CN1387984A - Formation techn of fiber reinforced ceramic-base composite material - Google Patents
Formation techn of fiber reinforced ceramic-base composite material Download PDFInfo
- Publication number
- CN1387984A CN1387984A CN 02137852 CN02137852A CN1387984A CN 1387984 A CN1387984 A CN 1387984A CN 02137852 CN02137852 CN 02137852 CN 02137852 A CN02137852 A CN 02137852A CN 1387984 A CN1387984 A CN 1387984A
- Authority
- CN
- China
- Prior art keywords
- ceramic
- composite material
- fiber reinforced
- base composite
- techn
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Producing Shaped Articles From Materials (AREA)
Abstract
The formation process of fiber reinforced ceramic-base composite material includes the following steps: compounding suspension with water, gel monomer, cross-linking agent monomer, organic dispersant and ceramic powder; stirring and ball milling of the suspension, adding initiator while and vacuum defoaming; filling the ceramic slurry into fiber prefabricated body inside one molding chamber under the action of pressure and supersonic vibration and curing to solidify; and demolding to obtain the fiber reinforced ceramic-base composite material. The said process can produce composite material with complicated shape, high density, high homogeneity, high strength and high toughness.
Description
Technical field
The present invention relates to a kind of formation techn of fiber reinforced ceramic-base composite material, belong to the preparation field of ceramic material and parts.
Background technology
Ceramic material makes it obtain using widely as the high performance structures material owing to have high strength, high rigidity, fabulous wear-resisting, high temperature resistant and decay resistance.Countries in the world all bar structure pottery regard that revolution has the hi tech and new material of significant role and gives primary study and development to futurity industry as.But because the intrinsic fragility of ceramic material itself is done to lack enough reliabilities when structural material uses, thereby is made its range of application be subjected to very big restriction.For many years, the ceramist utilizes different toughening mechanism, adopts different technologies of preparing, many dissimilar ceramic matric composites have been made, make the fragility of ceramic material make moderate progress, toughness is significantly improved, and is promoted the use of in some industrial circle.
In ceramic matric composite, the toughening effect of FRCMC is particularly remarkable, thereby extremely ceramic boundary pays close attention to, but because of the complexity of forming process, and the problem that exists at aspects such as reliability, costs, and limited its practical application.
The FRCMC shaping technology of preparing of current main employing is:
(1) winding shaping hot pressing sintering method, fiber is passed through ceramic mud, be wrapped on the drum of a rotation, obtain fiber-ceramic strip after the drying, strip is cut into required shape and size, they hot pressed sinterings that in layer stacks up, make one dimension or two-dimentional long fibre and strengthen ceramic matric composite again.
(2) slurry infiltration hot pressing sintering method by twining or be woven into precast body, with the ceramic size infiltration, obtains fiber three-dimensional long fibre and strengthens ceramic matric composite then.
Said method is owing to be to carry out hot pressed sintering after drying, therefore there is a product size, shape is subjected to very big restriction, or apparatus expensive, problem that cost is high, particularly infiltrate, flood and be difficult to fully, evenly, also be prone to defectives such as crackle in the dry run, cause composite quality lower thereafter.
(3) chemical vapour infiltration is promoted by chemical vapour deposition (CVD), and its shortcoming is that deposition velocity is slow, and production efficiency is lower.
(4) precursor method is infiltrate in the fibre preforms base colloidal sol, gel or liquid polymer, and heating is decomposed to form pottery and deposits on the prefabricated blank then.Its major defect is that contraction is bigger in the dry run, has high shrinkage cavity and low conversion ratio, is difficult to obtain the dense sintering body, and only limits to oxide-based pottery.
Summary of the invention
The purpose of this invention is to provide a kind of formation techn of fiber reinforced ceramic-base composite material, make ceramic concentrate suspension pressure injection, infiltration fortifying fibre precast body by press injector, in-situ solidifying is shaped then, the FRCMC of, high density complex-shaped to prepare, high uniformity, high strength, high tenacity.
