CN107140985A - A kind of high performance ceramic material preparation method based on increasing material manufacturing technique - Google Patents
A kind of high performance ceramic material preparation method based on increasing material manufacturing technique Download PDFInfo
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Abstract
The present invention proposes a kind of high performance ceramic material preparation method based on increasing material manufacturing technique, and the first step, ceramic powders/binding agent binary system rapid prototyping material prepares link；Second step, polyacrylonitrile solution prepares link；3rd step, greenwave is obtained by ceramic powders/binding agent binary system rapid shaping link；4th step, greenwave degreasing and pre-sintered link；5th step, it is pre-sintered after greenwave infiltrate and infiltrates in PAN solution after greenwave in PAN and DMSO Thermal inactive links；Being detained in 6th step, greenwave microvoid has the sintering after PAN and carbonization link.Material of the present invention is that the high-performance ceramic particle of the carbon material filled high-temperature sintering reacted by Cyclization ira situ is constituted, the features such as having ceramics and carbon material two-arch tunnel, the enhancing of stereoeffect interface, micropore in structure.The preparation of three-dimensional carbon structure activeness and quietness increasing material manufacturing ceramic can be achieved, processing method of the invention can improve the intensity and toughness of increasing material manufacturing ceramic.
Description
Technical field
The present invention relates to a kind of high-performance ceramic, more particularly, to a kind of high-performance ceramic increasing material manufacturing method.
Background technology
High-performance ceramic is huge in the domain requirement amount such as Aero-Space, automobile, electronics, national defence.Rapid shaping technique has
Shaping speed is fast, printable complex component, personalization, low cost, short molding cycle the advantages of, for the fast short-term training of ceramic material
Type technology turns into the study hotspot of Material Field in recent years.Ceramic rapid shaping technique is widely used to ceramic contact pin, electricity
The shaping manufacture of sub- ceramic component, ceramic foam filter part, the product that ceramic tooth equidimension is small, complex-shaped, precision is high.But
It is that brittleness of ceramics is difficult with greatly rapid shaping technique machine-shaping, as a key factor for restricting its development and application.
The content of the invention
The present invention proposes a kind of high performance ceramic material preparation method based on increasing material manufacturing technique.The material model is by original
The high-performance ceramic powder of the carbon material filled high-temperature sintering of position cyclization is constituted, and has ceramics and carbon material double in structure
The features such as continuous phase, the enhancing of stereoeffect interface, micropore.When being destroyed by external force, broken by crack deflection, carbon material
Split and the mechanism such as extract and absorb energy and realize the high-strength and high-ductility of material, while the electric conductivity of material can be lifted.It is same with this
When, it is proposed that the preparation technology of performance function ceramic matric composite, realizes the controllable of high-performance ceramic composite
It is standby.
According to the functionalization ceramic material model of space in-situ carburization Material reinforcement toughness reinforcing, the present invention is proposed in ceramic powder
Pre-dispersed carbon materials material precursor polyacrylonitrile (PAN), PAN carbonizations and the preparation principle of ceramic powder sintering integratedization, are carried in end
The processing method based on fusion sediment increasing material manufacturing method is gone out：Infiltrate in-situ carburization technique.
The present invention proposes a kind of high performance ceramic material preparation method based on increasing material manufacturing technique, and preparation process order is such as
Under：The first step, ceramic powders/binding agent binary system rapid prototyping material prepares link；Second step, polyacrylonitrile (PAN) is molten
Liquid prepares link；3rd step, ceramic powders/binding agent binary system rapid shaping link obtains greenwave；4th step, greenwave degreasing
With pre-sintered link；5th step, it is pre-sintered after greenwave infiltrate and infiltrate in PAN solution after greenwave in PAN and DMSO it is hot
Cause phase separation link；Being detained in 6th step, greenwave microvoid has the sintering after PAN and carbonization link.
A kind of high performance ceramic material preparation method based on increasing material manufacturing technique of the present invention, it is first in material prepares link
First carry out ceramic powders/binding agent binary system rapid prototyping material to prepare, based on early-stage Study basis and carbon material and ceramics
Interfacial bonding property consider, the present invention using spherical carborundum (SiC) as ceramic raw material, with polyethylene (PE) or PLA
(PLA) as binding agent；Twin-screw mixer extruder and micro-nano are used with certain ceramic particle size, useful load, binding agent ratio
It is laminated orderly blending equipment and rapid shaping binary system consumptive material is made.
