CN102501548A - High-toughness anti-impact ceramic-based layered composite material and preparation method thereof - Google Patents

High-toughness anti-impact ceramic-based layered composite material and preparation method thereof Download PDF

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Publication number
CN102501548A
CN102501548A CN2011103265570A CN201110326557A CN102501548A CN 102501548 A CN102501548 A CN 102501548A CN 2011103265570 A CN2011103265570 A CN 2011103265570A CN 201110326557 A CN201110326557 A CN 201110326557A CN 102501548 A CN102501548 A CN 102501548A
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preparation
ceramic
potsherd
plasticity
adhesive resin
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饶平根
李伟信
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South China University of Technology SCUT
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South China University of Technology SCUT
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Abstract

The invention discloses a high-toughness anti-impact ceramic-based layered composite material and a preparation method thereof. The method comprises the following steps of: cutting a ceramic piece and a material serving as plastic interlayer into blocks, and washing with ultrasonic wave for use; mixing the adhesive resin and a curing agent to obtain the bonding strength of 15-30 MPa, and de-foaming for 20-30 minutes in vacuum condition; coating the mixture on the surface of the processed ceramic piece, and placing the plastic interlayer; and placing the ceramic piece coated with the mixture on the surface of the plastic interlayer, and superposing in this way to obtain a layered structure; and maintaining pressure of 5-10 MPa of the layered structure for 1-24 hours to obtain the high-toughness anti-impact ceramic-based layered composite material. According the invention, the strength of the prepared ceramic-based layered composite material is closed to that of the ceramic matrix, and the material has the characteristics of high fracture toughness and high impact toughness as well as excellent impact resistance.