The technical scheme that realizes above-mentioned purpose is: a kind of formation techn of fiber reinforced ceramic-base composite material comprises following each step:
A, batching, the gel monomer and the cross-linking monomer that add 6～35wt% in water are mixed with premixed liquid, the ratio of gel monomer and cross-linking monomer is between 5: 1～250: 1, and in premixed liquid, add the organic dispersing agent of ceramic powder quality 0.01～1wt%, add ceramic powder again in above-mentioned premixed liquid, addition is 50～60vol% volume fraction of premixed liquid and ceramic powder total amount;
B, stirring, the ceramic concentrate suspension of above-mentioned preparation is carried out stirring ball-milling 1～48h, the blank of preparation dynamic viscosity＜0.25Pas remains on blank temperature between 0～25 ℃, by adding 0.1～30ml initator in every 1000g water. and the limit is evenly stirred the limit and is carried out froth in vacuum;
C, pressure injection, infiltration, curing, fiber preform is placed in the press injector mould, again the above-mentioned high solid loading that stirs, low viscosity ceramic size are joined in the press injector feed compartment, injection under pressure and ultrasonic vibration condition, filling, infiltration fiber preform behind the mold closing, after treating that this process is fully carried out, implement the heating pressurize, mold temperature is between 25～95 ℃, institute's plus-pressure is between 0.1～200Mpa, dwell time is between 1min～30min, blank solidifies under the effect of temperature and pressure, and with fiber preform secure bond combined shaping;
D, the demoulding, the demoulding obtains the FRCMC blank, carries out sintering then and obtains finished product.
The technology that the present invention proposes is a kind of low cost of preparation high-performance complicated shape FRCMC of innovation, the near net-shape forming technique, the infiltration of ceramic base blank in fiber preform is compound to be realized by following method: elder generation is scattered in ceramic powder in the aqueous solution that contains organic monomer and forms stable and uniform, high solid loading, low viscosity slurry, again slurry is injected under pressure, be infiltrated up in the fiber preform that is preset in the mould, then in certain catalysis, temperature, under the pressure condition, the organic monomer polymerization crosslinking becomes tridimensional network, be infiltrated up to the slurry in-situ solidifying in the fiber preform, with the fiber preform combined shaping, obtain the FRCMC base substrate.The forming technique that the present invention proposes is compared with existing FRCMC shaping technology of preparing, all has obvious superiority, curring time is short, the production efficiency height, forming temperature is low, to the ceramic species wide adaptability, but the FRCMC goods of shaping form complexity, content of organics is minimum in the blank, and degreasing process is significantly simplified, and degreasing time shortens greatly.The present invention combines pressure injection, annotates the principle of coagulating, infiltrating, and in order to preparation complicated shape, even, the high-intensity ceramic matric composite base substrate of structural constituent density, carries out sintering again and obtains the high tenacity ceramic matrix composite articles.
The specific embodiment
The present invention is further detailed explanation below in conjunction with specific embodiment.
Embodiment 1 fiber reinforcement alumina ceramic-base composites forming technique
Commercially available α-Al
2O
3Powder material about particle average grain diameter 1 μ m, is sneaked into 5wt%ZrO
2Nano-powder, the acrylamide and the methylene-bisacrylamide that dissolve in 18wt% in deionized water form premixed liquid, and acrylamide and methylene-bisacrylamide ratio are 62: 1, add 0.3wt%Al in the premixed liquid
2O
3The organic dispersing agent of powder quality---modified polyacrylic acid ammonium; the composite ceramic material that adds the 54vol% volume fraction then; make the ceramic size of viscosity＜0.25Pas through stirring ball-milling; the ratio that adds the 3ml ammonium persulfate in 1000g water adds initator in blank; mix the final vacuum de-bubble; the perforated grill shape precast body of SiC short fiber whisker being made fiber content 25% places in the mould; again with the above-mentioned high solid loading that stirs; the low viscosity ceramic size joins in the press injector feed compartment; under pressure and under the ultrasonic vibration condition, inject behind the mold closing; filling; the infiltration fiber preform; after treating that this process is fully carried out; implement the heating pressurize; mold temperature is 60 ℃, and institute's plus-pressure is 50MPa, solidified forming behind the 5min; the demoulding obtains the FRCMC blank, and sintering obtains finished product then.
