CN102212763A - Method for preparing ramie-form SiC ceramic/Al-based composite material - Google Patents
Method for preparing ramie-form SiC ceramic/Al-based composite material Download PDFInfo
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- CN102212763A CN102212763A CN 201110125768 CN201110125768A CN102212763A CN 102212763 A CN102212763 A CN 102212763A CN 201110125768 CN201110125768 CN 201110125768 CN 201110125768 A CN201110125768 A CN 201110125768A CN 102212763 A CN102212763 A CN 102212763A
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- ramie
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Abstract
The invention discloses a method for preparing a ramie-form SiC ceramic/Al-based composite material, comprising the following steps of: firstly, pre-treating ramie fibers; then performing vacuum and pressure impregnation of SiO2 sol on the pre-treated ramie fibers so as to obtain a ramie/SiO2 precursor; then performing anoxic and aerobic compound calcination on the ramie/SiO2 precursor so as to obtain ramie-form porous SiC ceramic precast body; and finally, performing vacuum and pressure impregnation on the ramie-form porous SiC ceramic precast body so as to obtain the ramie-form SiC ceramic/Al-based composite material. The ramie-form SiC ceramic/Al-based composite material prepared with the method in the invention has the advantages of light weight, shock absorbability, sound absorbability and good antifriction wear resistance and can be used for reducing thermal expansion coefficient and density, thereby having a wider application prospect.
Description
Technical field
The invention belongs to the Composite Preparation technical field, relate to a kind of preparation method of ecological ceramic/metal-base composites, be specifically related to a kind of method for preparing ramie form SiC pottery/Al based composites.
Background technology
At present, the technology of known ecological ceramic/metal-base composites has: 1. article " progress of network interpenetrating structural composite material " (functional materials [J], 2002,33(1): 22～25); 2. the article research theory and the progress of material " lose attitude " (material Leader [J], 2006,10:5～7); Article " preparation and the performance analysis of high damping wood ceramics/MB15 matrix material " (matrix material journal [J], 2003,20(1): 8～11); 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 SiC pottery/Al based composites.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing ramie form SiC pottery/Al based composites, solved the mechanical strength and the relatively poor problem of wear resistance of existing biomorph C ceramic/metal composite materials.
The technical solution adopted in the present invention is, a kind of method for preparing ramie form SiC pottery/Al based composites is specifically implemented according to following steps:
Step 1: ramee is carried out pre-treatment;
Step 2: the ramee after the pre-treatment that step 1 is obtained carries out vacuum-pressure impregnation SiO
2Colloidal sol obtains ramie/SiO
2Precursor;
Step 3: ramie/SiO that step 2 is obtained
2Precursor carries out the compound calcining of anoxybiotic-aerobic, obtains ramie form porous SiC ceramics preparative body;
Step 4: the ramie form porous SiC ceramics preparative body that step 3 is obtained carries out vacuum pressure infiltration, obtains ramie form SiC pottery of the present invention/Al based composites.
Characteristics of the present invention also are,
The wherein pre-treatment in the step 1, specifically implement: comprise washing, beat fibre, come unstuck and alkaline purification according to following steps, come unstuck to adopt and come unstuck fully or not exclusively come unstuck, 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.
Wherein vacuum-the pressure impregnation in the step 2 is specifically implemented according to following steps: at first, be that 1:1:4 takes by weighing tetraethoxy, ethanol and H according to mol ratio
2O mixes to obtain mixing solutions, and the ramee after the pre-treatment that step 1 is obtained immerses in this mixing solutions, and regulating pH value is 4～5, is positioned over 24h under the room temperature, and regulating pH value again under 60 ℃ of water-bath environment is 8～9, and dipping is treated SiO
2Colloidal sol is reunited and is transformed into gel, and dry 24h under 60 ℃ beats the SiO that presoma shakes off to fall to stick to the ramee surface then
2Gel takes out drying, and repeatable operation makes SiO
2Reach 3:6～7 with the weight ratio of ramee, obtain ramie/SiO
2Presoma.
The wherein compound calcining of the anoxybiotic-aerobic in the step 3 is specifically implemented according to following steps: ramie/SiO that step 2 is obtained
2Presoma is put into vacuum oven or nitrogen protection tube furnace; in temperature is under 1400～1500 ℃ of conditions; insulation reaction obtained the SiC/C matrix material in 1～2 hour, again the SiC/C matrix material was obtained ramie form porous SiC ceramics preparative body at 600～800 ℃ of aerobic calcining 1～2h.
The vacuum pressure infiltration in the step 4 wherein, specifically implement according to following steps: it is 750～800 ℃ that temperature is set, pressure is 4～5MPa, and aluminium alloy is infiltrated the ramie form porous SiC ceramics preparative body that step 3 obtains, and the volume ratio of aluminium alloy and porous SiC ceramics preparative body is 5: 4.
