solvent is dehydrated alcohol and 2-butanone 1:1 mixed preparing by volume; Described softening agent is glycerol and dioctyl phthalate (DOP) 1:1 mixed preparing by volume; Described defoamer is propyl carbinol and ethylene glycol 1:1 mixed preparing by volume;
Step a2: whisker slurry is carried out curtain coating, after dry under room temperature, the demoulding obtains silicon nitride crystal whisker precast body thin layer;
Step 2, employing CVI method prepare silicon nitride matrix in silicon nitride crystal whisker film precast body, complete the preparation of single-layer silicon nitride silicon whisker reinforcement silicon nitride ceramics: depositing operation is: take silicon tetrachloride as silicon source, ammonia is nitrogenous source, hydrogen is carrier gas, argon gas is diluent gas, depositing temperature is 800 ~ 1000 DEG C, and depositing time is 20 ~ 40h.The flow of described silicon tetrachloride is 0.8 ~ 1.2L/min, and the flow of ammonia is 0.5 ~ 0.7L/min, and the flow of hydrogen is 0.8 ~ 1.2L/min, and the flow of argon gas is 0.8 ~ 1.2L/min.
2. silicon nitride crystal whisker strengthens the ceramic layered preparation method of silicon nitride according to claim 1, it is characterized in that: it is substrate that the silicon nitride crystal whisker obtained with step 2 strengthens silicon nitride ceramics sheet, repeating step a2, prepares whisker preform thin layer at substrate front and back; Repeating step 2 again, cvd nitride silicon substrate in the whisker preform thin layer that step 3 obtains; Repeatedly repeat this process, repeatedly carry out curtain coating and depositing operation, until ceramic layered thickness satisfies the demands.
3. silicon nitride crystal whisker strengthens the ceramic layered preparation method of silicon nitride according to claim 1, it is characterized in that: described ball milling carries out in ball grinder.
4. according to claim 1 or 2, silicon nitride crystal whisker strengthens the ceramic layered preparation method of silicon nitride, it is characterized in that: the curtain coating in described step a2 adopts casting machine, the front scraper height of adjustment casting machine is 0.2 ~ 0.8mm, rear scraper height is 0.4 ~ 1.2mm, and passing speed belt speed is 0.2 ~ 1m/min.
5. silicon nitride crystal whisker strengthens the ceramic layered preparation method of silicon nitride according to claim 2, it is characterized in that: described repeatedly multiplicity is 3 ~ 10 times.
6. silicon nitride crystal whisker strengthens the ceramic layered preparation method of silicon nitride according to claim 1, and it is characterized in that: the silicon nitride crystal whisker diameter in described step 1 is 0.1 ~ 5 μm, length is 3 ~ 20 μm.
7. silicon nitride crystal whisker strengthens the ceramic layered preparation method of silicon nitride according to claim 1, it is characterized in that: the gauge control of the silicon nitride crystal whisker precast body thin layer of the curtain coating in described step a2 is between 200 μm ~ 500 μm.
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Cited By (7)
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| CN106431421A (en) * | 2016-09-27 | 2017-02-22 | 广东工业大学 | Axial laminated ceramic and diamond composite spray nozzle and preparation method thereof |
| CN106588124A (en) * | 2016-11-10 | 2017-04-26 | 西北工业大学 | Low-temperature preparation method of ceramic coating absorbing waves in frequency band of 8-18 GHz |
| CN107698271A (en) * | 2017-09-11 | 2018-02-16 | 西北工业大学 | High-temperature-resistant high toughness nitrogenizes silicon substrate wave-penetrating composite material and preparation method |
| CN111620711A (en) * | 2020-05-21 | 2020-09-04 | 贵研铂业股份有限公司 | Bionic silicon nitride ceramic material and preparation method thereof |
| CN111925215A (en) * | 2020-07-20 | 2020-11-13 | 宁波伏尔肯科技股份有限公司 | Preparation method of enhanced layered ceramic bulletproof piece |
| CN114853482A (en) * | 2022-05-11 | 2022-08-05 | 西安交通大学 | High-toughness silicon nitride nanowire/silicon nitride layered ceramic and preparation method thereof |
| CN114956858A (en) * | 2022-05-11 | 2022-08-30 | 西安交通大学 | Layered elastic-plastic silicon nitride ceramic and preparation method thereof |
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Cited By (10)
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| CN106431421A (en) * | 2016-09-27 | 2017-02-22 | 广东工业大学 | Axial laminated ceramic and diamond composite spray nozzle and preparation method thereof |
| CN106431421B (en) * | 2016-09-27 | 2019-09-10 | 广东工业大学 | Axial ceramic layered diamond composite nozzle and preparation method thereof |
| CN106588124A (en) * | 2016-11-10 | 2017-04-26 | 西北工业大学 | Low-temperature preparation method of ceramic coating absorbing waves in frequency band of 8-18 GHz |
| CN107698271A (en) * | 2017-09-11 | 2018-02-16 | 西北工业大学 | High-temperature-resistant high toughness nitrogenizes silicon substrate wave-penetrating composite material and preparation method |
| CN107698271B (en) * | 2017-09-11 | 2020-11-06 | 西北工业大学 | High-temperature-resistant high-strength and high-toughness silicon nitride-based wave-transparent composite material and preparation method thereof |
| CN111620711A (en) * | 2020-05-21 | 2020-09-04 | 贵研铂业股份有限公司 | Bionic silicon nitride ceramic material and preparation method thereof |
| CN111620711B (en) * | 2020-05-21 | 2021-08-24 | 贵研铂业股份有限公司 | Bionic silicon nitride ceramic material and preparation method thereof |
| CN111925215A (en) * | 2020-07-20 | 2020-11-13 | 宁波伏尔肯科技股份有限公司 | Preparation method of enhanced layered ceramic bulletproof piece |
| CN114853482A (en) * | 2022-05-11 | 2022-08-05 | 西安交通大学 | High-toughness silicon nitride nanowire/silicon nitride layered ceramic and preparation method thereof |
| CN114956858A (en) * | 2022-05-11 | 2022-08-30 | 西安交通大学 | Layered elastic-plastic silicon nitride ceramic and preparation method thereof |
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