Description

A kind of high-tenacity and shock-resistance ceramic base laminar composite and preparation method thereof
Technical field
The present invention relates to high performance structure ceramic material and composite, field, specifically be meant a kind of high-tenacity and shock-resistance ceramic base laminar composite and preparation method thereof.
Background technology
The ceramic base laminar composite comes across the beginning of the nineties in last century, and it serves as that the fragility deadly defect that solves ceramic material provides a new solution route with its particular structure characteristics with to the characteristic property of crackle " blunt ".At present; The research of ceramic base laminar composite mainly concentrates in the research to the design of layer structure and preparation technology; Having occurred is three kinds of laminated ceramic composites of tack coat with metal material, Inorganic Non-metallic Materials and organic material respectively, and its fracture toughness and energy to failure have obtained very big improvement.But the layer structure that exists at present and preparation technology's ubiquity that structure is single, complicated process of preparation, require characteristics such as equipment is high-end, are difficult to the batch process of realization product.
Summary of the invention
The objective of the invention is shortcoming, a kind of high-tenacity and shock-resistance ceramic base laminar composite and preparation method thereof is provided to prior art.
The present invention utilizes the skeleton of potsherd for composite; Structure through the appropriate design laminar composite; The high-strength height of giving full play to ceramic material is hard, the ductility of metal material and the characteristics such as plasticity, caking property of prolonging of resin material; Disperse and multistage energy consumption through stress, thereby significantly improve energy to failure, the fracture toughness of ceramic base laminar composite, prepare the high-performance and low-cost laminated ceramic composite.
The object of the invention realizes through following technical scheme:
A kind of preparation method of high-tenacity and shock-resistance ceramic base laminar composite comprises the steps:
(1) become block to potsherd with material cut as the plasticity interlayer, ultrasonic waves for cleaning is totally subsequent use;
(2) adhesive resin and curing agent are mixed, and reach the adhesion strength of 15 ~ 30MPa, deaeration is subsequent use after 20 ~ 30 minutes under vacuum;
(3) mixture with step (2) is coated in the potsherd surface of handling through step (1), places the plasticity interlayer then, places the potsherd that is coated with said mixture again at the plasticity sandwiching surface, and so overlapping putting obtains layer structure;
(4) with above-mentioned layer structure, pressurize is 1 ~ 24 hour under 5 ~ 10MPa pressure, can obtain required high-tenacity and shock-resistance ceramic base laminar composite.
Said potsherd is alumina wafer, Zirconia reinforced alumina (ZTA) sheet, silicon carbide plate, nitrogenize silicon chip or boron carbide sheet.
Said plasticity interlayer is woven wire, sheet metal, macromolecule silk screen or polymer sheets.
Said metal is iron, steel or aluminium, and said macromolecule is polyurethane, nylon.
Said adhesive resin is epoxy resin or polyurethane.
When adopting the epoxy resin as adhesive resin, the dwell time is 1 ~ 2 hour in the said step (4); When adopting polyurethane to make adhesive resin, the dwell time is 5 ~ 8 hours in the said step (4).
Another object of the present invention is to provide a kind of high-tenacity and shock-resistance ceramic base laminar composite that is formed by method for preparing.
The present invention has following advantage and effect:
(1) adopt the matrix of the ceramic sheet of sintering as the ceramic base laminar composite, alternative ceramic sheet kind and multi-size can satisfy the use under the different application condition.
(2) sintering process that has combined to have replaced generally to adopt now with adhesive combines, not only technology is simple, accomplishes scale production easily, and has overcome the shortcoming that ceramic layer and binder course in the sintering are difficult to reach at same temperature spot optimal performance.The technology of unburned knot also has great importance aspect energy-saving and environmental protection.
(3) can control the adhesion strength of plasticity interlayer and ceramic layer through the composition of change adhesive and the content of curing agent etc., thereby change the performance of ceramic base laminar composite, satisfy different application.
(4) the ceramic base laminar composite of preparation has high tenacity and high energy to failure, can satisfy the use under the high speed impact environment.
The specific embodiment