The invention has the beneficial effects as follows,
1, realize chemical ingredients and regulating microstructure by the ramee pre-treatment, ramee is respectively raw ramie, alkaline purification fiber crops and the degummed ramie of ramee after pre-treatment.
2, utilize the impregnation technology prioritization scheme to improve colloidal sol-ramie dipping homogeneity, improve the sol impregnation rate.
3, obtain a kind of ramie form porous SiC ceramics preparative body through the compound calcining process of anoxybiotic-aerobic.
4, obtain ramie form SiC pottery/Al based composites through the vacuum pressure infiltration aluminium alloy.
The present invention is based on ramee and lose the attitude structure, a kind of preparation method that ramee is lost the SiC pottery/Al based composites of attitude structure that has is provided.Ramie form SiC pottery/Al based composites that the inventive method prepares has light weight, the characteristics that weakening, sound-absorbing and anti-friction wear-resistant are good, and can reduce thermal expansivity and density, have more wide application prospect.
Embodiment
The present invention is described in detail below in conjunction with embodiment.
The present invention prepares the method for ramie form SiC pottery/Al based composites, specifically implements 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 ramee after the pre-treatment that step 1 is obtained carries out vacuum-pressure impregnation SiO
2Colloidal sol obtains ramie/SiO
2Precursor.At first, be that 1:1:4 takes by weighing tetraethoxy (TEOS), ethanol (C according to mol ratio
2H
5OH) and H
2O mixes to obtain mixing solutions, and the ramee after the pre-treatment that step 1 is obtained immerses in this mixing solutions, regulating pH value is 4～5, is positioned over 24h under the room temperature, and regulating pH value again under 60 ℃ of water-bath environment is 8～9, and adopt multiple impregnation method repeatedly to flood, treat SiO
2Colloidal sol is reunited and is transformed into gel, and dry 24h under 60 ℃ beats the SiO that presoma shakes off to fall to stick to the ramee surface then
2Gel takes out dry.Through repeatable operation, make SiO
2Reach 3:6～7 with the weight ratio of ramee, obtain ramie/SiO
2Presoma.
Step 3: ramie/SiO that step 2 is obtained
2Precursor carries out the compound calcining of anoxybiotic-aerobic and obtains ramie form SiC ceramics preparative body.Ramie/SiO that step 2 is obtained
2Presoma is put into vacuum or nitrogen protection tube furnace, and the sintering preparation in 1～2 hour of 1400～1500 ℃ of insulation reaction has the SiC/C matrix material that ramee is lost the attitude structure.Again the SiC/C matrix material is obtained ramie form porous SiC ceramics preparative body at 600～800 ℃ of aerobic calcining 1～2h.
Step 4: the ramie form porous SiC ceramics preparative body that step 3 is obtained carries out vacuum pressure infiltration and prepares ramie form SiC pottery/Al based composites.In the vacuum pressure infiltration device, 750～800 ℃, under 4～5MPa pressure aluminium alloy is infiltrated ramie form porous SiC ceramics preparative body, the volume ratio of aluminium alloy and porous SiC ceramics preparative body is 5: 4, obtains ramie form SiC pottery of the present invention/Al based composites.
Embodiment 1
It is long that the ramie raw ramie is trimmed to 5～10mm, and the back is immersed and utilized tetraethoxy (TEOS), ethanol (C in advance
2H
5OH) and H
2O is about in the solution of 1:1:4 proportioning in molar ratio, and to regulate pH value be 4～5, is positioned over 24h under the room temperature, and to regulate pH value again under 60 ℃ of water-bath environment be 8～9 and be aided with ultrasonic vibration dipping 2h, treats SiO
2Colloidal sol is reunited and is transformed into gel, obtains ramie/SiO behind the dry 24h down at 60 ℃
2Presoma beats the SiO that presoma shakes off to fall to stick to the ramee surface then
2Gel takes out dry.Repeatable operation makes SiO
2Reaching weight ratio with the ramie raw ramie is 3:7; With the ramie raw ramie/SiO behind the impregnation drying
2Presoma is put into vacuum or nitrogen protection tube furnace, and 1400 ℃ of insulation reaction 2h sintering preparations have the SiC/C matrix material that ramee is lost the attitude structure; 2h obtains ramie form porous SiC with 600 ℃ of aerobic calcinings of SiC/C matrix material; In the vacuum pressure infiltration device, 750 ℃, under the 5MPa pressure aluminium alloy is infiltrated ramie form porous SiC, the volume ratio of aluminium alloy and porous SiC ceramics preparative body is 5: 4, obtains ramie form SiC pottery/Al based composites.