A kind of high performance ceramic material preparation method based on increasing material manufacturing technique of the present invention, polyacrylonitrile (PAN) solution
Prepare concretely comprising the following steps for link：PAN powder and DMSO are weighed respectively by certain mass ratio, and test tube or beaker are loaded after mixing,
Test tube or beaker are vertically fixed in 160 DEG C of oil baths and preheated, magnetic agitation is opened or mechanical agitation (is more than for PAN concentration
25wt% system), at the uniform velocity stir to polymer and all dissolve, obtain the solution of transparent and homogeneous.
A kind of high performance ceramic material preparation method based on increasing material manufacturing technique of the present invention, rapid shaping link it is specific
Step is that screw rod heats blending extrusion feed device carry on three-dimensional motion device, and screw rod melting conveying binary system raw material is simultaneously
Molten state consumptive material is extruded, three-dimensional motion device makes screw extrusion apparatus be moved according to certain track by computer control, diploid
It is that molten state consumptive material deposits cooling and solidifying generation greenwave blank on shaped platform.
A kind of high performance ceramic material preparation method based on increasing material manufacturing technique of the present invention, it is carbonized and pre-sintered link
Specific steps be divided into following three step：
1. degreasing and pre-sintered link
Degreasing route according to the binary system material of design is heated to greenwave, make high polymer cemented dose decompose and with
Gas form is uniformly escaped；Greenwave is continued again temperature being increased to 2130 DEG C (theoretical sintering temperatures of SiC ceramic), insulation one
The section time forms pre-sintered part, it is ensured that sample has certain intensity, forms the ceramic pre-burning with communicate-type microvoid structure
Tie part.
2. PAN solution impregnations and Thermal inactive link
The greenwave crossed with the PAN solution impregnations pre-sintering configured, applies certain pressure to PAN solution, it is ensured that its is equal
Communicate-type microvoid in greenwave is filled evenly.Then PAN/DMSO mixed solutions are heated to more than 109 DEG C (DMSO fusing points), when
Temperature is gradually decrease in room temperature, greenwave PAN and DMSO coolings split-phase crystallization in mixed solution, is extracted with extractant in greenwave
Thermal inactive occurs for DMSO crystal.When temperature is reduced, the DMSO just precipitations out of greenwave, can be by order to accelerate DMSO extraction
Greenwave is put into the extractants such as methanol, ethanol or water and extracted, and PAN is just trapped in the microvoid in greenwave.
3. sinter and carbonization link
Pre-sintered part comprising carbon materials material precursor PAN and ceramic matrix is carbonized and sintered.In air atmosphere
Greenwave temperature is risen to 250 DEG C with certain programming rate (0.5 DEG C/min) and two hours are incubated, makes PAN resins oxidation-stabilized
Process；800 DEG C are risen to the speed of certain programming rate (4 DEG C/min) again and be incubated a hour, PAN is occurred cyclisation carbon
Change reaction.Continue to raise temperature to the sintering temperature of ceramic powders and be incubated a period of time, be finally made a kind of space in-situ carbon
Change the ceramic material of Material reinforcement toughness reinforcing.Realize the preparation of three-dimensional carbon structure activeness and quietness increasing material manufacturing ceramic, the processing
Method can improve the intensity and toughness of increasing material manufacturing ceramic to a certain degree in three dimensions.
Because the big factor of ceramic material itself fragility makes that its difficulty in commercial Application is larger, the present invention proposes one kind
The functionalization ceramic material model of space in-situ carburization Material reinforcement toughness reinforcing, and propose the preparation work based on increases material manufacturing technology
Skill route (Spatial and Orthotopic Carbide Materials Reinforced Ceramic based on
Addictive Manufacture, abbreviation SOCC-AM).
The present invention it is advantageous that：A kind of high performance ceramic material based on increasing material manufacturing technique is reacted by Cyclization ira situ
Carbon material filled high-temperature sintering high-performance ceramic particle constitute, in structure have ceramics and carbon material two-arch tunnel,
The features such as enhancing of stereoeffect interface, micropore.Three-dimensional carbon structure activeness and quietness increasing material manufacturing ceramic can be achieved
Prepare, the processing method can improve the intensity and toughness of increasing material manufacturing ceramic to a certain degree in three dimensions.
Brief description of the drawings
Fig. 1 is 3D after a kind of material of the high performance ceramic material preparation method based on increasing material manufacturing technique of the present invention is blended
Material component schematic diagram after printing.
