CN1163437C - Reticular microwave-absorbing body ceramic and its producing method - Google Patents
Reticular microwave-absorbing body ceramic and its producing method Download PDFInfo
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- CN1163437C CN1163437C CNB001258788A CN00125878A CN1163437C CN 1163437 C CN1163437 C CN 1163437C CN B001258788 A CNB001258788 A CN B001258788A CN 00125878 A CN00125878 A CN 00125878A CN 1163437 C CN1163437 C CN 1163437C
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Abstract
The present invention discloses a reticular ceramic microwave-absorbing body, and a producing method thereof, and belongs to the technical field of preparing microwave absorption materials. The reticular ceramic microwave-absorbing body is formed by the method that a polyurethane foam with an opening three-dimensional network type skeleton structure is adopted; the ingredients with the microwave absorption function are made into ceramic slurry with thixotropy; then, the slurry is uniformly coated on the reticular organic foam, and after the slurry is dried, the organic foam is burned out and a blank body is sintered, and thus, a reticular ceramic microwave-absorbing body is formed. The reticular ceramic microwave-absorbing body can be in a single-layer structure as well as in a multi-layer structure, and can be designed and controlled according to practical application. The ingredients for absorbing microwave can be made of microwave absorbing materials, such as silicon carbide, ferrite, metal miropowder, etc.
Description
The present invention relates to a kind of mesh-type microwave-absorbing body and manufacture method thereof, belong to the microwave absorbing material preparation field.
Microwave absorbing material is meant can the attenuation by absorption incident electromagnetic wave, and converts its electromagnetism wave energy to heat energy and the class material that dissipates or make hertzian wave to disappear because of interference.It is a kind of important functional material, plays an important role in national economy all departments.Along with the continuous development of technology such as micro-wave communication, radar, space flight, electromagnetic compatibility and electronic countermeasure, its application is increasingly extensive, for example, and in the antagonism of military technique, at the aspects such as performance that improve microwave device, scientific instrument and industrial equipments.
Microwave absorbing material is divided into application type and structure-type two big classes by its moulding process and supporting capacity.Application type be with absorption agent be coated on target surface after binding agent mixes and form microwave absorbing coating.The structure-type wave-absorption material is a kind of multifunctional composite, is made of through reasonable structural design absorbing material and polymer matrix composites.The structure-type wave-absorption material can carry makes structural part, can absorb hertzian wave preferably again, and the parts of plastic various complicated shapes have become the important developing direction of contemporary absorbing material.The structure-type wave-absorption material generally adopts three-decker, promptly is made up of wave permeation layer, suction ripple layer and reflecting layer (claiming plaque layer again).Early stage " burnt graceful " (Jaummann) absorbing material is exactly a kind of typical structural wave-absorbing material, and it is made by the paper of seven layers of carbonaceous powder, separates with dielectric spacer material between every layer.In order to improve absorbing property, material is designed to staged multilayer absorbing material, fill different loss fillers for every layer, make the absorbing material front surface layer arrive each layer impedance of laminar substrate down, press exponential taper to low impedance value by high resistance, by changing the content of weighting agent, obtain best microwave absorbing property.On the basis of " burnt graceful " absorbing material, people have been developed circuit analog absorbing material, conducting material are made the suction ripple thin slice of thin fillet, grid, cruciform or more complicated figure.
Recently developed the sandwich structure absorbing material again, sandwich structure has following advantage: (1) is because the effect of sandwich can significantly improve the structure section moment of inertia, thus raising structural strength and the weight that alleviates structure; (2) consider that from absorbing property the effect of sandwich is more outstanding, the hertzian wave that enters structure from surperficial wave permeation layer carries out repeatedly scattering and absorption by cellular sandwich.Most typical sandwich structure is honeycomb-like sandwich structure, just inhales the ripple layer and adopts polynuclear plane, filled and process absorbing material in honeycomb.Honeycomb core is made by carbon fiber, glass fibre, enhanced polymkeric substance usually.Design more complicated for Honeycomb Sandwich Microwave Absorbing Materials, on the basis of following the electricity coupling, to carry out comprehensive consideration to these class effect of material performance such as kind, performance, distribution form and resin matrix, strongthener and attenuator of absorption agent, to obtain to have the material of efficient absorbing property.In order to improve absorbing property, the honeycomb structure type absorbing material often is designed to multilayered structure.
