CN102212764A - Method for preparing ramie-structured Al2O3 ceramic/Al-based composite material - Google Patents
Method for preparing ramie-structured Al2O3 ceramic/Al-based composite material Download PDFInfo
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- CN102212764A CN102212764A CN2011101257692A CN201110125769A CN102212764A CN 102212764 A CN102212764 A CN 102212764A CN 2011101257692 A CN2011101257692 A CN 2011101257692A CN 201110125769 A CN201110125769 A CN 201110125769A CN 102212764 A CN102212764 A CN 102212764A
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- ramie
- aqueous solution
- pottery
- based composites
- ramee
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Abstract
The invention discloses a method for preparing a ramie-structured Al2O3 ceramic/Al-based composite material, which comprises the following steps: firstly, pretreating ramie fibers; subsequently, immersing the pretreated ramie fibers in an Al(OH)3 hydroxide aqueous solution of which the mass concentration is 15% in a vacuum-pressure impregnation mode, drying, and repeating the operation until the weight ratio of the hydroxide to the ramie fibers is 5:(4-6), thus obtaining a ramie/Al(OH)3 precursor; then, sintering and annealing the ramie/Al(OH)3 precursor in the presence of oxygen, thus obtaining a ramie-structured porous Al2O3 ceramic preform; and finally, in a vacuum pressure impregnation device, impregnating the ramie-structured porous Al2O3 ceramic preform with aluminum alloy. The ramie-structured Al2O3 ceramic/Al-based composite material prepared by the method has the characteristics of light weight, vibration damping, noise absorption and good friction and wear resistance, and can reduce the thermal expansion coefficient and density, thereby having wide application prospects.
Description
Technical field
The invention belongs to the composite preparing technical field, relate to a kind of preparation method of ecological ceramic/metal-base composites, be specifically related to a kind of ramie form Al for preparing
2O
3The method of pottery/Al based composites.
Background technology
At present, the technology of known ecological ceramic/metal-base composites has: 1. article " preparation and the performance analysis of high damping wood ceramics/MB15 matrix material " (matrix material journal [J], 2003,20(1): 8～11); 2. the article research theory and the progress of material " lose attitude " (material Leader [J], 2006,10:5～7); Article " progress of network interpenetrating structural composite material " (functional materials [J], 2002,33(1): 22～25); 4. article " wood ceramics matrix material " (investigation of materials journal [J], 2002,16:259～262) with network interpenetrating structure; 5. patent name: " preparation method of ecological ceramic/metal composite ", application number: 02137503.8, publication number: CN1403620, open day: 2003.03.19; 6. patent name: " flaxen fiber is lost the preparation method of attitude structure C/Sn or C/Al matrix material ", application number: 200810231642.7, publication number: CN101381855, open day: 2009.3.11; 7. patent name: " preparation method of hemp fabric construction morph-genetic C/metal composite ", application number: 201010301408.4, publication number: CN101838782, open day: 2010.9.22.
More than disclosed technology mainly relate to natural phant such as timber, bamboo, flaxen fiber and tobacco rod and lose the attitude structures and prepare biomorph C ceramic/metal composite materials, C ceramic composition in this class material has lubricated and cushioning effect, but there is not strengthening effect, thereby make the wear resistance of biomorph C ceramic/metal composite materials relatively poor, be difficult to industrial application.In addition, do not relate to more than and utilize ramee something lost attitude structure to prepare ramie form Al
2O
3Pottery/Al based composites.
Summary of the invention
The purpose of this invention is to provide a kind of ramie form Al for preparing
2O
3The method of pottery/Al based composites has solved mechanical strength and the relatively poor problem of wearability of existing biomorph C ceramic/metal composite materials.