Embodiment 2 fiber reinforcement SiC ceramic matric composite forming techniques
Commercially available SiC powder, particle diameter are 0.6 μ m, with 3wt% (B
4C+C) powder mixes, and the oxirane monomers and the ethylene glycol that dissolve in 14wt% in deionized water form premixed liquid, and oxirane and ethylene glycol ratio are 10: 1.Dispersant---the tetramethyl ammonium hydroxide that in premixed liquid, adds 0.3wt% hybrid ceramic powder quality; the composite ceramic material that adds the 57vol% volume fraction then; make the ceramic size of viscosity＜0.25Pas through stirring ball-milling; the ratio that adds the 2ml tetramethylethylenediamine in 1000g water adds initator in blank; mix the final vacuum de-bubble; the 3 D weaving precast body that long carbon fiber is formed places in the mould; fiber volume fraction 40%; with the above-mentioned high solid loading that stirs; the low viscosity ceramic size joins in the press injector feed compartment; under pressure and ultrasonic vibration condition, inject behind the mold closing; filling; the infiltration fiber preform; after treating that this process is fully carried out; implement the heating pressurize; mold temperature is 60 ℃, and institute's plus-pressure is 50MPa, solidified forming behind the 10min; the demoulding obtains the FRCMC blank, and sintering obtains finished product then.
Embodiment 3 fiber reinforcement Si
3N
4The ceramic matric composite forming technique
Commercially available Si
3N
4Powder, particle diameter 0.6 μ m sneaks into 10wt% (Y
2O
5+ Al
2O
3) powder; the acrylamide and the methylene-bisacrylamide that dissolve in 16wt% in deionized water form premixed liquid; acrylamide and methylene-bisacrylamide ratio are 50: 1; the organic dispersing agent polycarboxylic acids ammonium that adds 0.01wt% composite ceramic material quality in the premixed liquid; the composite ceramic material that adds 53wt% then; make the ceramic size of viscosity＜0.25Pas through stirring ball-milling; the ratio that adds the 2ml ammonium persulfate in 1000g water adds initator in blank; mix the final vacuum de-bubble; long carbon fiber 3 D weaving precast body is placed in the mould; fiber volume fraction 36%, with the above-mentioned high solid loading that stirs, the low viscosity ceramic size joins in the press injector feed compartment; under pressure and ultrasonic vibration condition, inject behind the mold closing; filling; the infiltration fiber preform; after treating that this process is fully carried out, implement the heating pressurize, mold temperature is 60 ℃; institute's plus-pressure is 50MPa; solidified forming behind the 10min, the demoulding obtains the FRCMC blank, and sintering obtains finished product then.
The key of present technique, the one, flow filling, infiltration process of the ceramic batch pressure injection after guaranteeing to dispose is reliable.The 2nd, realize that quick in situ solidifies, should be controlled at 1min～30min hardening time.Curing rate is fast, the controllability of technology, operability worsens, on the contrary curing rate is slow, and production efficiency is low.The way that solves is: by regulating monomer, initiator type and consumption, reduce blank temperature and postpone hardening time, in parking before blank solidifies, the operating process, temperature should be controlled between 0～25 ℃, so the container of splendid attire blank and press feed compartment should adopt water-cooled.The realization of the quick solidified forming of blank realizes by heating mould and pressurization pressurize.That is to say that blank flows and not allow to occur any curing phenomenon before the filling infiltration filling type, and after solidified forming as early as possible.
Claims (5)
1, a kind of formation techn of fiber reinforced ceramic-base composite material is characterized in that: this technology comprises following each step:
A, batching, the gel monomer and the cross-linking monomer that add 6～35wt% in water are mixed with premixed liquid, the ratio of gel monomer and cross-linking monomer is between 5: 1～250: 1, and in premixed liquid, add the organic dispersing agent of ceramic powder quality 0.01～1wt%, add ceramic powder again in above-mentioned premixed liquid, addition is 50～60vol% volume fraction of premixed liquid and ceramic powder total amount;
B, stirring, the ceramic concentrate suspension of above-mentioned preparation is carried out stirring ball-milling 1～48h, and the blank of preparation dynamic viscosity＜0.25Pas remains on blank temperature between 0～25 ℃, by adding 0.1～30ml initator in every 1000g water, the limit is evenly stirred the limit and is carried out froth in vacuum;
C, pressure injection, infiltration, curing, fiber preform is placed in the press injector mould, again the above-mentioned high solid loading that stirs, low viscosity ceramic size are joined in the press injector feed compartment, injection under pressure and ultrasonic vibration condition, filling, infiltration fiber preform behind the mold closing, after treating that this process is fully carried out, implement the heating pressurize, mold temperature is between 25～95 ℃, institute's plus-pressure is between 0.1～200Mpa, dwell time is between 1min～30min, blank solidifies under the effect of temperature and pressure, and with fiber preform secure bond combined shaping;
D, the demoulding, the demoulding obtains the FRCMC blank, carries out sintering then and obtains finished product.