No matter being application type or structure-type microwave absorbing material, up to now, mainly is to be the matrix material of matrix with synthetic resins, this class material anti-corrosion-resistant and high temperature resistant aspect have significantly deficiency.For this reason, people have been developed the sintered compact microwave-absorbing body.What application was maximum at present is the ferrite cemented body absorbing material.Though having, ferrite absorbs advantage strong, the frequency band broad, shortcomings such as density is big, hot properties difference that it also has.In order to overcome the deficiency of ferrite cemented body absorbing material, people have been developed silicon carbide ceramics sintering wave-absorber again.Advantage such as absorbing property is good because silicon carbide has, low-thermal-expansion, high heat conductance, corrosion-resistant and proportion are little, becoming has the microwave absorbing of development potentiality stupalith most.
In order to improve the microwave absorbing property of ceramic post sintering wave-absorber, except selecting the good raw material of absorbing property, the more important thing is the structure that to improve wave-absorber.The inventor is subjected to the inspiration of honeycomb sandwich construction, and imagination is designed to a kind of vesicular structure with microwave-absorbing body.The structure of porous material mainly contains honeycomb type, foam type and mesh-type.The duct of honeycomb type is straight, and the duct in the structure of foam type is isolated, and these two kinds of structures all are unfavorable for absorption of electromagnetic wave.The mesh-type structured material but is a kind of high porosity (70-95%) material with the three-dimensional netted skeleton structure of perforate, the technology of making this screen like and porous ceramic material is that United States Patent (USP) U.S Pat.No.3 090 094 proposes, this class mesh-type structured material has been used as strainer, support of the catalyst and heat exchanger, but does not see the report that is used for microwave-absorbing body as yet.Consider electromagnetic scattering effect, this eyed structure can be improved the microwave absorbing property of material.
The object of the present invention is to provide a kind of reticular microwave-absorbing body ceramic and manufacture method thereof, reach the effect of hertzian wave abundant in material structure " saturating, diffusing, suction ", thereby improve the absorbing property of material by the eyed structure of mutual perforation.Compare with other structural wave-absorbing material, except having excellent absorbing property, also have significantly high temperature resistant, high strength, low creep, low bulk, chemical stability is good and premium properties such as corrosion-resistant.
Desire to reach purpose of the present invention, must solve two gordian technique points, the one, the material that selection can absorb microwave is that main component is made slurry, the 2nd, the homogeneity that slurry applies on the organic foam body of mesh-type structure,
It is that per inch contains 5-100 hole that purpose of the present invention is implemented to be to rely on the organic foam body with the three-dimensional netted skeleton structure of perforate, void content 75-95% hole dimension.The component that will contain microwave absorption is made ceramic size, then slurry is coated on the organic foam reticulate body equably, burns the organic foam body after the drying and obtains a kind of mesh pottery wave-absorber.The selection that is used to prepare the organic foam material of mesh wave-absorber must be perforate and have certain wetting ability, but also enough rebound resiliences should be arranged, after guaranteeing extruding unnecessary slurry, can promptly recover shape.In addition, must volatilize being lower than under the ceramic firing temperature, and do not pollute pottery, the organic foam material that adapts to this requirement has the own ester of polyurethane (urethane), polyvinyl chloride, polystyrene, latex, Mierocrystalline cellulose etc.Perhaps the mesh-type wave-absorber is designed to the multilayered structure that aperture or pore change in gradient.
The preferential recommendation of the present invention selects for use the polyurethane sponge shape foams with eyed structure as matrix, and its hole dimension is 5-100ppi (ppi is the abbreviation hole count per square inch of pores per inch).In order further to improve the adhesivity between sponge matrix and the ceramic size, the present invention also carries out surface modification with the cmc soln of 0.2-2wt% concentration to washed sponge skeleton.
Solid matter as the microwave absorbing function can be silicon carbide, ferrite (as Ni ferrite, Zn ferrite, barium ferrite), metal fine powder (as nickel powder, iron powder, cobalt powder), their particle shape is preferably disc or aciculiform, and particle diameter should be less than 45 μ m.
