CN1597619A - Preparation method of whisker and pacticle toughening ceramic base composite - Google Patents
Preparation method of whisker and pacticle toughening ceramic base composite Download PDFInfo
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- CN1597619A CN1597619A CN 200410026337 CN200410026337A CN1597619A CN 1597619 A CN1597619 A CN 1597619A CN 200410026337 CN200410026337 CN 200410026337 CN 200410026337 A CN200410026337 A CN 200410026337A CN 1597619 A CN1597619 A CN 1597619A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 10
- 239000002131 composite material Substances 0.000 title claims description 29
- 238000002360 preparation method Methods 0.000 title claims description 12
- 239000002245 particle Substances 0.000 claims abstract description 46
- 238000000034 method Methods 0.000 claims abstract description 22
- 238000000151 deposition Methods 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 6
- 239000013078 crystal Substances 0.000 claims abstract 4
- 239000011153 ceramic matrix composite Substances 0.000 claims description 31
- 239000000463 material Substances 0.000 claims description 19
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 13
- 239000011230 binding agent Substances 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 11
- 239000011159 matrix material Substances 0.000 claims description 11
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 11
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 9
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 230000008021 deposition Effects 0.000 claims description 7
- 238000005469 granulation Methods 0.000 claims description 6
- 230000003179 granulation Effects 0.000 claims description 6
- 230000002787 reinforcement Effects 0.000 claims description 6
- 229920005989 resin Polymers 0.000 claims description 6
- 239000011347 resin Substances 0.000 claims description 6
- 230000008595 infiltration Effects 0.000 claims description 5
- 238000001764 infiltration Methods 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 238000007873 sieving Methods 0.000 claims description 4
- 239000000758 substrate Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 239000002243 precursor Substances 0.000 claims description 3
- 238000007723 die pressing method Methods 0.000 claims description 2
- 238000000462 isostatic pressing Methods 0.000 claims description 2
- 238000012216 screening Methods 0.000 claims description 2
- 230000003014 reinforcing effect Effects 0.000 abstract 1
- 239000000835 fiber Substances 0.000 description 18
- 229910052581 Si3N4 Inorganic materials 0.000 description 9
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 9
- 230000000694 effects Effects 0.000 description 5
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 4
- 239000005011 phenolic resin Substances 0.000 description 4
- 229920001568 phenolic resin Polymers 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000007731 hot pressing Methods 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 238000009417 prefabrication Methods 0.000 description 3
- 239000002296 pyrolytic carbon Substances 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 238000001272 pressureless sintering Methods 0.000 description 2
- 229920001187 thermosetting polymer Polymers 0.000 description 2
- 238000013459 approach Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 229910052575 non-oxide ceramic Inorganic materials 0.000 description 1
- 239000011225 non-oxide ceramic Substances 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
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Abstract
A crystal whisker and particle toughened ceramic-based composition used to make large thin-wall member is prepared through granulating to prepare the coagulated substance of crystal whiskers and particles, preparing the prefabricated body of crystal whisker-particle reinforcing body, and depositing the ceramic base in said prefabricated body by chemical vapour osmosis process.
Description
The technical field is as follows:
the invention relates to a preparation method of a whisker and particle ceramic matrix composite material.
(II) background technology:
the ceramic matrix composite material is a new generation strategic thermal structure material replacing metal, has the outstanding advantages of high temperature resistance and low density, and has wide application prospect in the fields of aviation, aerospace and the like. The ceramic matrix composite mainly has three toughening modes of continuous fiber, whisker and particle, wherein the fiber toughened composite has the fracture behavior similar to that of the prior art, is insensitive to cracks and has the high-reliability characteristic of no catastrophic damage, and the whisker and particle composite has the characteristic of low cost. Therefore, the fiber, whisker and particle composite material form a complete ceramic matrix composite material system and all play an important role in the application process of the ceramic matrix composite material.
The whisker and particle ceramic matrix composite material is prepared through mixing whisker and particle reinforcement with ceramic matrix powder, molding or hot pressing and sintering. Because the reinforcement and the matrix are difficult to be uniformly mixed, the toughening effect is not ideal, and the application of the particle ceramic matrix composite material is severely limited. In order to further improve the toughening effect, the whisker and particle composite materials are increasingly adopting ultrafine powder or nano powder matrix. However, the finer the matrix, the more difficult it is to uniformly disperse the composite, and the lower the performance of the composite. No matter the mould pressing or the injection molding, the large complex thin-wall whisker and particle composite material green body is difficult to obtain, and the pressureless sintering whisker and particle ceramic matrix composite material has low performance, and the application range of the hot-pressing sintering is more limited. In summary, the existing preparation method of whisker and particle toughened ceramic matrix composite material has the following problems which are difficult to solve:
(1) the composite material is difficult to disperse uniformly, so that the performance is low;
(2) it is difficult to obtain large complex thin-walled composite components.