The technical solution adopted in the present invention is a kind of ramie form Al for preparing
2O
3The method of pottery/Al based composites, specifically implement according to following steps:
Step 1: ramee is carried out pre-treatment;
Step 2: it is 15% Al(OH that the ramee after the pre-treatment that step 1 is obtained adopts vacuum-pressure infiltration mode to immerse mass concentration)
3In the hydroxide aqueous solution, take out drying, repeatable operation makes Al(OH)
3It is 5:4～6 that oxyhydroxide and ramee reach weight ratio, obtains ramie/Al(OH)
3Precursor;
Step 3: the ramie that step 2 is obtained/Al(OH)
3Precursor carries out aerobic sintering and annealing, obtains ramie form porous Al
2O
3Ceramic performs;
Step 4: in the vacuum pressure infiltration device, aluminium alloy is infiltrated the ramie form porous Al that step 3 obtains
2O
3Ceramic performs, aluminium alloy and porous Al
2O
3The volume ratio of ceramic performs is 5: 4, prepares ramie form Al of the present invention
2O
3Pottery/Al based composites.
Characteristics of the present invention also are,
The wherein pre-treatment in the step 1, comprise washing, beat fibre, come unstuck and alkaline purification, the described employing of coming unstuck is come unstuck fully or is not exclusively come unstuck, described alkaline purification is that ramee is soaked 10h～30h in mass concentration is 5%～25% the NaOH aqueous solution, be washed with water to neutrality again, 60～105 ℃ of drying 2～4h.
The Al(OH in the step 2 wherein)
3Hydroxide aqueous solution specifically is prepared from according to following steps: according to volume ratio is that 100:1～3 take by weighing the Al that volumetric molar concentration is 0.25mol/L
2(SO
4)
3The aqueous solution and ammoniacal liquor are at Al
2(SO
4)
3Aqueous solution dropping ammonia chemical coprecipitation prepares Al(OH)
3Nanometer oxyhydroxide is with Al(OH)
3Nanometer oxyhydroxide is water-soluble, and to obtain mass concentration be 15% Al(OH)
3Hydroxide aqueous solution.
Wherein aerobic sintering and the annealing in the step 3, specifically implement according to following steps: the ramie that step 2 is obtained/Al(OH)
3Precursor is put into atmosphere furnace, and it is 800～1200 ℃ that temperature is set, and heat preservation sintering 0.5～2h is again through 100～250 ℃ of annealing 2～4h.
Wherein in the step 4, the temperature that is provided with in the vacuum pressure infiltration device is 750～800 ℃, and pressure is 4～5MPa.
The invention has the beneficial effects as follows,
1, realize chemical composition and regulating microstructure by the ramee pre-treatment, ramee is respectively raw ramie, alkali treatment fiber crops and the degummed ramie of ramee after pre-treatment.
2, utilize the impregnation technology prioritization scheme to improve solution-ramie dipping uniformity, improve the sol impregnation rate.
3, obtain a kind of ramie form porous Al through high temperature aerobic calcine technology
2O
3Ceramic performs.
4, obtain ramie form Al through the vacuum pressure infiltration aluminium alloy
2O
3Pottery/Al based composites.
The present invention is based on ramee and lose the attitude structure, a kind of Al that ramee is lost the attitude structure that has is provided
2O
3The preparation method of pottery/Al based composites.The ramie form Al that the inventive method prepares
2O
3Pottery/Al based composites has light weight, the characteristics that weakening, sound-absorbing and anti-friction wear-resistant are good, and can reduce thermal coefficient of expansion and density, have broad application prospects.
Embodiment
The present invention is described in detail below in conjunction with embodiment.
The present invention prepares ramie form Al
2O
3The method of pottery/Al based composites, specifically implement according to following steps:
Step 1: ramee is carried out pre-treatment, comprise washing, beat fibre, come unstuck and alkaline purification, ramee comprises raw ramie, alkaline purification fiber crops and the degummed ramie of ramee.Come unstuck to adopt and come unstuck fully or not exclusively come unstuck, all adopt existing conventional weaving retting technology.Alkaline purification is that natural remie fiber is soaked 10h～30h in concentration is the NaOH aqueous solution of 5wt%～25wt%, is washed with water to neutrality (pH=7) again, 60～105 ℃ of drying 2～4h.