When the powder that will contain the microwave absorbing component was made slurry, its solid content was between 40-80% (weight).The most frequently used solvent of preparation slurry is a water, also can be organic solvent such as ethanol, b propanol, acetone, trieline etc.According to the requirement of technological forming, slurry not only has certain fluidity, and has preferably thixotropy and promptly require slurry to have to be in curdled appearance when static, but recovers mobile characteristic again under external force.The flowing property of slurry guarantees that slurry is penetrated in the organic foam body in steeping process, and is coated in equably on the hole wall of foam network.The thixotropy of slurry can guarantee at dipping sizing agent with when extruding unnecessary slurry, in shearing action decline low viscosity, improves the flowability of slurry, help moulding, and when moulding finished, the viscosity of slurry raises, mobile reduction.This finalizes the design attached to the slurry on the hole wall solidifies easily with regard to making, in order to avoid influence the homogeneity of goods because slurry mobile causes the serious plug-hole of base substrate.In order to improve the intensity of biscuit, and prevent that base substrate from subsiding in the organism exclusion process, in slurry, add binding agent, can guarantee that the sintering wave-absorber has enough physical strengths.For making solid powder energy homodisperse in solvent often need add certain amount of dispersant to obtain well slurry of stability.For the rheological property that improves slurry especially thixotropy, generally need to add a spot of rheological agent.When viscosity is on the low side, should adds small amount of flocculant (increase and touch agent) and improve adhesivity between slurry and the organic foam body to improve viscosity.In the pulp preparation process, generally can produce a large amount of bubbles, add a small amount of defoamer usually to eliminate bubble.For ease of describing, plan the additive that when the preparation slurry, must add such as dispersion agent, binding agent, rheological agent, flocculation agent (increase and touch agent), used material commonly used and the corresponding add-on of defoamer is summarized in table 1.
Additive and consumption that table 1 dipping is used always with slurry
| Title | The material that uses | Add-on (%) |
| Dispersion agent | The ammonium salt or the sodium salt of Sodium hexametaphosphate 99, coke deflection acid sodium, positive sodium-metaphosphate, aluminium colloidal sol, polyacrylic acid (PAA) and polymethyl acrylic acid (PMAA) | 0.05-5 |
| Binding agent | The inorganic sol polyoxyethylene glycol that water glass, phosphoric acid salt and silicon oxide, aluminum oxide or zirconium white form, polyvinyl alcohol, polyvinyl butyral acetal, poly-acetic acid hexene ester, hydroxyl hexyl Mierocrystalline cellulose etc. | 0.2-10 |
| Rheological agent | Wilkinite, kaolin, carboxymethyl cellulose, hydroxyl hexyl Mierocrystalline cellulose etc. | 0.01-2 |
| Flocculation agent | Polymine, polyacrylamide (polyacrylamide), carboxymethyl cellulose | 0.001-0.5 |
| Defoamer | Low-molecular-weight alcohol, silicone, Nopco 267-A | 0.005-0.5 |
Concrete preparation process is as follows:
The slurry for preparing is carried out dip treating to the organic foam body, in steeping process, should guarantee that slurry is full of all meshes of organic foam body.With the organic foam body of inhaling full slurry by a kind of pair roller single-lead-screw extruding briquetting machine (patent No. is ZL 99 2 39981.5) of designing voluntarily to remove redundant sizing agent, this kind extrusion machine two roller spacings up and down can be regulated on request, and the proportion of mesh porous insert is regulated by pair roller spacing and control extruding number of times.In order to guarantee that slurry is coated on the net muscle of organic foam body equably, and on the net muscle, have certain thickness, must optimize pair roller spacing and the number of times by pair roller.Through extruding the wet base of the mesh maintenance at room temperature earlier that unnecessary slurry obtains, carry out drying then, drying temperature is 110 ℃ can adopt oven dry or microwave drying.Dried sample can enter the stage of burning till.In sintering process, two important stages are arranged, promptly low thermophase and hot stage.At low thermophase, should slowly heat up makes the eliminating of slowly and fully volatilizing of organic foam body.In this stage,, can cause blank cracking and powder phenomenon-tion because of the organism vigorous oxidation produces a large amount of gases at short notice if it is too fast to heat up.Adopting oxidizing atmosphere to allow organism pass through oxidative pathway as it should be noted that more than this stage gets rid of.After organism is got rid of fully, then can be rapidly heated 1100-1900 ℃, sintering atmosphere is air, vacuum or atmosphere protection, soaking time is to realize that the sintering of ceramic powder was to obtain to have the mesh sintered compact of sufficient intensity in 1-5 hour.
The mesh sintered compact is carried out performance characterization comprise proportion, pore size, void content, transmitance, mechanical property, absorbing property and structure etc., especially absorbing property.
Mesh-type microwave-absorbing body provided by the invention, compare with present fiber-reinforced polymer cellular sandwich wave-absorber material and other sintered compact, except microwave absorbing material causes microwave attenuation, also have eyed structure to cause microwave attenuation, and this material do not select the tropism to the absorption of microwave, and is promptly almost irrelevant with electromagnetic incident angle.In addition, this wave-absorber also has the quite low (0.2-0.6g/cm of light weight, proportion
3) characteristics, thereby can reduce manufacturing cost.