Chemical Vapor Infiltration (CVI) is the most advanced and commercially available method of manufacturing continuous fiber ceramic matrix composites today, comprising the following core elements:
(1) using a fiber preform which is not limited by shape and can be shaped;
(2) using an organic precursor capable of pyrolysis into a ceramic matrix;
(3) the precursor is pyrolytically deposited in the preform under suitable conditions.
Because the preform is woven in the form of fiber bundles, the fiber toughened ceramic matrix composite material prepared by CVI has a remarkable bundle structure microscopic characteristic (figure 1). Researches show that the bundle structure characteristic enables the fiber toughened ceramic matrix composite material to show a remarkable non-uniform composite material effect, and is an important reason that the fiber composite material has high performance. The basic starting point of the invention is that according to the enlightenment of the fiber composite material, the idea of the preparation method of the whisker and particle composite material is changed from the pursuit of dispersion uniformity to the pursuit of non-uniform composite effect.
(III) the invention content:
in order to overcome the defects that the composite material is difficult to disperse uniformly in the prior art, so that the composite material is low in performance, a large complex thin-walled whisker and particle composite material blank is difficult to obtain, the performance of the whisker and particle ceramic matrix composite material is low by pressureless sintering, and the application range of hot-pressing sintering is more limited, the invention provides a method for preparing a particle and whisker toughened ceramic matrix composite material by chemical vapor infiltration.
The technical scheme of the invention comprises the following three core links:
(1) and (4) granulating to enable the whiskers and the particles to be uniform aggregates similar to fiber bundles. Thermosetting resin is used as a granulation binder, ethanol or acetone is used as a diluent of the resin, the thermosetting resin and particles or whiskers are uniformly mixed, and screening is carried out after multiple die pressing crushing processes to obtain uniform aggregates with a certain diameter. After drying, the agglomerates have the compressive strength required for preforming. In order to make full use of the raw materials, the sieved pellets may be subjected to a further process of die crushing and sieving to obtain the desired agglomerates.
(2) And performing prefabrication and forming to enable the whiskers and the particles to be similar to a blank of a fiber preform. After granulation, whisker and particle preforms can be prepared by two preform forming modes of mould pressing and isostatic pressing, the uniformity of the preforms is improved by adopting a vibration charging method, and the forming strength of the preforms is improved by adding a polyvinyl alcohol aqueous solution binder.
(3) Vapor infiltration produces a particle-diameter composite material similar to a fibrous composite material. Proper weak interface bonding strength is the key for toughening the ceramic matrix composite, and the pyrolytic carbon is an important interface layer material for realizing weak interface bonding. The binder pyrolytically decomposes during deposition to form a pyrolytic carbon interface layer, so whisker and particle composites generally do not require a separate interface layer preparation process, whereas fibrous composites require the preparation of pyrolytic carbon or other interface layers. The CVI process for whisker and particle composites is essentially the same as for fiber composites, and commonly used ceramic substrates are silicon carbide and silicon nitride, and the deposition process for these two substrates can be represented by the following chemical reaction equation:
the whisker and particle ceramic matrix composite prepared by the method of combining CVI and the preform has a similar microstructure to the fiber woven ceramic matrix composite (figure 3), and thus has three important toughening approaches:
(1) toughening the weak interface layer properly;
(2) toughening the porous nano matrix;
(3) toughening by non-uniform composite effect
Because the technical scheme that the CVI is combined with the preform to prepare the whisker and particle ceramic matrix composite is adopted, the toughness of the material is increased, so that the ceramic matrix composite prepared by the invention has the characteristics of good performance and strong designability, and a large thin-wall complex component and a whisker and particle toughened ceramic matrix composite component with high requirement on dimensional accuracy can be obtained. The method is particularly suitable for manufacturing non-oxide ceramic matrix composite materials such as silicon nitride, silicon carbide and the like, and can also be used for manufacturing other composite materials. .
(IV) description of the drawings:
FIG. 1 shows the microstructure characteristics of CVI produced fiber woven ceramic matrix composites.
FIG. 2 is a block diagram of a process flow for preparing whisker and particulate ceramic matrix composites by a CVI bonded preform method.
FIG. 3 is a microstructure characterization of whisker and particulate ceramic matrix composites prepared by the CVI bond preform method.
In the figure:
1-surface coating 2-fiber bundle 3-fiber filament 4-fiber bundle gap 5-whisker group
6-whiskers 7-whisker interstitial gaps 8-particle clusters 9-particles 10-inter-particle cluster gaps.
(V) specific embodiment:
the first embodiment is asfollows:
this example is the preparation of a silicon carbide whisker toughened silicon carbide ceramic matrix composite.