Step 2: the preparation of nanometer oxyhydroxide and vacuum-pressure impregnation: according to volume ratio is that 100:1～3 take by weighing the Al that volumetric molar concentration is 0.25mol/L
2(SO
4)
3The aqueous solution and ammoniacal liquor are at Al
2(SO
4)
3Aqueous solution dropping ammonia chemical coprecipitation prepares Al(OH)
3Nanometer oxyhydroxide.It is in 15% hydroxide aqueous solution that ramee after the pre-treatment that step 1 is obtained adopts vacuum-pressure infiltration mode to immerse mass concentration, takes out dry.Repeatable operation, making oxyhydroxide and ramee reach weight ratio is 5:4～6, the acquisition ramie/Al(OH)
3Precursor.
Step 3: aerobic sintering and annealing, the ramie that step 2 is obtained/Al(OH)
3Precursor is put into atmosphere furnace, through 800～1200 ℃, and insulation 0.5～2h sintering.After the taking-up, through 100～250 ℃ of annealing 2～4h, prepare ramie form porous Al again
2O
3Ceramic performs.
Step 4: vacuum pressure infiltration prepares ramie form Al
2O
3Pottery/Al based composites: in the vacuum pressure infiltration device, 750～800 ℃, under 4～5MPa pressure aluminium alloy infiltrated the ramie form porous Al that step 3 obtains
2O
3Ceramic performs, aluminium alloy and porous Al
2O
3The volume ratio of ceramic performs is 5: 4, prepares ramie form Al of the present invention
2O
3Pottery/Al based composites.
Embodiment 1
It is long that raw ramie is trimmed to 5～10mm, puts into 20wt%NaOH aqueous solution soaking 24h, is washed to pH and is neutral (pH=7), and 85 ℃ of vacuum-drying 3h are standby; Utilize Al
2(SO
4)
3Aqueous solution dropping ammonia chemical coprecipitation preparation of nano Al(OH)
3Flaxen fiber is immersed nanometer Al(OH)
3In the aqueous solution, take out 85 ℃ of dry 3h behind the 1h.Through repeatable operation, make Al
2O
3With the raw ramie weight ratio be 5:4.With the raw ramie behind the impregnation drying/Al(OH)
3Precursor is put into atmosphere furnace, and through 800 ℃, insulation 2h sintering is again through 150 ℃ of annealing 2h.In the vacuum pressure infiltration device, 750 ℃, under the 5MPa pressure aluminium alloy infiltrated ramie form porous Al
2O
3, aluminium alloy and porous Al
2O
3The volume ratio of ceramic performs is 5: 4, obtains to have the Al that flaxen fiber is lost the attitude structure
2O
3Pottery/Al based composites.
Embodiment 2
It is long that the alkaline purification fiber crops are trimmed to 5～10mm, puts into 20wt%NaOH aqueous solution soaking 24h, is washed to pH and is neutral (pH=7), and 85 ℃ of vacuum-drying 3h are standby; Utilize Al
2(SO
4)
3Aqueous solution dropping ammonia chemical coprecipitation preparation of nano Al(OH)
3Flaxen fiber is immersed nanometer Al(OH)
3In the aqueous solution, take out 85 ℃ of dry 3h behind the 1h.Through repeatable operation, make Al
2O
3With alkali treatment fiber crops weight ratio be 5:5.With alkali treatment fiber crops behind the impregnation drying/Al(OH)
3Precursor is put into atmosphere furnace, and through 1000 ℃, insulation 2h sintering is again through 200 ℃ of annealing 2h.In the vacuum pressure infiltration device, 750 ℃, under the 5MPa pressure aluminium alloy infiltrated ramie form porous Al
2O
3, aluminium alloy and porous Al
2O
3The volume ratio of ceramic performs is 5: 4, obtains to have the Al that flaxen fiber is lost the attitude structure
2O
3Pottery/Al based composites.