2, formation techn of fiber reinforced ceramic-base composite material according to claim 1 is characterized in that: the perforated grill shape precast body that described fiber preform forms for the short fiber whisker.
3, formation techn of fiber reinforced ceramic-base composite material according to claim 1 is characterized in that: described fiber preform is the 3 D weaving precast body that long fibre forms.
4, according to claim 1 or 2 or 3 described formation techn of fiber reinforced ceramic-base composite material, it is characterized in that: described organic monomer is an acrylamide, and described cross-linking monomer is a methylene-bisacrylamide.
5, according to claim 1 or 2 or 3 described formation techn of fiber reinforced ceramic-base composite material, it is characterized in that: described initator is an ammonium persulfate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02137852 CN1387984A (en) | 2002-06-25 | 2002-06-25 | Formation techn of fiber reinforced ceramic-base composite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02137852 CN1387984A (en) | 2002-06-25 | 2002-06-25 | Formation techn of fiber reinforced ceramic-base composite material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1387984A true CN1387984A (en) | 2003-01-01 |
Family
ID=4749146
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 02137852 Pending CN1387984A (en) | 2002-06-25 | 2002-06-25 | Formation techn of fiber reinforced ceramic-base composite material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1387984A (en) |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100415690C (en) * | 2006-06-30 | 2008-09-03 | 中国科学院上海硅酸盐研究所 | Process for preparing composite materials capable of forming oxidation-resisting structure on the surface of fiber by in-situ reaction |
| CN100572312C (en) * | 2004-11-26 | 2009-12-23 | 鸿富锦精密工业（深圳）有限公司 | Die and manufacture method thereof |
| CN101717268A (en) * | 2009-11-06 | 2010-06-02 | 上海美标陶瓷有限公司 | Blank for mending ceramic paste preforms and preparation method and mending process thereof |
| CN103770195A (en) * | 2012-10-17 | 2014-05-07 | 上海久牵实业有限公司 | Fiber ceramic powder compression forming process |
| CN104942967A (en) * | 2015-05-27 | 2015-09-30 | 吾晓于 | Ceramic matrix composite material forming technology |
| CN106904952A (en) * | 2017-01-13 | 2017-06-30 | 航天材料及工艺研究所 | A kind of high-temperature-resistant high alumina fibre enhancing composite and preparation method thereof |
| CN109485444A (en) * | 2018-12-25 | 2019-03-19 | 中国科学院长春光学精密机械与物理研究所 | A kind of preparation method of silicon carbide fiber reinforced composite material |
| CN110563478A (en) * | 2019-10-15 | 2019-12-13 | 航天特种材料及工艺技术研究所 | fiber-reinforced ceramic matrix composite material and preparation method and application thereof |
| CN112279663A (en) * | 2020-10-29 | 2021-01-29 | 上海交通大学 | Method for preparing continuous fiber reinforced ceramic matrix composite by flash firing technology |
| CN112976221A (en) * | 2021-01-29 | 2021-06-18 | 河北工业大学 | 3D printing forming equipment and method for continuous fiber/ceramic composite material blank |
| CN114247729A (en) * | 2021-11-30 | 2022-03-29 | 陈文娟 | Method for quickly making bricks by using construction wastes |
-
2002
- 2002-06-25 CN CN 02137852 patent/CN1387984A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100572312C (en) * | 2004-11-26 | 2009-12-23 | 鸿富锦精密工业（深圳）有限公司 | Die and manufacture method thereof |
| CN100415690C (en) * | 2006-06-30 | 2008-09-03 | 中国科学院上海硅酸盐研究所 | Process for preparing composite materials capable of forming oxidation-resisting structure on the surface of fiber by in-situ reaction |
| CN101717268A (en) * | 2009-11-06 | 2010-06-02 | 上海美标陶瓷有限公司 | Blank for mending ceramic paste preforms and preparation method and mending process thereof |
| CN101717268B (en) * | 2009-11-06 | 2014-01-01 | 上海美标陶瓷有限公司 | Blank for mending ceramic paste preforms and preparation method and mending process thereof |
| CN103770195A (en) * | 2012-10-17 | 2014-05-07 | 上海久牵实业有限公司 | Fiber ceramic powder compression forming process |