Embodiment 2
It is long that ramie alkaline purification fiber crops are trimmed to 5～10mm, and the back is immersed and utilized tetraethoxy (TEOS), ethanol (C in advance
2H
5OH) and H
2O is about in the solution of 1:1:4 proportioning in molar ratio, and to regulate pH value be 4～5, is positioned over 24h under the room temperature, regulates pH value again and be 8～9 and adopt vacuum-pressure impregnation 2h under 60 ℃ of water-bath environment, treats SiO
2Colloidal sol is reunited and is transformed into gel, obtains ramie/SiO behind the dry 24h down at 60 ℃
2Presoma beats the SiO that presoma shakes off to fall to stick to the ramee surface then
2Gel takes out dry.Repeatable operation makes SiO
2Reach weight ratio with the alkaline purification fiber crops and (be 3:6; With the alkaline purification fiber crops/SiO behind the impregnation drying
2Presoma is put into vacuum or nitrogen protection tube furnace, and 1450 ℃ of insulation reaction 1h sintering preparations have the SiC/C matrix material that ramee is lost the attitude structure.1h obtains ramie form porous SiC with 700 ℃ of aerobic calcinings of SiC/C matrix material; In the vacuum pressure infiltration device, 750 ℃, under the 4MPa pressure aluminium alloy is infiltrated ramie form porous SiC, the volume ratio of aluminium alloy and porous SiC ceramics preparative body is 5: 4, obtains ramie form SiC pottery/Al based composites.
Embodiment 3
It is long that the ramie degummed ramie is trimmed to 5～10mm, and the back is immersed and utilized tetraethoxy (TEOS), ethanol (C in advance
2H
5OH) and H
2O is about in the solution of 1:1:4 proportioning in molar ratio, and to regulate pH value be 4～5, is positioned over 24h under the room temperature, regulates pH value again and be 8～9 and adopt vacuum-pressure impregnation 2h under 60 ℃ of water-bath environment, treats SiO
2Colloidal sol is reunited and is transformed into gel, obtains ramie/SiO behind the dry 24h down at 60 ℃
2Presoma beats the SiO that presoma shakes off to fall to stick to the ramee surface then
2Gel takes out dry.Repeatable operation makes SiO
2Reaching weight ratio with degummed ramie is 3:7; With the degummed ramie/SiO behind the impregnation drying
2Presoma is put into vacuum or nitrogen protection tube furnace, and 1500 ℃ of insulation reaction 1h sintering preparations have the SiC/C matrix material that ramee is lost the attitude structure.1h obtains ramie form porous SiC with 700 ℃ of aerobic calcinings of SiC/C matrix material; In the vacuum pressure infiltration device, 800 ℃, under the 4MPa pressure aluminium alloy is infiltrated ramie form porous SiC, the volume ratio of aluminium alloy and porous SiC ceramics preparative body is 5: 4, obtains ramie form SiC pottery/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, and middle hole obviously increases, fibre wall thickness increases, and is conducive to SiO2The infiltration of solution.
2. rational SiO2Technological parameter in the preparation of solution and the vacuum-pressure dipping is conducive to obtain uniform SiO2Solution improves infiltration uniformity and infiltration rate, is conducive to get rid of residual gas in the ramee by vacuum-pressure infiltration mode, guarantees SiO2Solution immerses in the ramee micropore.
3. reasonably aerobic sintering and annealing process can obtain ramie form porous SiC precast body, can eliminate the calcining defective by annealing.
4. reasonably the favourable formation infiltration liquid of the technological parameter of vacuum pressure infiltration flows, and makes molten aluminium alloy be impregnated into ramie form porous SiC precast body under pressure-suction effect.
The ramie form SiC pottery of the present invention's preparation/Al based composites is compared with existing composite, and this novel ceramic/metal composite materials can suppress plastic deformation and hot mastication and the serious three-body-abrasion of matrix alloy. With object to when mill the conduction of heat of self-lubricating function and the matrix alloy of remaining carbon-coating because ecological ceramic comes off, its coefficient of friction and wear rate are lower and stable than alloy material, so that the abrasion resistance of composite improves. Because the three-dimensional net structure of ceramic enhancement phase uniqueness is conducive to and will concentrates on a little or stress on the face disperses rapidly and transmits, can significantly improve the composite impact resistance in spatial dimension. 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. a method for preparing ramie form SiC pottery/Al based composites is characterized in that, specifically implements according to following steps:
Step 1: ramee is carried out pre-treatment;
Step 2: the ramee after the pre-treatment that step 1 is obtained carries out vacuum-pressure impregnation SiO
2Colloidal sol obtains ramie/SiO
2Precursor;
Step 3: ramie/SiO that step 2 is obtained
2Precursor carries out the compound calcining of anoxybiotic-aerobic, obtains ramie form porous SiC ceramics preparative body;
Step 4: the ramie form porous SiC ceramics preparative body that step 3 is obtained carries out vacuum pressure infiltration, obtains ramie form SiC pottery of the present invention/Al based composites.