Below in conjunction with specific embodiment the present invention is done further concrete detailed description the in detail, but embodiment of the present invention is not limited thereto, the technological parameter for not indicating especially can carry out with reference to routine techniques.
Embodiment 1
The first step: use alumina wafer to be ceramic skeleton, cut into 70mm * 60mm * 0.6mm, with 30 KHZ frequency ultrasonic cleaning 25 minutes; As the plasticity interlayer, be cut into 70mm * 60mm * 0.6mm with wire netting, it is back with 30 KHZ frequency ultrasonic cleaning 10 minutes that it is eliminated rust.
Second step: utilizing the agent of epoxy resin gluing as binding agent, is that 1:1 mixes epoxy resin and curing agent according to weight ratio, and deaeration is 20 minutes in vacuum drying chamber, sloughs bubble.
The 3rd step: on the alumina wafer of second adhesive coated gained in the first step of being prepared of step, place wire netting then, place alumina wafer behind the coated with adhesive again, the repetition said process is till stacking 7 layers of potsherd.
The 4th step: the layer structure of the 3rd step gained is placed in the special mould, is placed on mould under the forcing press then and exerts pressure, design of pressure is 6MPa; Dwell time is 24 hours; Remove pressure then, 3 as a child removed mould, obtained laminated ceramic composite after 48 hours;
The 5th step: the laminated ceramic composite sample to preparation carries out test analysis.Adopt drainage to measure the bulk density of sample; Adopt the three-point bending resistance method to measure the fracture strength of sample; With SENB method (SEBN) test fracture toughness, calculate energy to failure with the fracture strength test curve.
The alumina ceramic plate intensity that present embodiment uses is 300MPa, and fracture toughness is 3 MPam 1/2, the plasticity interlayer is commercial 200 order wire nettings, epoxy adhesive is bought on the market; Laminated ceramic composite sample density through method for preparing is 3.57g/cm 3, bending strength is 305MPa, fracture toughness is 15.6MPam 1/2, energy to failure is 2800J/m 2
Embodiment 2
The first step: use the ZTA sheet to be ceramic skeleton, cut into 70mm * 60mm * 0.6mm, with 30 KHZ frequency ultrasonic cleaning 25 minutes; As the plasticity interlayer, be cut into 70mm * 60mm * 0.6mm with nylon wire, it is back with 30 KHZ frequency ultrasonic cleaning 10 minutes that it is eliminated rust.
Second step: utilizing the agent of epoxy resin gluing as binding agent, is that 1:0.8 mixes epoxy resin and curing agent according to weight ratio, in vacuum drying chamber, carries out deaeration 30 minutes, sloughs bubble.
The 3rd step: on the ZTA sheet of second adhesive coated gained in the first step of being prepared of step, place nylon wire then, place the ZTA sheet behind the coated with adhesive again, the repetition said process is till stacking 7 layers of potsherd.
The 4th step: the layer structure of the 3rd step gained is placed in the special mould, is placed on mould under the forcing press then and exerts pressure, design of pressure is 7MPa; Dwell time is 1 hour; Remove pressure then, 3 as a child removed mould, obtained laminated ceramic composite after 48 hours;
The 5th step: the laminated ceramic composite sample to preparation carries out test analysis.Adopt drainage to measure the bulk density of sample; Adopt the three-point bending resistance method to measure the fracture strength of sample; With SENB method (SEBN) test fracture toughness, calculate energy to failure with the fracture strength test curve.
The ZTA sheet intensity that present embodiment uses is 650MPa, and fracture toughness is 10 MPam 1/2, nylon mesh is commercial 120 order silk screens, epoxy adhesive is bought on the market; Laminated ceramic composite sample density through method for preparing is 3.7g/cm 3, bending strength is 600MPa, fracture toughness is 17 MPam 1/2, energy to failure is 7000J/m 2
Embodiment 3
The first step: use silicon carbide plate to be ceramic skeleton, cut into 70mm * 60mm * 0.6mm, with 30 KHZ frequency ultrasonic cleaning 25 minutes; As the plasticity interlayer, be cut into 70mm * 60mm * 0.6mm with aluminum slice, in order to increase roughness, aluminum slice is through the polishing of 180# emery paper, with 30 KHZ frequency ultrasonic cleaning 10 minutes;
Second step: utilizing the agent of epoxy resin gluing as binding agent, is that 1:0.8 mixes epoxy resin and curing agent according to weight ratio, in vacuum drying chamber, carries out deaeration 27 minutes, sloughs bubble;
The 3rd step: on the silicon carbide plate described in the first step, place the metallic aluminium thin slice to second adhesive coated prepared of step then, place potsherd behind the coated with adhesive again, the repetition said process is till stacking 7 layers of silicon carbide plate;
The 4th step: the layer structure of the 3rd step gained is placed in the special mould, is placed on mould under the forcing press then and exerts pressure, design of pressure is 5MPa; Dwell time is 2 hours; Remove pressure then, 3 as a child removed mould, obtained laminated ceramic composite after 48 hours;