| CN104942967A (en) * | 2015-05-27 | 2015-09-30 | 吾晓于 | Ceramic matrix composite material forming technology |
| CN106904952A (en) * | 2017-01-13 | 2017-06-30 | 航天材料及工艺研究所 | A kind of high-temperature-resistant high alumina fibre enhancing composite and preparation method thereof |
| CN109485444A (en) * | 2018-12-25 | 2019-03-19 | 中国科学院长春光学精密机械与物理研究所 | A kind of preparation method of silicon carbide fiber reinforced composite material |
| CN110563478A (en) * | 2019-10-15 | 2019-12-13 | 航天特种材料及工艺技术研究所 | fiber-reinforced ceramic matrix composite material and preparation method and application thereof |
| CN110563478B (en) * | 2019-10-15 | 2022-02-01 | 航天特种材料及工艺技术研究所 | Fiber-reinforced ceramic matrix composite material and preparation method and application thereof |
| CN112279663A (en) * | 2020-10-29 | 2021-01-29 | 上海交通大学 | Method for preparing continuous fiber reinforced ceramic matrix composite by flash firing technology |
| CN112976221A (en) * | 2021-01-29 | 2021-06-18 | 河北工业大学 | 3D printing forming equipment and method for continuous fiber/ceramic composite material blank |
| CN114247729A (en) * | 2021-11-30 | 2022-03-29 | 陈文娟 | Method for quickly making bricks by using construction wastes |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103113124B (en) | Preparation method of fiber-toughened SiC ceramic-based composite material three-dimensional member | |
| CN104647760B (en) | A kind of 3D printing manufacture method of short fiber reinforced thermosetting resin joint product | |
| CN106278335B (en) | A kind of manufacturing method of fiber alignment toughening ceramic based composites turbo blade | |
| CN1387984A (en) | Formation techn of fiber reinforced ceramic-base composite material | |
| CN107673763A (en) | The method for preparing ceramic structures by fused glass pellet 3D printing using thermoplasticity ceramic forerunner | |
| CN1314725C (en) | Novel light-wave absorbing carbon fiber composite material preparation method | |
| CN104496508A (en) | Method for manufacturing SiC ceramic-based turbine blade based on photocurable 3D printing | |
| CN111040385B (en) | 3D printing grid ceramic reinforced resin composite material and preparation method thereof | |
| CN107686366A (en) | A kind of preparation method of nano wire and whisker coordination plasticizing ceramic matric composite | |
| CN101224989A (en) | Two-dimensional fiber cloth reinforced composite material and preparation method thereof | |
| CN102146196B (en) | Preparation method of high-damping epoxy resin composite material | |
| CN109761613A (en) | The short carbon fiber toughened ceramic composite forming method of gel injection-moulding based on 3D printing | |
| CN1775514A (en) | Injection apparatus for resin transfer moulding technology | |
| CN109485444A (en) | A kind of preparation method of silicon carbide fiber reinforced composite material | |
| CN108017378A (en) | A kind of water-based alumina base 3D printing base substrate method and its forming method | |
| CN109943024A (en) | A kind of solidified resin and its application being used to prepare carbon fibre composite | |
| CN111005229B (en) | Carbon fiber sizing agent and preparation method thereof | |
| KR20010050316A (en) | Low Volume Fraction Metal Matrix Preforms | |
| CN1915625A (en) | Method for preparing gradient material of strong magnetism and weak magnetism through pressure filtration molding in pulse magnetism | |
| CN1187289C (en) | Method for preparing gelatin mold made from functional gradient material in static magnetic field | |
| CN101386540A (en) | Ceramic-base compound material and forming technique | |
| CN1206069C (en) | Press filtering process to form functional gradient material in static magnetic field | |
| CN115849928B (en) | Injection-molded aluminum oxide fiber reinforced composite material containing lanthanum phosphate interface layer and preparation method thereof | |
| CN104890259B (en) | A kind of Processes and apparatus of fiber reinforcement MC nylon | |
| CN1164371C (en) | Process for preparing C/C composite material fastly using super critical fluid technology |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |