CN100348537C - Fiber reinforced alumina ceramic-base composites and method for preparing same - Google Patents
Fiber reinforced alumina ceramic-base composites and method for preparing same Download PDFInfo
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- CN100348537C CN100348537C CNB2006100919755A CN200610091975A CN100348537C CN 100348537 C CN100348537 C CN 100348537C CN B2006100919755 A CNB2006100919755 A CN B2006100919755A CN 200610091975 A CN200610091975 A CN 200610091975A CN 100348537 C CN100348537 C CN 100348537C
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Abstract
The present invention relates to a plasticizing alumina ceramic basis composite material of a mullite fiber, and a preparation method thereof. The composite material is prepared from the following raw materials of 69 wt% to 84.5 wt% of alpha-Al2 O3, 10 wt% to 20 wt% of mullite fibers, 0.5 wt% to 1 wt% of TiO2 and 5 wt% to 10 wt% of cosolvent CaO+MgO+SiO2. Compared with pure alumina ceramics, the bending strength of the composite material is enhanced 2 to 3 times, and the fracture toughness of the composite material is enhanced 4 to 5 times. The mechanical performance of alumina ceramics is enhanced. The traditional pressureless sintering technology is adopted by the preparation method, and the preparation method has the advantages of simple technology, short production period, low production cost, the convenient preparation of large members, convenient large-scale production, etc.
Description
(1) technical field under
The present invention relates to a kind of fiber reinforced alumina ceramic-base composites, particularly a kind of mullite fiber reinforced alumina ceramic-base composites, and their preparation method.
(2) background technology
Along with the developing rapidly and advance by leaps and bounds of science and technology, more and more higher, more and more tighter and increasing requirement is proposed material property.In many aspects, traditional single-material can not satisfy actual needs.Compoundization of material just becomes one of inexorable trend of material development, and it is extremely urgent to develop high performance matrix material.
Fiber reinforced ceramic matric composite be with fiber as toughness reinforcing body, fiber reinforced ceramic matrix by the combine general name of the material formed of certain recombining process.This class matrix material has high strength, high tenacity, excellent thermostability and chemical stability, is a class new structural material, is the most promising a kind of in the ceramic matric composite.Therefore, in recent years, the development of fiber reinforced ceramic matric composite is quite rapid.
The evolution that is used for the fiber of toughening ceramic based composites is: be steel fiber at first, as: W, Mo, Ta etc., they can obtain higher fracture toughness property (K
IC) and room temperature strength, but oxidation easily takes place when high temperature; Next is the C fiber, and it has higher intensity and Young's modulus, but equally easily oxidation takes place at high temperature, and with many ceramic matrix generation chemical reactions, make its reduction; Be on-oxide ceramic fibres such as SiC then, they have advantages such as good toughness, good stability, but shortcoming also is that high temperature oxidation easily takes place, and fiber weakness is big; Be exactly oxide fibre in addition; modal is sapphire whisker and mullite fiber; this fibrid temperature antioxidant property is good; can be applicable to 1400 ℃ high temperature occasion; production process is simple, equipment requirements is not high, does not need protection of inert gas etc., compares with other pyroceramics; having high cost performance and very big commercial value, is the inorganic fibre that enjoys attention in recent years.
In addition, because mullite fiber has been realized fairly large suitability for industrialized production in recent years, cost reduces greatly, and mullite fiber reinforced alumina ceramic-base composites manufacturing cost is reduced greatly, becomes possibility as structural timber.
In recent years, along with progress of science and technology, the method for preparing matrix material is also more and more, mainly contains following several:
Mud pickling process/pressure sintering is the traditional method of preparation fiber reinforcement glass and low melting point ceramic matric composite.But this method is because following deficiency is restricted its range of application: (1) hot pressing causes damage easily to fiber for the three-dimensional fiber reinforced composite; (2) because the limitation of heat pressing process is difficult to make complex-shaped large-scale component, so he can only prepare the CFCC material of one dimension or two dimension.
Chemical gas phase pickling process (Chemical Vapor Infiltration is called for short the CVI method) is the novel process that CFCC makes that is specifically designed to that grows up on chemical vapour deposition (chemical vapor reposition is called for short CVD) technology basis.Common CVI technology generally is that to utilize resistive heating to carry out matrix sedimentary, this general type of heating makes CVI preparation technology have the following shortcoming that is difficult to overcome: (1) deposition process has the trend of preferentially carrying out in billet surface, this just causes the sealing of deposition passage between fiber in the base substrate easily, hinders carrying out smoothly of CVI; (2) void content height, density unevenness is even.(3) size of sample and thickness all are restricted; (4) take time longlyer, energy consumption is big, material preparation cost height.
