CN104193345B - The method of microwave-absorbing ceramic parts is prepared based on 3D printing technique - Google Patents

The method of microwave-absorbing ceramic parts is prepared based on 3D printing technique Download PDF

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CN104193345B
CN104193345B CN201410409224.8A CN201410409224A CN104193345B CN 104193345 B CN104193345 B CN 104193345B CN 201410409224 A CN201410409224 A CN 201410409224A CN 104193345 B CN104193345 B CN 104193345B
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powder
microwave
sintering
absorbing
ceramic
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CN104193345A (en
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杜作娟
周丁
黄小忠
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Central South University
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Central South University
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Abstract

The invention discloses a kind of method preparing microwave-absorbing ceramic parts based on 3D printing technique; The method sets up 3D model by computer, ceramic powder, electromagnetic absorption agent powder mixed with organic adhesive, uses 3D to print laser sintering technology and prepare idiosome, then carry out densification sintering to idiosome, obtain microwave-absorbing ceramic parts.Ceramic component absorbing property prepared by the present invention is superior, keep Mechanical Property of Ceramics and corrosion resistant performance simultaneously, and can carry out any complex construction of personalized careful design as required, and the method is simple to operate, flow process is short, and floor space is little, meets suitability for industrialized production.

Description

The method of microwave-absorbing ceramic parts is prepared based on 3D printing technique
Technical field
The present invention relates to a kind of method preparing microwave-absorbing ceramic parts based on 3D printing technique, belong to microwave-absorbing ceramic Material Field.
Background technology
Stealthy technique not only affects the victory or defeat of modern war, but also will affect the pattern of modern war, and along with high-tech development, following weapons system will comprehensively adopt various stealthy technique to improve the prominent anti-and attack performance of weapons system.Absorbing material for weapons system needs simultaneously specifically good structure properties (intensity high, good toughness etc.) and environmental performance (wear-resisting, corrosion-resistant, high temperature resistant etc.), and high temperature absorbing material seems particularly urgent at modern battlefield.Stupalith has light weight, high temperature resistant, hardness is large, rub resistance, the advantages such as corrosion-resistant and special conductivity, but its fragility is larger, fatigue performance is poor, counter stress and crack-sensitivity, and metallic substance toughness is strong, can process, electrical and thermal conductivity is good, if stupalith and metallic substance can combine by imagination, the advantage of two class materials can be given full play to, change the electromagnetic performance on ceramic powder surface, strongthener is to electromagnetic absorption, but at present the research of ceramic metal composite wave-suction material is shown, only obtain and (be only limitted to SiC using fibrous ceramic as matrix, B 2o 3, SiO 2deng different materials, and cannot use simultaneously) ceramic metal absorbing material, particularly metallographic phase be difficult to be incorporated into ceramic matrix, and technique is complicated especially, is often difficult to realize industrial application, the ceramic metal composite wave-suction material simultaneously prepared, due to the thermal expansivity difference of two kinds of inhomogeneity materials, adds surface bonding difficulty, and in this series products, seldom therefore wave-absorbing effect is not good usually for metal content.The Layered manufacturing pattern that 3D prints technique can realize local temperature control and locally manufacture, and is conducive to dispersive stress, improves intensity.3D printing technique designs a model as source with Computerized three-dimensional, the discrete and numerical control molding system by software hierarchy, utilizes the mode such as laser beam, hot melt nozzle to manufacture metal parts, plastic prod, cell tissue, ceramic idiosome.Relative to traditional manufacture, the most outstanding advantage of 3D printing technique is without the need to mechanical workout or any mould, just directly can generate the device of any shape from computer graphics data, substantially reduce the lead time of product.This brings great convenience to research staff, by 3D printing technique can produce easily traditional method be difficult to manufacture high-end accurate device.In addition, because 3D printing technique does not need to use mould, it reduce the manufacturing cost of single products and pilot, be specially adapted to the exploitation of product innovation and the production of tailor-made product.Because this product is using pottery as external phase, metal as discrete phase distribution wherein, therefore preferably uses the sintering temperature and low pottery that refractory metal is arranged in pairs or groups relative, otherwise will have a strong impact on wave-absorbing effect when metal content is higher.
Summary of the invention
For the defect preparing the existence of ceramic metal composite wave-suction material in prior art, the object of the invention is to be that providing a kind of combines ceramic powder material and absorbing material, give full play to both advantages, prepare absorbing property superior, keep Mechanical Property of Ceramics and corrosion resistant performance simultaneously, and the method for the ceramic component of any complex construction of personalized careful design can be carried out as required, the method is simple to operate, flow process is short, and floor space is little, meets industrial production.
The invention provides a kind of method preparing microwave-absorbing ceramic parts based on 3D printing technique, the method comprises the following steps:
Step (1): modeling
Set up the 3D model of microwave-absorbing ceramic parts by computer, then press layer by computer and decompose, become by 3D model decomposition a series of thickness to be the two-dimensional model of 100 ~ 300 μm;
Step (2): batching
Ceramic powder, electromagnetic absorption agent powder and organic adhesive powder are carried out being mixed to get mixed powder material according to volume ratio 0.2 ~ 3:0.2 ~ 3:1;
Step (3): embryo processed
In the support equipment of the 3D model data input 3D printer that step (1) is built up, and print routine is set, again step (2) gained mixed powder material is injected 3D printer, under protective atmosphere environment, prepare two-dimensional slice by laser apparatus sintering processing and automatically realization is successively piled up shaping, obtain microwave-absorbing ceramic part blank;
Step (4): sintering
Microwave-absorbing ceramic parts idiosome step (3) obtained carries out densification sintering, obtains microwave-absorbing ceramic parts.
The method preparing microwave-absorbing ceramic parts based on 3D printing technique of the present invention also comprises following preferred version: in preferred scheme, electromagnetic absorption agent is one or more in iron, cobalt, nickel, aluminium, and/or be ferrite and/or zinc oxide, and/or be one or more in graphite, carbon black, carbon fiber.Preferred radio-radar absorber has the better compatibleness with stupalith, is conducive to improving ceramic absorbing property when not affecting Mechanical Property of Ceramics.
Ceramic powder particle diameter < 200 μm in preferred scheme; The ceramic powder of preferred size has better sphericity, mobility.
In preferred scheme, ceramic powder is one or more powdered materials in aluminum oxide, zirconium white, silicon oxide, magnesium oxide, silicon carbide, norbide; Most preferably be at least two kinds of powdered materials in aluminum oxide, zirconium white, silicon oxide, magnesium oxide, silicon carbide, norbide; Preferred ceramic powder has and radio-radar absorber and the better compatibleness of binding agent, is more conducive to the mechanical property and the functionalization that keep pottery.
Organic binder bond powder diameter < 150 μm in preferred scheme; The organic binder bond powder of preferred size has better dispersing property.
In preferred scheme, organic adhesive powder is one or more in polystyrene, resin, paraffin, nylon powder; Preferred organic adhesive and stupalith and electromagnetic absorption agent have better compatibility, are more conducive to preventing the deformation of ceramic post sintering process, cracking etc.
In preferred scheme, densification sintering is pressureless sintering, hot pressed sintering, HIP sintering, reaction sintering or microwave sintering.
In preferred scheme, protective atmosphere is one or more in nitrogen, argon gas, helium.
The working conditions of laser apparatus in preferred scheme: power is 10 ~ 500 watts, working cylinder temperature 40 ~ 250 DEG C, scanning speed is greater than 200m/s.It is shaping that preferred laser work condition is more conducive to ceramic part blank.
Beneficial effect of the present invention: the present invention on the basis of existing technology, successfully just 3D printing technique uses suction wave energy field of ceramic material preparation, not only ceramic powder and absorbing material are combined well, give full play of both advantages, have good mechanical property and corrosion resistant performance and absorbing property concurrently, the ceramic absorption flat plate with periodicity side's cone array surface as prepared by the inventive method can be realized 8 ~ 12GHz frequency internal reflection rate at 2mm thickness and all be less than-10dB (northeastern Japan college professor vows that island sage makes the magnetic silicon carbide ceramic fiber absorbing material of preparation just can reach this effect under 6mm thickness), compare like product thickness obviously to reduce, significantly reduce the area density of product, and personalized careful design can be carried out to microwave-absorbing ceramic parts as required, prepare arbitrary shape, complicated, that there is fine structure ceramic idiosome easily, minimum control formed precision reaches 0.8mm, is conducive to research and development and the production of the product with complicated shape and fine structure requirement.
Accompanying drawing explanation
The microwave-absorbing ceramic member surface plate reflectance test result that [Fig. 1] obtains for embodiment 1.
The microwave-absorbing ceramic member surface plate reflectance test result that [Fig. 2] obtains for embodiment 2.
Embodiment
Following examples are intended to further illustrate content of the present invention, instead of limit the scope of the invention.
Embodiment 1
The 3D model of the microwave-absorbing ceramic parts required for setting up with proE software in a computer, then press layer decomposition by computer, 3D model decomposition is become a series of two-dimensional slice model, and the thickness of each thin slice is set as 200 μm.Get out raw material by following volume percent: silicon carbide powder 50%, nickel powder 30%, epoxy powder 20%, three kinds of powder are put into Homogeneous phase mixing in specific container.The powder mixed pours 3D printer raw cylinder into.Carry out instrument testing, arrange between laser power 15 ~ 50 watts, working cylinder temperature 55 DEG C, scanning speed is greater than 200m/s.Carry out overlaying powder operation until working position paving powder is smooth.Multilayer manufacture is carried out by computer.Multilayer processing terminates rear naturally cooling, and the careful Yu Fenhou that removes obtains idiosome.Hot pressed sintering is carried out to idiosome.Sintering process carries out protection of inert gas to idiosome.Obtained ceramic component reflectance test curve is as Fig. 1 (thickness 1.2mm).
Embodiment 2
Set up the 3D model of required microwave-absorbing ceramic parts in a computer, then press layer decomposition by computer, 3D model decomposition is become a series of two-dimensional slice model, and the thickness of each thin slice is set as 150 μm.Raw material is got out: boron carbide powder 40%, carbon black powder 30%, nylon powder 30% by following volume percent.Three kinds of powder are put into Homogeneous phase mixing in specific container.The powder mixed pours 3D printer raw cylinder into.Carry out instrument testing, arrange between laser power 170 ~ 200 watts, working cylinder temperature 180 DEG C, scanning speed is greater than 200m/s.Carry out overlaying powder operation until working position paving powder is smooth.Multilayer manufacture is carried out by computer.Multilayer processing terminates rear naturally cooling, and the careful Yu Fenhou that removes obtains idiosome.HIP sintering is carried out to idiosome.Sintering process carries out protection of inert gas to idiosome.Obtained ceramic component reflectance test curve is as Fig. 2 (thickness 1.1mm).
Embodiment 3
The 3D model of the microwave-absorbing ceramic parts required for setting up with proE software in a computer, then press layer decomposition by computer, 3D model decomposition is become a series of two-dimensional slice model, and the thickness of each thin slice is set as 250 μm.Get out raw material by following volume percent: alumina powder 25%, silicon carbide powder 25%, nickel powder 30%, epoxy powder 20%, three kinds of powder are put into Homogeneous phase mixing in specific container.The powder mixed pours 3D printer raw cylinder into.Carry out instrument testing, arrange between laser power 15 ~ 50 watts, working cylinder temperature 55 DEG C, scanning speed is greater than 200m/s.Carry out overlaying powder operation until working position paving powder is smooth.Multilayer manufacture is carried out by computer.Multilayer processing terminates rear naturally cooling, and the careful Yu Fenhou that removes obtains idiosome.HIP sintering is carried out to idiosome.Sintering process carries out protection of inert gas to idiosome.Obtained ceramic component is all less than-8dB in 8 ~ 18GHz internal reflection rate, and absorption peak is less than-10dB.
Embodiment 4
The 3D model of the microwave-absorbing ceramic parts required for setting up with proE software in a computer, then press layer decomposition by computer, 3D model decomposition is become a series of two-dimensional slice model, and the thickness of each thin slice is set as 200 μm.Get out raw material by following volume percent: alumina powder 15%, silicon carbide powder 20%, silicon oxide 15%, iron powder 30%, epoxy powder 20%, three kinds of powder are put into Homogeneous phase mixing in specific container.The powder mixed pours 3D printer raw cylinder into.Carry out instrument testing, arrange between laser power 15 ~ 50 watts, working cylinder temperature 55 DEG C, scanning speed is greater than 200m/s.Carry out overlaying powder operation until working position paving powder is smooth.Multilayer manufacture is carried out by computer.Multilayer processing terminates rear naturally cooling, and the careful Yu Fenhou that removes obtains idiosome.Hot pressed sintering is carried out to idiosome.Sintering process carries out protection of inert gas to idiosome.Obtained ceramic component is all less than-8dB in 8 ~ 18GHz internal reflection rate, and absorption peak is less than-10dB.