Fig. 1 is the structure photo of microwave ceramics microwave-absorbing body.Canescence is the skeleton structure of mesh microwave-absorbing body, and the solid matter that contains the microwave absorbing function is in these positions, and black is the mesh hole, and these holes are interconnected.
Fig. 2 is the absorbing property curve with microwave-absorbing body of different width of meshs.X-coordinate is frequency (GHz), and ordinate zou is microwave attenuation amount (dB).A represents solid wave-absorber in the curve, and b represents 23ppi mesh wave-absorber, and c represents 10ppi mesh wave-absorber.
Fig. 3 is the absorbing property curve of the 10ppi mesh microwave-absorbing body of different thickness.The same Fig. 2 of X-coordinate and ordinate zou.
Further illustrate creativeness of the present invention below in conjunction with embodiment but absolutely not only be confined to described embodiment.
Embodiment 1
As microwave absorbing material, particle diameter is less than 45 μ m with silicon carbide.The slurry component is silicon carbide 70g, aluminum oxide 20g, clay 3g, silicon sol 26g, deionized water 9g, 4wt% cmc soln 5g, defoamer (Nopco 267-A) 0.5g.Prepare slurry by ball-milling technology.Slurry dipping hole dimension is respectively two kinds of polyurethane sponge shape foams of 10ppi and 23ppi.In order to improve the adhesivity between foams and the ceramic size, present embodiment carries out surface modification with the cmc soln of 1wt% concentration to the sponge skeleton.The sponge that inhales full slurry gets rid of redundant sizing agent by the pair roller extruding.After the wet base maintenance at room temperature of the mesh of forming, under 110 ℃, carry out drying, carry out sintering then.By slowly heating up to get rid of organism, the 1450 ℃ of sintering that are rapidly heated then obtain the mesh microwave-absorbing body before 600 ℃, and its structure as shown in Figure 1.The proportion of 10ppi and 23ppi mesh sintered compact is respectively 0.45g/cm
3, 0.60g/cm
3, flexural strength is respectively 3.46MPa, 2.34MPa, and their absorbing property is seen Fig. 2 and Fig. 3.
As can be seen, with respect to solid wave-absorber, mesh-type structure wave-absorber shows excellent absorbing property, and the thickness of increase cartridge can improve absorbing property.
Embodiment 2
With silicon carbide as microwave absorbing material.Slurry component and pulp preparation process are with embodiment 1.Slurry dipping hole dimension is respectively 10ppi, 23ppi, 50ppi and four kinds of polyurethane sponges of 80ppi.The sponge that inhales full slurry gets rid of redundant sizing agent by the pair roller extruding, obtains the wet base of mesh of four kinds of pore sizes, stacks from big to small by the aperture then and forms the bore diameter gradient structure.After the multilayer mesh base substrate maintenance at room temperature of forming, under 110 ℃, carry out drying, carry out sintering then.By slowly heating up to get rid of organism, the 1450 ℃ of sintering that are rapidly heated then obtain multilayer mesh microwave-absorbing body before 600 ℃.
Embodiment 3
As microwave absorbing material, particle is a disc with barium ferrite, and particle diameter is about 5 μ m.The slurry component is barium ferrite 100g, MnCO
31g, kaolin 1g, aluminium colloidal sol 20g, deionized water 10g, 10wt% polyacrylic acid ammonium solution 2g, 4wt% cmc soln 5g, defoamer (Nopco267-A) 0.5g.Prepare slurry by ball-milling technology.Slurry dipping hole dimension is the polyurethane sponge of 23ppi.The sponge that inhales full slurry gets rid of redundant sizing agent by the pair roller extruding.After the wet base maintenance at room temperature of the mesh of forming, under 110 ℃, carry out drying, carry out sintering then.Heat up to get rid of organism by slow at 600 ℃, the 1300 ℃ of sintering that are rapidly heated then obtain the mesh microwave-absorbing body.All the other are with embodiment 1.
As microwave absorbing material, particle is a disc with the nickel micro mist, and particle diameter is about 10 μ m.The slurry component is aluminum oxide 50g, and chromic oxide 10g, nickel powder are 40g, magnesiumcarbonate 1g, kaolin 3g, aluminium colloidal sol 30g, deionized water 20g, 4wt% cmc soln 5g, defoamer (Nopco267-A) 0.5g.Prepare slurry by ball-milling technology.Slurry dipping hole dimension is the polyurethane sponge of 50ppi.The sponge that inhales full slurry gets rid of redundant sizing agent by the pair roller extruding.After the wet base maintenance at room temperature of the mesh of forming, under 110 ℃, carry out drying, carry out sintering then.Before 600 ℃,, in vacuum environment, obtain the mesh microwave-absorbing body then at 1600 ℃ of sintering by slowly heating up to get rid of organism.All the other are with embodiment 1.