Embodiment 3
It is long that degummed ramie is trimmed to 5～10mm, puts into 20wt%NaOH aqueous solution soaking 24h, is washed to pH and is neutral (pH=7), and 85 ℃ of vacuum-drying 3h are standby; Utilize Al
2(SO
4)
3Aqueous solution dropping ammonia chemical coprecipitation preparation of nano Al(OH)
3Flaxen fiber is immersed nanometer Al(OH)
3In the aqueous solution, take out 85 ℃ of dry 3h behind the 1h.Through repeatable operation, make Al
2O
3With the flaxen fiber weight ratio be 5:6.With the degummed ramie behind the impregnation drying/Al(OH)
3Precursor is put into atmosphere furnace, through 1200 ℃, insulation 1h sintering, again through 200 ℃ of annealing 2h.In the vacuum pressure infiltration device, 800 ℃, under the 4MPa pressure aluminium alloy infiltrated ramie form porous Al
2O
3, aluminium alloy and porous Al
2O
3The volume ratio of ceramic performs is 5: 4, obtains to have the Al that flaxen fiber is lost the attitude structure
2O
3Pottery/Al based composites.
From the principle aspect beneficial effect of the present invention is described:
1. pre-treating technology is mainly realized the regulation and control to ramee chemical composition and microstructure, technological parameter in the pre-treatment is the parameter through optimization of orthogonal test, can make the ramee cross section expand round, middle hole obviously increases, fibre wall thickness increases, and more is conducive to the infiltration of nanometer hydroxide solution.
2. the technological parameter during reasonably the preparation of nanometer hydroxide and vacuum-pressure flood is conducive to obtain uniform nanometer hydroxide solution, improve infiltration uniformity and infiltration rate, be conducive to get rid of residual gas in the ramee by vacuum-pressure infiltration mode, guarantee that the nanometer hydroxide solution immerses in the ramee micropore.
3. reasonably aerobic sintering and annealing process can obtain ramie form porous Al2O
3Precast body can be eliminated the calcining defective by annealing.
4. the rational favourable formation infiltration of vacuum pressure infiltration technological parameter metal alloy liquid stream makes the molten aluminium alloy ramie form porous Al of infiltrating under pressure-suction effect2O
3Precast body.
The ramie form Al of the present invention's preparation2O
3Pottery/Al based composites is compared with existing composite, because porous Al2O
3Strengthen body and can form the three-dimensional network interpenetrating structure with aluminum matrix alloy, this novel three-dimensional network structure can suppress plastic deformation and the hot mastication of matrix alloy, can be so that the abrasion resistance raising of composite. Because of Al2O
3The three-dimensional net structure of ceramic enhancement phase uniqueness is conducive to and will concentrates on a little or stress on the face disperses in spatial dimension rapidly and transmits, and can significantly improve the composite impact resistance. Simultaneously, the structure of the three-dimensional co-continuous of its matrix and wild phase also may cause the structural interlock effect, so that material has higher damage tolerance.
Claims (5)
1. one kind prepares ramie form Al
2O
3The method of pottery/Al based composites is characterized in that, specifically implements according to following steps:
Step 1: ramee is carried out pre-treatment;
Step 2: it is 15% Al(OH that the ramee after the pre-treatment that step 1 is obtained adopts vacuum-pressure infiltration mode to immerse mass concentration)
3In the hydroxide aqueous solution, take out drying, repeatable operation makes Al(OH)
3It is 5:4～6 that oxyhydroxide and ramee reach weight ratio, obtains ramie/Al(OH)
3Precursor;
Step 3: the ramie that step 2 is obtained/Al(OH)
3Precursor carries out aerobic sintering and annealing, obtains ramie form porous Al
2O
3Ceramic performs;
Step 4: in the vacuum pressure infiltration device, aluminium alloy is infiltrated the ramie form porous Al that step 3 obtains
2O
3Ceramic performs, aluminium alloy and porous Al
2O
3The volume ratio of ceramic performs is 5: 4, prepares ramie form Al of the present invention
2O
3Pottery/Al based composites.