Fig. 2 is a kind of binding agent devolatilization pottery of high performance ceramic material preparation method based on increasing material manufacturing technique of the present invention
Material component schematic diagram after porcelain is pre-sintered.
Fig. 3 is a kind of PAN/DMSO solution of the high performance ceramic material preparation method based on increasing material manufacturing technique of the present invention
The pre-sintered greenwave material component schematic diagram of infiltration.
Fig. 4 is that a kind of heat phase separation of high performance ceramic material preparation method based on increasing material manufacturing technique of the present invention is extracted
Material component schematic diagram after solution.
Fig. 5 is a kind of cast material component of the high performance ceramic material preparation method based on increasing material manufacturing technique of the present invention
(after PAN in-situ carburizations and ceramic post sintering) schematic diagram.
In figure：1- ceramic powder particles；2- binding agents；3-DMSO solvents；4-PAN powder particles；5- spaces carbon structure.
Embodiment
The invention provides a kind of high performance ceramic material manufacture method based on increasing material manufacturing technique, by ceramic powders/
Binding agent binary system rapid prototyping material prepares link, polyacrylonitrile (PAN) solution and prepares link, rapid shaping link, takes off
Fat is constituted with pre-sintered link, PAN solution impregnations and Thermal inactive link and sintering with carbonization link.
A kind of high performance ceramic material manufacture method based on increasing material manufacturing technique of the present invention, with spherical carborundum
(SiC) as ceramic raw material, binding agent is used as using polyethylene (PE) or PLA (PLA)；With certain ceramic particle size, load
Amount, binding agent ratio are laminated orderly blending equipment using twin-screw mixer extruder and micro-nano and rapid shaping binary system consumption are made
Material, as shown in Figure 1.Polyacrylonitrile (PAN) solution is configured, is filled by certain mass than weighing respectively after PAN powder is mixed with DMSO
Enter test tube or beaker, test tube or beaker are vertically fixed in 160 DEG C of oil baths and preheated, opening magnetic agitation or mechanical agitation (is used for
PAN concentration is more than 25wt% system), at the uniform velocity stir to polymer and all dissolve, obtain the solution of transparent and homogeneous.Screw rod is heated
Blending extrusion feed device carry is on three-dimensional motion device, and screw rod melting conveying binary system raw material simultaneously extrudes molten state consumption
Material, three-dimensional motion device makes screw extrusion apparatus be moved according to certain track by computer control, binary system molten state consumptive material
The deposition cooling and solidifying generation greenwave blank on shaped platform.Degreasing route according to the binary system material of design enters to greenwave
Row heating, makes high polymer cemented dose to decompose and uniform effusion in gaseous form.Greenwave is continued to be warming up to 2130 DEG C of (SiC ceramics
Theoretical sintering temperature), insulation a period of time forms pre-sintered part, it is ensured that sample has certain intensity, and being formed has connection
The pre-sintered part of ceramics of type microvoid structure, as shown in Figure 2.It is molten to PAN with the pre-sintered greenwave of the PAN solution impregnations configured
Liquid applies certain pressure, it is ensured that it fills uniformly with communicate-type microvoid in greenwave, as shown in Figure 3.Then by PAN and DMSO
Mixed solution is heated to more than 109 DEG C, when temperature is gradually decrease to PAN and DMSO coolings split-phase crystallization in room temperature, solution, with extraction
Take agent to extract DMSO crystal and occur Thermal inactive, the material structure of greenwave is as shown in Figure 4.To including carbon materials material precursor PAN
It is carbonized and is sintered with the pre-sintered part of ceramic matrix.By greenwave temperature with certain programming rate (0.5 in air atmosphere
DEG C/min) rise to 250 DEG C and be incubated two hours, make the oxidation-stabilized process of PAN resins；Again with certain programming rate (4 DEG C/
Min speed) rises to 800 DEG C and is incubated a hour, PAN is occurred cyclisation carburizing reagent.Continue to raise temperature to ceramic powder
The sintering temperature at end is simultaneously incubated a period of time, is finally made a kind of ceramic material of space in-situ carburization Material reinforcement toughness reinforcing, such as
Shown in Fig. 5.The preparation of three-dimensional carbon structure activeness and quietness increasing material manufacturing ceramic is realized, the processing method can be in three dimensions
The intensity and toughness of increasing material manufacturing ceramic are improved to a certain degree.