Claims (9)
1, a kind of reticular microwave-absorbing body ceramic, it has tridimensional network, it is characterized in that:
(1) hole is to connect mutually, and void content volume percent 75-95, hole dimension are a per inch 5-100 hole;
(2) three-dimensional netted skeleton is made up of silicon carbide, ferrite or metal fine powder.
2, by the described microwave-absorbing body of claim 1, the particle shape that it is characterized in that described silicon carbide, ferrite or metal fine powder is disc or aciculiform, and particle diameter is less than 45 μ m, and content is between 30wt%-80wt%.
3, by the described microwave-absorbing body of claim 1, it is characterized in that the mesh-type structure is single layer structure or is designed to the aperture and the multilayered structure of void content gradual change.
4, a kind of manufacture method by the described mesh microwave-absorbing body ceramic of claim 1 is characterized in that:
(1) selects to have the organic foam body of tridimensional network and perforation pore as skeleton;
(2) use the slurry with thixotropic behavior that the organic foam body is flooded, guarantee that slurry is full of all ducts, the solid matter in the slurry is silicon carbide or ferrite or metal fine powder;
(3) the organic foam body that will inhale full slurry by the pair roller single-lead-screw extruding briquetting machine to get rid of unnecessary slurry;
(4) the wet base maintenance at room temperature of the mesh of forming, dry down at 110 ℃ then;
(5) two stages burnt till; low thermophase slowly heats up fully to get rid of the organic foam body in oxidizing atmosphere; and then be rapidly heated 1100～1900 ℃, and being incubated 1～5 hour and realizing sintering under the condition to obtain the mesh sintered compact, sintering atmosphere is air, vacuum or atmosphere protection.
5, by the manufacture method of the described mesh microwave-absorbing body ceramic of claim 4, it is characterized in that the organic foam body is the own ester foams of polyurethane or polyvinyl chloride foam body or styrofoam.
6, by the manufacture method of claim 4 or 5 described mesh microwave-absorbing body ceramics, it is characterized in that selecting for use the own ester foams of polyurethane, pore is communicated with, and hole dimension is a per inch 5-100 hole.
7, by the manufacture method of the described mesh microwave-absorbing body ceramic of claim 4, it is characterized in that adopting the cmc soln of 0.2-2wt% concentration that washed organic foam body skeleton is carried out surface modification.
8, by the manufacture method of the described mesh microwave-absorbing body ceramic of claim 4, it is characterized in that pulp preparation is:
(1) solvent is that water or organic solvent comprise ethanol, acetone or trieline, and solid content is between weight percent 40-80%;
(2) dispersion agent that uses in the slurry is a kind of in the ammonium salt of Sodium hexametaphosphate 99, coke deflection acid sodium, positive sodium-metaphosphate, aluminium colloidal sol, polyacrylic ammonium salt or sodium salt, polymethyl acrylic acid or the sodium salt, and add-on is the 0.05-5% of system solid phase gross weight;
(3) binding agent that adds in the slurry is the inorganic sol that water glass, phosphoric acid salt and silicon oxide, aluminum oxide or zirconium white form; The organic polymer that adds is polyoxyethylene glycol, polyvinyl alcohol, polyvinyl butyral acetal, poly-acetic acid hexene ester or hydroxyl hexyl Mierocrystalline cellulose, and add-on is the 0.2-10% of system solid phase gross weight;
(4) rheological agent that adds in the slurry is kaolin or wilkinite or carboxymethyl cellulose, and add-on is the 0.01-2% of system solid phase gross weight;
(5) flocculation agent that adds in the slurry is polymine, polyacrylamide or carboxymethyl cellulose, and add-on is the 0.001-0.5% of system solid phase gross weight;
(6) other material that adds as defoamer in the slurry is low-molecular-weight alcohol or silicone, and add-on is the 0.005-0.5% of system solid phase gross weight.
9, by the manufacture method of the described mesh microwave-absorbing body ceramic of claim 4, it is characterized in that slurry in the organic foams process of dipping, the coating quality of mesh-type porous insert and proportion are by regulating the pair roller spacing and pushing number of times and control.
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