Claims (6)

1. prepare the method for microwave-absorbing ceramic parts based on 3D printing technique, it is characterized in that, comprise the following steps:
Step (1): modeling
Set up the 3D model of microwave-absorbing ceramic parts by computer, then press layer by computer and decompose, become by 3D model decomposition a series of thickness to be the two-dimensional model of 100 ~ 300 μm;
Step (2): batching
Ceramic powder, electromagnetic absorption agent powder and organic adhesive powder are carried out being mixed to get mixed powder material according to volume ratio 0.2 ~ 3:0.2 ~ 3:1; Described porcelain powder diameter < 200 μm; Described organic binder bond powder diameter < 150 μm;
Step (3): embryo processed
In the support equipment of the 3D model data input 3D printer that step (1) is built up, and print routine is set, again step (2) gained mixed powder material is injected 3D printer, under protective atmosphere environment, prepare two-dimensional slice by laser apparatus sintering processing and automatically realization is successively piled up shaping, obtain microwave-absorbing ceramic part blank; The working conditions of laser apparatus: power is 10 ~ 500 watts, working cylinder temperature 40 ~ 250 DEG C, scanning speed is greater than 200m/s;
Step (4): sintering
Microwave-absorbing ceramic parts idiosome step (3) obtained carries out densification sintering, obtains microwave-absorbing ceramic parts.
2. described method according to claim 1, it is characterized in that, described electromagnetic absorption agent is one or more in iron, cobalt, nickel, aluminium, and/or is ferrite and/or zinc oxide, and/or is one or more in graphite, carbon black, carbon fiber.
3. described method according to claim 1, it is characterized in that, described ceramic powder is one or more powdered materials in aluminum oxide, zirconium white, silicon oxide, magnesium oxide, silicon carbide, norbide.
4. method according to claim 1, is characterized in that, described organic adhesive powder is one or more in polystyrene, resin, paraffin, nylon powder.
5. method according to claim 1, is characterized in that, described densification sintering is pressureless sintering, hot pressed sintering, HIP sintering, reaction sintering or microwave sintering.
6. method according to claim 1, is characterized in that, described protective atmosphere is one or more in nitrogen, argon gas, helium.
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