Polymer impregnated cracking process claims precursor conversion method or precursor cracking process again, is the preparation technology of development in recent years a kind of FRCMC of getting up.Similar to sol-gel, the precursor conversion method also is to utilize organic precursor method cracking at high temperature and a kind of method of being converted into the inorganic ceramic matrix.But because small molecules overflows in the Pintsch process process, the porosity height of material is difficult to prepare the material of complete densification; And be converted into the inorganic ceramic process from organic precursor method that material is long-pending to be shunk greatly, shrink the performance that the internal stress that produces is unfavorable for improving material, preparation cycle is long.
The molten metal direct oxidation method is effective ways of making the three-dimensional net structure FRCMC, because of being that U.S. Lanxide company at first proposes and begins one's study, so is called the Lanxide method again.Because more or less meeting is residual in the matrix material a certain amount of metal arranged, cause the high-temperature creep resistance of material to reduce.Prepared material density is low to have a certain amount of metal because more or less meeting is residual in the matrix material, causes the high-temperature creep resistance of material to reduce.Prepared material density is lower.
(3) summary of the invention
The present invention is in order to solve the shortcoming of alumina-ceramic poor toughness, improve its bending strength and fracture toughness property, a kind of fiber reinforced alumina ceramic-base composites is provided, has good thermodynamic compatibility, make matrix material generation fiber when fracture extract and glue and take off effect, can increase substantially the bending strength and the fracture toughness property of alumina-ceramic, it is applied in more field.
Another object of the present invention is to provide the preparation method of above-mentioned matrix material, this preparation method has that technology is more simple, the production cycle is shorter, production cost is lower, be convenient to prepare advantages such as large-scale component, the scale operation of being more convenient for.
The present invention realizes by following measure:
Fiber reinforced alumina ceramic-base composites of the present invention is to be made by following raw materials by weight percent:
α-A1
2O
3Be 69%～84.5%,
Mullite fiber is 10%～20%,
TiO
2Be 0.5%～1%,
Fusing assistant CaO+MgO+SiO
2Be 5%～10%.
The fiber reinforced alumina ceramic-base composites of the invention described above, described α-Al
2O
3Powder is 2000～2500 orders, and the length of mullite fiber is 3～7mm.
The fiber reinforced alumina ceramic-base composites of the invention described above, described CaO, MgO, SiO
2The per-cent that accounts for the fusing assistant gross weight respectively is 30%, 9%, 61%.
The preparation method of the fiber reinforced alumina ceramic-base composites of the invention described above may further comprise the steps:
With α-Al
2O
3Powder and fusing assistant ball milling mixed 72～90 hours, and grinding medium is a dehydrated alcohol, dry back sieving for standby;
Mullite fiber is cut into 3～7mm length, with acetone fiber is carried out surface treatment, handle washing with water after 24～48 hours, with magnetic stirrer it is disperseed, dry back is standby;
With mixed α-Al
2O
3, the fusing assistant powder and handle after mullite fiber put into ball grinder by a certain percentage, add grinding element and dispersion agent simultaneously, the weight ratio of grinding element and raw material is 2: 1, the weight ratio of dispersion agent and raw material is 1: 1, ball milling also fully stirs, behind the ball milling 2～3 hours, through 36～48 hours dryings, temperature was 80～100 ℃; Add polyvinyl alcohol and carry out granulation, stewing material 24 hours adopts the shaping method to suppress compacting in flakes then, and forming pressure is 50～100Mpa; Then with base substrate 80～100 ℃ baking oven inner drying 36～48 hours, to the sample of oven dry in traditional non-pressure sintering furnace through 1450～1500 ℃ of sintering, soaking time is 2～3 hours.
The mullite fiber that the present invention selects for use has that high-temperature oxidation resistance is good, the stable performance of high temperature calorifics, good with alumina ceramic-base body heat mechanics matching, the more important thing is that the two interface bond strength is moderate, producing fiber during fracture of composite materials extracts and glues and take off, can increase substantially the bending strength and the fracture toughness property of alumina-ceramic, make matrix material have excellent mechanical property and thermal property, prolong the work-ing life of matrix material.Therefore, such composite study has wide significance with exploitation for the range of application of widening alumina-ceramic and minimizing catastrophic failure.
Added a small amount of solubility promoter simultaneously, alumina-ceramic can be reduced the surface reaction degree between fiber and the aluminum oxide, and improve bending strength and fracture toughness property at dense sintering under the cold condition.Make its can be under 1450～1500 ℃ condition dense sintering, cut down the consumption of energy, enhance productivity.
The three-point bending strength of general pure alumina pottery is 280～330MPa, and fracture toughness property is 2～3MPa
1/2And the fiber reinforced alumina ceramic-base composites that the present invention becomes as toughness reinforcing system with mullite fiber, its bending strength improves 2～3 times with pure alumina ceramic phase ratio, and fracture toughness property improves 4～5 times, improves the mechanical property of alumina-ceramic.
Preparation method of the present invention adopts traditional pressureless sintering technology to prepare matrix material, and excellent performance improves the bending strength and the fracture toughness property of alumina-ceramic greatly, has increased the toughness of alumina-ceramic.Compare with other methods that prepare fiber reinforced ceramic matric composite, sintering method of the present invention has that technology is more simple, the production cycle is shorter, production cost is lower, be convenient to prepare advantages such as large-scale component, the scale operation of being more convenient for.
(4) embodiment
Embodiment 1:
Take by weighing following raw materials by weight percent, adopt following preparation method, the preparation fiber reinforced alumina ceramic-base composites gets matrix material 1.
2000 order α-Al
2O
3Be 79%,
The mullite fiber of 5mm is 10%,
TiO
2Be 1%,
Fusing assistant CaO+MgO+SiO
2Be 10%.Wherein CaO, MgO, SiO
2The per-cent that accounts for the fusing assistant gross weight respectively is 30%, 9%, 61%.
Adopt following method preparation:
With α-Al
2O
3Powder and fusing assistant ball milling mixed 72～90 hours, and grinding medium is a dehydrated alcohol, dry back sieving for standby;
Mullite fiber carries out surface treatment with acetone to fiber, handles to wash with water after 24～48 hours, with magnetic stirrer it is disperseed, and dry back is standby;
With mixed α-Al
2O
3, the fusing assistant powder and handle after mullite fiber put into ball grinder by a certain percentage, add grinding element and dispersion agent simultaneously, the weight ratio of grinding element and raw material is 2: 1, the weight ratio of dispersion agent and raw material is 1: 1, ball milling also fully stirs, behind the ball milling 2～3 hours, through 36～48 hours dryings, temperature was 80～100 ℃; Add polyvinyl alcohol and carry out granulation, stewing material 24 hours adopts the shaping method to suppress compacting in flakes then, and forming pressure is 50～100Mpa; Then with base substrate 80～100 ℃ baking oven inner drying 36～48 hours, to the sample of oven dry in traditional non-pressure sintering furnace through 1450～1500 ℃ of sintering, soaking time is 2～3 hours.
Embodiment 2
Take by weighing following raw materials by weight percent, adopt the preparation method of embodiment 1, the preparation fiber reinforced alumina ceramic-base composites gets matrix material 2.
2500 order α-Al
2O
3Be 74%,
The 6mm mullite fiber is 20%,
TiO
2Be 1%
Fusing assistant CaO+MgO+SiO
2Be 5%.Wherein CaO, MgO, SiO
2The per-cent that accounts for the fusing assistant gross weight respectively is 30%, 9%, 61%.
Embodiment 3
Take by weighing following raw materials by weight percent, adopt the preparation method of embodiment 1, the preparation fiber reinforced alumina ceramic-base composites gets matrix material 3.
2500 order α-Al
2O
3Be 76%,
The 4mm mullite fiber is 15%,
TiO
2Be 1%,
Fusing assistant CaO+MgO+SiO
2Be 8%.Wherein CaO, MgO, SiO
2The per-cent that accounts for the fusing assistant gross weight respectively is 30%, 9%, 61%.
Embodiment 4
Take by weighing following raw materials by weight percent, adopt the preparation method of embodiment 1, the preparation fiber reinforced alumina ceramic-base composites gets matrix material 4.
1600 order α-Al
2O
3Be 83%,
The 2mm mullite fiber is 10%,
TiO
2Be 0.5%,
Fusing assistant CaO+MgO+SiO
2Be 6.5%.Wherein CaO, MgO, SiO
2The per-cent that accounts for the fusing assistant gross weight respectively is 30%, 20%, 50%.
Embodiment 5
Take by weighing following raw materials by weight percent, adopt the preparation method of embodiment 1, the preparation fiber reinforced alumina ceramic-base composites gets matrix material 3.
2500 order α-Al
2O
3Be 70.5%,
The 4mm mullite fiber is 20%,
TiO
2Be 0.5%,
Fusing assistant CaO+MgO+SiO
2Be 9%.Wherein CaO, MgO, SiO
2The per-cent that accounts for the fusing assistant gross weight respectively is 50%, 9%, 41%.