The 5th step: the laminated ceramic composite sample to preparation carries out test analysis.Adopt drainage to measure the bulk density of sample; Adopt the three-point bending resistance method to measure the fracture strength of sample; With SENB method (SEBN) test fracture toughness, calculate energy to failure with the fracture strength test curve.
The silicon carbide plate intensity that present embodiment uses is 480MPa, and fracture toughness is 3 MPam 1/2, the plasticity interlayer is the metallic aluminium thin slice, and thickness is 0.1mm, and epoxy adhesive is bought on the market; Laminated ceramic composite sample density through method for preparing is 3. 1g/cm 3, bending strength is 450MPa, fracture toughness is 12.0MPam 1/2, energy to failure is 2850J/m 2
Embodiment 4
The first step: use the nitrogenize silicon chip to be ceramic skeleton, cut into 70mm * 60mm * 0.6mm, with 30 KHZ frequency ultrasonic cleaning 25 minutes; As the plasticity interlayer, be cut into 70mm * 60mm * 0.6mm with sheet of polyurethane respectively, with 30 KHZ frequency ultrasonic cleaning 10 minutes;
Second step: utilizing adhesive for polyurethane as binding agent, is that 1:0.6 mixes epoxy resin and curing agent according to weight ratio, in vacuum drying chamber, carries out deaeration 20 minutes;
The 3rd step: on the nitrogenize silicon chip of second adhesive coated gained in the first step of being prepared of step, place one deck sheet of polyurethane then, place potsherd behind the coated with adhesive again, the repetition said process is till stacking 7 layers of potsherd;
The 4th step: the layer structure of the 3rd step gained is placed in the special mould, is placed on mould under the forcing press then and exerts pressure, design of pressure is 10MPa; Dwell time is 5 hours; Remove pressure then, 3 as a child removed mould, obtained laminated ceramic composite after 48 hours;
The 5th step: the laminated ceramic composite sample to preparation carries out test analysis.Adopt drainage to measure the bulk density of sample; Adopt the three-point bending resistance method to measure the fracture strength of sample; With SENB method (SEBN) test fracture toughness, calculate energy to failure with the fracture strength test curve.
The nitrogenize silicon chip intensity that present embodiment uses is 800MPa, and fracture toughness is 8 MPam 1/2, buy on sheet of polyurethane and the polyurethane resin binding agent market; Laminated ceramic composite sample density through method for preparing is 2.9 g/cm 3, bending strength is 700MPa, fracture toughness is 18.0MPam 1/2, energy to failure is 8500J/m 2
Embodiment 5
The first step: use the boron carbide sheet to be ceramic skeleton, cut into 70mm * 60mm * 0.6mm, with 30 KHZ frequency ultrasonic cleaning 25 minutes; Use stainless steel cloth to be the plasticity interlayer, be cut into 70mm * 60mm * 0.6mm, with 30 KHZ frequency ultrasonic cleaning 10 minutes.
Second step: utilizing adhesive for polyurethane as binding agent, is that 1:1.0 mixes polyurethane resin and curing agent according to weight ratio, in vacuum drying chamber, carries out deaeration 25 minutes.
The 3rd step: on the boron carbide sheet of second adhesive coated gained in the first step of being prepared of step, place one deck plasticity stainless steel cloth preferably then, place the boron carbide sheet behind the coated with adhesive again, the repetition said process is till stacking 7 layers of boron carbide sheet.
The 4th step: the layer structure of the 3rd step gained is placed in the special mould, is placed on mould under the forcing press then and exerts pressure, design of pressure is 10MPa; Dwell time is 8 hours; Remove pressure then, 8 as a child removed mould, obtained laminated ceramic composite after 48 hours;
The 5th step: the laminated ceramic composite sample to preparation carries out test analysis.Adopt drainage to measure the bulk density of sample; Adopt the three-point bending resistance method to measure the fracture strength of sample; With SENB method (SEBN) test fracture toughness, calculate energy to failure with the fracture strength test curve.
The boron carbide sheet intensity that present embodiment uses is 400MPa, and fracture toughness is 3.2 MPam 1/2, stainless steel cloth is commercial 200 order silk screens, polyurethane adhesive is bought on the market; Laminated ceramic composite sample density through method for preparing is 2.6g/cm 3, bending strength is 380MPa, fracture toughness is 14.5MPam 1/2, energy to failure is 3200J/m 2
The foregoing description is a preferred implementation of the present invention; But embodiment of the present invention is not restricted to the described embodiments; Other any do not deviate from change, the modification done under spirit of the present invention and the principle, substitutes, combination, simplify; All should be the substitute mode of equivalence, be included within protection scope of the present invention.