2. preparation ramie form Al according to claim 1
2O
3The method of pottery/Al based composites, it is characterized in that, pre-treatment in the described step 1, comprise washing, beat fibre, come unstuck and alkali treatment, the described employing of coming unstuck is come unstuck fully or is not exclusively come unstuck, described alkali treatment is that ramee is soaked 10h～30h in mass concentration is 5%～25% the NaOH aqueous solution, is washed with water to neutrality, 60～105 ℃ of drying 2～4h again.
3. preparation ramie form Al according to claim 1
2O
3The method of pottery/Al based composites is characterized in that, the Al(OH in the described step 2)
3Hydroxide aqueous solution specifically is prepared from according to following steps: according to volume ratio is that 100:1～3 take by weighing the Al that volumetric molar concentration is 0.25mol/L
2(SO
4)
3The aqueous solution and ammoniacal liquor are at Al
2(SO
4)
3Aqueous solution dropping ammonia chemical coprecipitation prepares Al(OH)
3Nanometer oxyhydroxide is with Al(OH)
3Nanometer oxyhydroxide is water-soluble, and to obtain mass concentration be 15% Al(OH)
3Hydroxide aqueous solution.
4. preparation ramie form Al according to claim 1
2O
3The method of pottery/Al based composites is characterized in that, aerobic sintering and annealing in the described step 3 are specifically implemented according to following steps: the ramie that step 2 is obtained/Al(OH)
3Precursor is put into atmosphere furnace, and set temperature is 800～1200 ℃, and heat preservation sintering 0.5～2h is again through 100～250 ℃ of annealing 2～4h.
5. preparation ramie form Al according to claim 1
2O
3The method of pottery/Al based composites is characterized in that, in the described step 4, the temperature that arranges in the vacuum pressure infiltration device is 750～800 ℃, and pressure is 4～5MPa.
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|---|---|---|---|
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|---|---|---|---|
| CN2011101257692A CN102212764A (en) | 2011-05-16 | 2011-05-16 | Method for preparing ramie-structured Al2O3 ceramic/Al-based composite material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106555140A (en) * | 2016-11-10 | 2017-04-05 | 哈尔滨工业大学 | A kind of method that use vacuum pressure infiltration method prepares network structure aluminum matrix composite |
| CN106676433A (en) * | 2017-03-01 | 2017-05-17 | 大连大学 | Low-pressure infiltration preparation method of Al2O3 ceramic fiber/particle reinforced metal-matrix composite |
| CN110642607A (en) * | 2019-10-17 | 2020-01-03 | 西安工程大学 | Method for preparing alumina porous ceramic by utilizing biological template method |
| CN112273116A (en) * | 2020-10-19 | 2021-01-29 | 西安工程大学 | Preparation method of morph-genetic structure carbon-modified sunshade net film material |
| CN112300428A (en) * | 2020-10-19 | 2021-02-02 | 西安工程大学 | Preparation method of agricultural film material modified by morph-genetic aluminum oxide |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106555140A (en) * | 2016-11-10 | 2017-04-05 | 哈尔滨工业大学 | A kind of method that use vacuum pressure infiltration method prepares network structure aluminum matrix composite |
| CN106555140B (en) * | 2016-11-10 | 2018-05-04 | 哈尔滨工业大学 | A kind of method that net structure aluminum matrix composite is prepared with vacuum pressure infiltration method |
| CN106676433A (en) * | 2017-03-01 | 2017-05-17 | 大连大学 | Low-pressure infiltration preparation method of Al2O3 ceramic fiber/particle reinforced metal-matrix composite |
| CN110642607A (en) * | 2019-10-17 | 2020-01-03 | 西安工程大学 | Method for preparing alumina porous ceramic by utilizing biological template method |
| CN112273116A (en) * | 2020-10-19 | 2021-01-29 | 西安工程大学 | Preparation method of morph-genetic structure carbon-modified sunshade net film material |
| CN112300428A (en) * | 2020-10-19 | 2021-02-02 | 西安工程大学 | Preparation method of agricultural film material modified by morph-genetic aluminum oxide |
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Application publication date: 20111012 |