By U.S. ASTM C1161-90-990 (flexural strength standard test methods under the advanced ceramics room temperature) and ASTM C1421-2001 (advanced ceramic fracture toughness property testing standard under the room temperature) standard, the matrix material of above-mentioned preparation is carried out Mechanics Performance Testing, concrete numerical value such as following table:
| Matrix material 1 | Matrix material 2 | Matrix material 3 | Matrix material 4 | Matrix material 5 | |
| Flexural strength (MPa) | 556.55 | 610.32 | 704.52 | 532.37 | 596.54 |
| Fracture toughness property (MPa 1/2) | 8.36 | 9.71 | 12.04 | 7.92 | 10.28 |
Claims (4)
1. fiber reinforced alumina ceramic-base composites is characterized in that: be to make by following raw materials by weight percent,
α-Al
2O
3Be 69%～84.5%,
Mullite fiber is 10%～20%,
TiO
2Be 0.5%～1%,
Fusing assistant CaO+MgO+SiO
2Be 5%～10%.
2. fiber reinforced alumina ceramic-base composites according to claim 1 is characterized in that: described α-Al
2O
3Be 2000～2500 orders, the length of mullite fiber is 3～7mm.
3. fiber reinforced alumina ceramic-base composites according to claim 1 is characterized in that: described CaO, MgO, SiO
2The per-cent that accounts for the fusing assistant gross weight respectively is 30%, 9%, 61%.
4. the preparation method of the described fiber reinforced alumina ceramic-base composites of claim 1 is characterized in that: may further comprise the steps,
(1) with α-Al
2O
3Mixed 72～90 hours with the fusing assistant ball milling, grinding medium is a dehydrated alcohol, dry back sieving for standby;
(2) mullite fiber is cut into 3～7mm length, with acetone fiber is carried out surface treatment, handle washing with water after 24～48 hours, with magnetic stirrer it is disperseed, dry back is standby;
(3) with mixed α-Al
2O
3, TiO
2Put into ball grinder in proportion with the mullite fiber after handling, add grinding element and dispersion agent simultaneously, the weight ratio of grinding element and raw material is 2: 1, the weight ratio of dispersion agent and raw material is 1: 1, ball milling also fully stirs, behind the ball milling 2～3 hours, through 36～48 hours dryings, temperature was 80～100 ℃; Add polyvinyl alcohol and carry out granulation, stewing material 24 hours adopts the shaping method to suppress compacting in flakes then, and forming pressure is 50～100MPa; Then with base substrate 80～100 ℃ baking oven inner drying 36～48 hours, to the sample of oven dry in traditional non-pressure sintering furnace through 1450～1500 ℃ of sintering, soaking time is 2～3 hours.
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| CN102225863A (en) * | 2011-04-12 | 2011-10-26 | 陕西理工学院 | Preparation method of alumina-based composite continuous fibers |
| CN104122202B (en) * | 2014-07-29 | 2017-05-03 | 厦门大学 | Method for testing interfacial bonding strength of ceramic fiber-reinforced resin matrix composite material |
| CN104355650A (en) * | 2014-10-29 | 2015-02-18 | 安徽省皖捷液压科技有限公司 | Cracking-resistant ceramic for nozzles and preparation method of crack-resisting ceramic |
| CN104355649A (en) * | 2014-10-29 | 2015-02-18 | 安徽省皖捷液压科技有限公司 | Special ceramics for nozzle and preparation method for special ceramics |
| CN105272288B (en) * | 2015-10-16 | 2018-05-29 | 河南东普热能科技有限公司 | Microwave high-temperature special-purpose thermal insulation refractory material and preparation method thereof |
| CN106810285A (en) * | 2017-01-14 | 2017-06-09 | 中国矿业大学(北京) | A kind of preparation method of the carbon fiber-reinforced aluminium oxide ceramics of in-situ preparation |
| CN107619262B (en) * | 2017-08-01 | 2020-08-14 | 德化县凯得利工艺品有限公司 | Bone china and preparation method thereof |
| CN107555958A (en) * | 2017-09-02 | 2018-01-09 | 佛山市嘉亿艺术陶瓷研究有限公司 | A kind of pottery mullite fiber toughness reinforcing clay |
| CN109336565A (en) * | 2018-12-24 | 2019-02-15 | 焦作市德邦科技有限公司 | A kind of preparation method of Zirconia reinforced alumina wear-resistant ceramic |
| CN113816729B (en) * | 2021-08-17 | 2023-07-04 | 山东大学 | Electrostatic spinning nanofiber toughened alumina ceramic and preparation method thereof |
| CN115180968A (en) * | 2022-08-02 | 2022-10-14 | 宜兴市海森陶瓷科技有限公司 | Novel fiber-toughened alumina ceramic and preparation method thereof |
| CN116621592B (en) * | 2023-05-31 | 2024-03-22 | 苏州晶瓷超硬材料有限公司 | Corrosion-resistant alumina ceramic and preparation method thereof |
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