Claims (7)

1. the preparation method of a high-tenacity and shock-resistance ceramic base laminar composite is characterized in that, comprises the steps:
(1) become block to potsherd with material cut as the plasticity interlayer, ultrasonic waves for cleaning is totally subsequent use;
(2) adhesive resin and curing agent are mixed, and reach the adhesion strength of 15 ~ 30MPa, deaeration is subsequent use after 20 ~ 30 minutes under vacuum;
(3) mixture with step (2) is coated in the potsherd surface of handling through step (1), places the plasticity interlayer then, places the potsherd that is coated with said mixture again at the plasticity sandwiching surface, and so overlapping putting obtains layer structure;
(4) with above-mentioned layer structure, pressurize is 1 ~ 24 hour under 5 ~ 10MPa pressure, can obtain required high-tenacity and shock-resistance ceramic base laminar composite.
2. preparation method according to claim 1 is characterized in that, said potsherd is alumina wafer, Zirconia reinforced alumina sheet, silicon carbide plate, nitrogenize silicon chip or boron carbide sheet.
3. preparation method according to claim 1 and 2 is characterized in that, said plasticity interlayer is woven wire, sheet metal, macromolecule silk screen or polymer sheets.
4. according to claim 3, it is characterized in that said metal is iron, steel or aluminium, said macromolecule is polyurethane, nylon.
5. preparation method according to claim 4 is characterized in that, said adhesive resin is epoxy resin or polyurethane.
6. preparation method according to claim 5 is characterized in that, when adopting the epoxy resin as adhesive resin, the dwell time is 1 ~ 2 hour in the said step (4); When adopting polyurethane to make adhesive resin, the dwell time is 5 ~ 8 hours in the said step (4).
7. a high-tenacity and shock-resistance ceramic base laminar composite is characterized in that, is prepared from any method of said claim 1 to 6.
CN2011103265570A 2011-10-25 2011-10-25 High-toughness anti-impact ceramic-based layered composite material and preparation method thereof Pending CN102501548A (en)

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Cited By (7)

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Publication number Priority date Publication date Assignee Title
CN103382099A (en) * 2013-07-12 2013-11-06 河海大学 Sandwich structure bulletproof ceramic sheet and low temperature sintering preparation method
CN105459516A (en) * 2014-08-28 2016-04-06 比亚迪股份有限公司 Ceramic substrate and preparation method thereof, and power module
CN105503226A (en) * 2015-12-24 2016-04-20 中南大学 Ultra-thin carbon-based composite panel and preparation method
CN111136999A (en) * 2019-12-24 2020-05-12 南京工程学院 High-toughness shell brick mud structure-imitated ceramic matrix composite material and preparation method thereof
US10710936B2 (en) 2014-08-28 2020-07-14 Byd Company Limited Ceramic substrate and its manufacturing method, power module
CN114807788A (en) * 2022-04-13 2022-07-29 苏州诚亮粉末冶金有限公司 ZTA ceramic net film modified nano powder metallurgy material and preparation method thereof
CN115895387A (en) * 2022-11-18 2023-04-04 浙江安胜科技股份有限公司 Long-service-life ceramic coating, preparation method and rolling wheel

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103382099A (en) * 2013-07-12 2013-11-06 河海大学 Sandwich structure bulletproof ceramic sheet and low temperature sintering preparation method
CN105459516A (en) * 2014-08-28 2016-04-06 比亚迪股份有限公司 Ceramic substrate and preparation method thereof, and power module
CN105459516B (en) * 2014-08-28 2018-05-08 比亚迪股份有限公司 A kind of ceramic substrate and preparation method thereof and a kind of power module
US10710936B2 (en) 2014-08-28 2020-07-14 Byd Company Limited Ceramic substrate and its manufacturing method, power module
CN105503226A (en) * 2015-12-24 2016-04-20 中南大学 Ultra-thin carbon-based composite panel and preparation method
CN111136999A (en) * 2019-12-24 2020-05-12 南京工程学院 High-toughness shell brick mud structure-imitated ceramic matrix composite material and preparation method thereof
CN114807788A (en) * 2022-04-13 2022-07-29 苏州诚亮粉末冶金有限公司 ZTA ceramic net film modified nano powder metallurgy material and preparation method thereof
CN114807788B (en) * 2022-04-13 2023-07-07 苏州诚亮粉末冶金有限公司 ZTA ceramic omentum modified nano powder metallurgy material and preparation method thereof
CN115895387A (en) * 2022-11-18 2023-04-04 浙江安胜科技股份有限公司 Long-service-life ceramic coating, preparation method and rolling wheel

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Application publication date: 20120620