2. the method for preparing ramie form SiC pottery/Al based composites according to claim 1, it is characterized in that, pre-treatment in the described step 1, specifically implement: comprise washing, beat fibre, come unstuck and alkaline purification according to following steps, come unstuck to adopt and come unstuck fully or not exclusively come unstuck, alkaline purification is that ramee is soaked 10h～30h in mass concentration is 5%～25% the NaOH aqueous solution, is washed with water to neutrality again, 60～105 ℃ of drying 2～4h.
3. the method for preparing ramie form SiC pottery/Al based composites according to claim 1, it is characterized in that, vacuum-pressure impregnation in the described step 2 is specifically implemented according to following steps: at first, be that 1:1:4 takes by weighing tetraethoxy, ethanol and H according to mol ratio
2O mixes to obtain mixing solutions, and the ramee after the pre-treatment that step 1 is obtained immerses in this mixing solutions, and regulating pH value is 4～5, is positioned over 24h under the room temperature, and regulating pH value again under 60 ℃ of water-bath environment is 8～9, and dipping is treated SiO
2Colloidal sol is reunited and is transformed into gel, and dry 24h under 60 ℃ beats the SiO that presoma shakes off to fall to stick to the ramee surface then
2Gel takes out drying, and repeatable operation makes SiO
2Reach 3:6～7 with the weight ratio of ramee, obtain ramie/SiO
2Presoma.
4. the method for preparing ramie form SiC pottery/Al based composites according to claim 1 is characterized in that the compound calcining of the anoxybiotic-aerobic in the described step 3 is specifically implemented according to following steps: ramie/SiO that step 2 is obtained
2Presoma is put into vacuum oven or nitrogen protection tube furnace; in temperature is under 1400～1500 ℃ of conditions; insulation reaction obtained the SiC/C matrix material in 1～2 hour, again the SiC/C matrix material was obtained ramie form porous SiC ceramics preparative body at 600～800 ℃ of aerobic calcining 1～2h.
5. the method for preparing ramie form SiC pottery/Al based composites according to claim 1, it is characterized in that, vacuum pressure infiltration in the described step 4, specifically implement according to following steps: it is 750～800 ℃ that temperature is set, pressure is 4～5MPa, aluminium alloy is infiltrated the ramie form porous SiC ceramics preparative body that step 3 obtains, and the volume ratio of aluminium alloy and porous SiC ceramics preparative body is 5: 4.
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Cited By (2)
| 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 |
| CN110368921A (en) * | 2019-07-29 | 2019-10-25 | 姚光纯 | Catalyst carrier and preparation method thereof with three-dimensional netted inertia skeleton structure |
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| CN1403527A (en) * | 2002-10-17 | 2003-03-19 | 上海交通大学 | Prepn of composite friction material |
| CN101381098A (en) * | 2008-10-09 | 2009-03-11 | 西安工程大学 | Linen fiber morph-genetic structure tin oxide or aluminium oxide compound material |
| CN101660225A (en) * | 2009-09-21 | 2010-03-03 | 国际竹藤网络中心 | SiC fiber and fabric and preparation method thereof |
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2011
- 2011-05-16 CN CN 201110125768 patent/CN102212763A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1403527A (en) * | 2002-10-17 | 2003-03-19 | 上海交通大学 | Prepn of composite friction material |
| CN101381098A (en) * | 2008-10-09 | 2009-03-11 | 西安工程大学 | Linen fiber morph-genetic structure tin oxide or aluminium oxide compound material |
| CN101660225A (en) * | 2009-09-21 | 2010-03-03 | 国际竹藤网络中心 | SiC fiber and fabric and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 《兵器材料科学与工程》 20110331 贺辛亥等 SiC/C遗态陶瓷的制备工艺研究 第1-4页 第34卷, 第2期 * |
| 《材料热处理技术》 20101231 赵文侠等 气压浸渗法制备Al2O3(sf)/Al复合材料的缺陷分析 第124-127页 第1-5 第39卷, 第24期 * |
Cited By (4)
| 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 |
| CN110368921A (en) * | 2019-07-29 | 2019-10-25 | 姚光纯 | Catalyst carrier and preparation method thereof with three-dimensional netted inertia skeleton structure |
| CN110368921B (en) * | 2019-07-29 | 2022-03-22 | 姚光纯 | Catalyst carrier with three-dimensional reticular inert framework structure and preparation method thereof |
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Application publication date: 20111012 |