Silicon carbide whiskers with the diameter of 1.5 microns and the length-diameter ratio of 8-10 are selected as reinforcements, 5% PVA (polyvinyl alcohol) aqueous solution is used as a preformed binder, phenolic resin ethanol solution is used as a granulation binder, and the concentration of the solution is 0.5 g/ml.
During preparation, 150g of silicon carbide whiskers are mixed with 100ml of phenolic resin solution, mould pressing and crushing are carried out for four times under the pressure of 10-20 MPa, drying is carried out for 24 hours in the shade at room temperature, and drying is carried out for 2 hours at 120 ℃. After crushing, sieving and granulating, selecting a particle group with the diameter of 0.6-1.0 mm to be mixed with 15-30 wt% of PVA aqueous solution, and performing prefabrication molding under the pressure of 3-8 MPa. And drying the formed prefabricated body in the shade at room temperature for 24 hours, drying the prefabricated body at 120 ℃ for 2 hours, and then putting the prefabricated body into a deposition furnace to deposit a silicon carbide substrate to prepare the silicon carbide toughened silicon carbide ceramic-based composite material.
The process conditions of this example are: the deposition temperature is 900-1100 ℃, the atmosphere pressure is 2-5 kPa, the flow rate of H2 gas is 200-350 ml/min, the flow rate of Ar is 300-400 ml/min, the temperature of MTS is 30-40 ℃, the molar mass ratio of H2 to MTS is 10, and the deposition time is 100-200H.
Example two:
this example is the preparation of silicon nitride particle-toughened silicon nitride ceramic matrix composites
Silicon nitride powder withthe diameter of 6 mu m is selected as a particle reinforcement, 5 percent PVA aqueous solution is selected as a preformed binder, phenolic resin ethanol solution is selected as a granulation binder, and the concentration of the solution is 0.5 g/ml.
During preparation, 150g of silicon nitride powder is mixed with 50ml of phenolic resin solution, mould pressing and crushing are carried out for four times under the pressure of 10-20 MPa, drying is carried out for 24 hours in the shade at room temperature, and drying is carried out for 2 hours at 120 ℃. After crushing, sieving and granulating, selecting a particle group with the diameter of 0.6-1.0 mm to be mixed with 10-25 wt% of PVA aqueous solution, and performing prefabrication molding under the pressure of 3-8 MPa. And drying the formed prefabricated body in the shade at room temperature for 24 hours, drying the prefabricated body at 120 ℃ for 2 hours, and then putting the prefabricated body into a deposition furnace to deposit a silicon nitride matrix to prepare the silicon nitride particle toughened silicon nitride ceramic matrix composite.
The process conditions of this example are: SiCl at 800-1100 deg.C and 500-1500 Pa4The flow rate is 40-200 ml/min, the NH3 flow rate is 120-300 ml/min, and the deposition time is 100-200 h.
Claims (5)
1. A preparation method of whisker and particle toughened ceramic matrix composite material is characterized in that:
a. preparing whiskers and particle aggregates by adopting a granulation method, and preparing a preform of the whiskers and the particle reinforcement by utilizing the aggregates;
b. depositing a ceramic matrix in the prefabricated part by adopting a chemical vapor infiltration method, and converting the ceramic matrix into aninterface layer by using a binder;
c. by sieving, the size of the crystal whisker and the particle reinforcement and the diameter and uniformity of the aggregate are controlled.
2. The method of claim 1, wherein the ceramic matrix is deposited by chemical vapor infiltration and converted to an interfacial layer by a binder to ensure weak bonding at the interface.
3. The method for preparing whisker and particle toughened ceramic matrix composite material according to claim 1, wherein the process for realizing the method comprises the following steps:
a. mixing the particles or the whiskers with the resin solution, carrying out mould pressing and crushing for multiple times, and drying;
b. screening, selecting particle groups with the diameter of 0.6-1.0 mm, mixing the particle groups with a PVA (polyvinyl alcohol) aqueous solution, performing pressure forming, and drying;
c. and putting the formed prefabricated body into a deposition furnace to deposit a silicon carbide substrate to prepare the silicon carbide whisker or silicon carbide particle toughened silicon carbide composite material.
4. The process for preparing whisker and particle toughened ceramic matrix composites as claimed in claims 1 and 2, wherein a resin ethanol solution or a resin acetone solution is used as a granulation binder.