In Fig. 1-Fig. 5, the carbon material obtained after SiC, PAN and sintering is all actually the grain in respective winding arrangement, figure
Footpath is to illustrate, in the model finally given, and SiC is sintered to turn into the space structure with microvoid, and PAN and DMSO is to greenwave
Infiltration, PAN is distributed in SiC microvoid with molecular state, and PAN situ convertings are carbon material, carbon material after sintering again
It is distributed in the chi structure in space in SiC microvoid, so end article has high intensity and high tenacity.
Claims (9)
1. a kind of high performance ceramic material preparation method based on increasing material manufacturing technique, it is characterised in that preparation process order is such as
Under：The first step, ceramic powders/binding agent binary system rapid prototyping material prepares link；It is prepared by second step, polyacrylonitrile solution
Link；3rd step, greenwave is obtained by ceramic powders/binding agent binary system rapid shaping link；4th step, greenwave degreasing with
Pre-sintered link；5th step, it is pre-sintered after greenwave infiltrate and infiltrates in PAN solution after greenwave in PAN and DMSO thermics
Phase separation link；Being detained in 6th step, greenwave microvoid has the sintering after PAN and carbonization link.
2. a kind of high performance ceramic material preparation method based on increasing material manufacturing technique according to claim 1, its feature
It is：Ceramic powders/binding agent binary system rapid prototyping material is prepared in link using spherical carborundum as ceramic raw material,
Using polyethylene or PLA as binding agent, it is laminated orderly blending equipment using twin-screw mixer extruder and micro-nano and is made quickly
It is molded binary system consumptive material.
3. a kind of high performance ceramic material preparation method based on increasing material manufacturing technique according to claim 1, its feature
It is：Polyacrylonitrile solution prepares concretely comprising the following steps for link：PAN powder and DMSO are weighed respectively by certain mass ratio, are mixed
Load test tube or beaker afterwards, beaker is vertically fixed in 160 DEG C of oil baths and preheated, open magnetic agitation or mechanical agitation, at the uniform velocity
Stirring is all dissolved to polymer, obtains the solution of transparent and homogeneous.
4. a kind of high performance ceramic material preparation method based on increasing material manufacturing technique according to claim 1, its feature
It is：The screw rod that concretely comprises the following steps of rapid shaping link heats blending extrusion feed device carry on three-dimensional motion device, spiral shell
Bar melting conveying binary system raw material simultaneously extrudes molten state consumptive material, and three-dimensional motion device makes screw extrusion apparatus by computer control
Moved according to certain track, binary system molten state consumptive material deposits cooling and solidifying generation greenwave on shaped platform.
5. a kind of high performance ceramic material preparation method based on increasing material manufacturing technique according to claim 1, its feature
It is：Degreasing makes high poly- with being heated in pre-sintered link according to the degreasing route of the binary system material of design to greenwave
Thing binding agent is decomposed and uniform effusion in gaseous form；Greenwave is continued again temperature being increased to 2130 DEG C, insulation a period of time
Pre-sintered part is formed, the pre-sintered part of ceramics with communicate-type microvoid structure is formed.
6. a kind of high performance ceramic material preparation method based on increasing material manufacturing technique according to claim 1, its feature
It is：The greenwave crossed in PAN solution impregnations and Thermal inactive link with the PAN solution impregnations pre-sintering configured, it is molten to PAN
Liquid applies certain pressure, and PAN solution fills uniformly with communicate-type microvoid in greenwave.
7. a kind of high performance ceramic material preparation method based on increasing material manufacturing technique according to claim 6, its feature
It is：PAN/DMSO mixed solutions are heated to more than 109 DEG C, when temperature is gradually decrease in room temperature, greenwave in mixed solution
PAN and DMSO cooling split-phase crystallizations, extract DMSO crystal in greenwave with extractant and occur Thermal inactive.
8. a kind of high performance ceramic material preparation method based on increasing material manufacturing technique according to claim 7, its feature
It is：Extractant is methanol, ethanol or water.
9. a kind of high performance ceramic material preparation method based on increasing material manufacturing technique according to claim 1, its feature
It is：Sintering is carbonized and sintered to the pre-sintered part comprising carbon materials material precursor PAN and ceramic matrix with being carbonized in link,
Greenwave temperature is risen to 250 DEG C with certain programming rate in air atmosphere and two hours are incubated, makes PAN resins oxidation-stabilized
Process；800 DEG C are risen to the speed of certain programming rate again and be incubated a hour, PAN is occurred cyclisation carburizing reagent；After
High-temperature of continuing rising to ceramic powders sintering temperature and be incubated a period of time, be finally made a kind of space in-situ carburization Material reinforcement
The ceramic material of toughness reinforcing.
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