5. The method of preparing a whisker and particle toughened ceramic matrix composite material according to claim 1, wherein the precursor is formed by using an aqueous solution of PVA as a preform forming binder and by using a vibration die pressing or isostatic pressing method.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410026337 CN1271008C (en) | 2004-07-19 | 2004-07-19 | Preparation method of whisker and pacticle toughening ceramic base composite |
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|---|---|---|---|
| CN 200410026337 CN1271008C (en) | 2004-07-19 | 2004-07-19 | Preparation method of whisker and pacticle toughening ceramic base composite |
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| Publication Number | Publication Date |
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| CN1597619A true CN1597619A (en) | 2005-03-23 |
| CN1271008C CN1271008C (en) | 2006-08-23 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101172877B (en) * | 2006-10-16 | 2010-06-16 | 宁波大学 | Process for manufacturing multicomponent combination toughness reinforcing silicon carbide ceramic including crystal whisker and fibre |
| WO2013020317A1 (en) * | 2011-08-05 | 2013-02-14 | 华南理工大学 | Tungsten carbide composite material comprising aluminium oxide particles and silicon nitride whiskers and preparation process thereof |
| CN102964139A (en) * | 2012-12-04 | 2013-03-13 | 西北工业大学 | Preparation method of whisker and particle synergistically toughened laminar ceramic matrix composite |
| CN103086732A (en) * | 2013-01-21 | 2013-05-08 | 天津师范大学 | Fiber enhanced silicon carbide porous ceramic and preparation method and application thereof |
| CN104803685A (en) * | 2015-04-08 | 2015-07-29 | 西北工业大学 | Preparation method of micro-nanofiber/ceramic matrix composite |
| CN106542829A (en) * | 2016-11-08 | 2017-03-29 | 西安建筑科技大学 | A kind of preparation and application of silicon carbide whisker/silicon-carbide particle composite granule |
| CN108706978A (en) * | 2018-06-08 | 2018-10-26 | 西北工业大学 | The method that mist projection granulating combination 3DP and CVI prepare carbon/silicon carbide ceramic matrix composite |
-
2004
- 2004-07-19 CN CN 200410026337 patent/CN1271008C/en active Active
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101172877B (en) * | 2006-10-16 | 2010-06-16 | 宁波大学 | Process for manufacturing multicomponent combination toughness reinforcing silicon carbide ceramic including crystal whisker and fibre |
| WO2013020317A1 (en) * | 2011-08-05 | 2013-02-14 | 华南理工大学 | Tungsten carbide composite material comprising aluminium oxide particles and silicon nitride whiskers and preparation process thereof |
| GB2506287A (en) * | 2011-08-05 | 2014-03-26 | Univ South China Tech | Tungsten carbide composite material comprising aluminium oxide particles and silicon nitride whiskers and preparation process thereof |
| GB2506287B (en) * | 2011-08-05 | 2019-07-31 | Univ South China Tech | Tungsten Carbide Composite Containing Alumina Grains and Silicon Nitride Whiskers and the Preparation Method Thereof |
| CN102964139A (en) * | 2012-12-04 | 2013-03-13 | 西北工业大学 | Preparation method of whisker and particle synergistically toughened laminar ceramic matrix composite |
| CN102964139B (en) * | 2012-12-04 | 2014-11-12 | 西北工业大学 | Preparation method of whisker and particle synergistically toughened laminar ceramic matrix composite |
| CN103086732A (en) * | 2013-01-21 | 2013-05-08 | 天津师范大学 | Fiber enhanced silicon carbide porous ceramic and preparation method and application thereof |
| CN103086732B (en) * | 2013-01-21 | 2014-12-03 | 天津师范大学 | Fiber enhanced silicon carbide porous ceramic and preparation method and application thereof |
| CN104803685A (en) * | 2015-04-08 | 2015-07-29 | 西北工业大学 | Preparation method of micro-nanofiber/ceramic matrix composite |
| CN106542829A (en) * | 2016-11-08 | 2017-03-29 | 西安建筑科技大学 | A kind of preparation and application of silicon carbide whisker/silicon-carbide particle composite granule |
| CN108706978A (en) * | 2018-06-08 | 2018-10-26 | 西北工业大学 | The method that mist projection granulating combination 3DP and CVI prepare carbon/silicon carbide ceramic matrix composite |
| CN108706978B (en) * | 2018-06-08 | 2020-11-06 | 西北工业大学 | Method for preparing silicon carbide ceramic matrix composite by combining spray granulation with 3DP and CVI |
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| CN1271008C (en) | 2006-08-23 |
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Effective date of registration: 20191008 Address after: 710117 West Section 912 of Biyuan Road, Xi'an High-tech Zone, Shaanxi Province Patentee after: XI'AN GOLDEN MOUNTAIN CERAMIC COMPOSITES CO.,LTD. Address before: 710072 Xi'an friendship West Road, Shaanxi, No. 127 Patentee before: Northwestern Polytechnical University |
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Address after: 710117 West Section 912 of Biyuan Road, Xi'an High-tech Zone, Shaanxi Province Patentee after: Xi'an Xinyao Ceramic Composite Co.,Ltd. Country or region after: China Address before: 710117 West Section 912 of Biyuan Road, Xi'an High-tech Zone, Shaanxi Province Patentee before: XI'AN GOLDEN MOUNTAIN CERAMIC COMPOSITES CO.,LTD. Country or region before: China |
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