CN101181798A - Multi-gradient porous ceramic mold for ceramic injection forming and making method - Google Patents
Multi-gradient porous ceramic mold for ceramic injection forming and making method Download PDFInfo
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- CN101181798A CN101181798A CNA2007101719197A CN200710171919A CN101181798A CN 101181798 A CN101181798 A CN 101181798A CN A2007101719197 A CNA2007101719197 A CN A2007101719197A CN 200710171919 A CN200710171919 A CN 200710171919A CN 101181798 A CN101181798 A CN 101181798A
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Abstract
The invention discloses a multi-layer gradient and porous ceramic mould for ceramic grouting forming and a manufacturing method of the ceramic mould, which is especially suitable for advanced ceramic grouting forming. The structure of the porous ceramic mould comprises a carrier layer (3), a middle layer (2) and a surface separating layer (1); the aperture reduces layer by layer from the carrier layer to the surface separating layer, and forms an asymmetric gradient distribution. The invention has the advantages of no pollution, high intensity, high grouting efficiency and long service life, etc. and provides a high quality and durable mould for the advanced ceramic grouting forming.
Description
Technical field
The present invention relates to a kind of multi-gradient porous ceramic mold for ceramic injection forming and preparation method, belong to the injection forming mould applications.
Background technology
Injection forming is a kind of easy and practical ceramic molding, usually with gypsum as forming mould.But gypsum mold is very easily impaired in slip casting, dry run, enters biscuit of ceramics and become impurity.These micro-impurity can not cause tangible influence to traditional ceramics.But the advanced ceramics that purity is high is very responsive to impurity component, is enough to cause the variation of its physics, chemical property by the trace impurity of gypsum introducing.For example in the transparent alumina ceramics slip-casting shaping process, the calcium ion pollution in the gypsum mold can cause that alumina grain grows up unusually, causes light transmittance to descend, and can't satisfy normal instructions for use.Though, can remove wherein pollutant by certain method after the moulding, can increase operation undoubtedly, raise the cost.
In addition, along with the development of advanced ceramics technology, many new filling forming methods (as slip casing by pressure, centrifugal grouting, pressure filtration molding etc.) occurred, these methods are had higher requirement to mould.Traditional gypsum mold blocks owing to surface apertures is big, easy, intensity is low, has been difficult to satisfy the requirement of production.So researching and developing new mould seems and is even more important.
Porous ceramics is a kind of widely used separation and purification process material, and it is good to have chemical stability, mechanical strength height, easily regeneration, advantages such as long service life.In addition, the aperture of porous ceramics is little, and capillarity is obvious, and has good suction separating property.In recent years, researchers more both domestic and external propose porous ceramics is used as the mould that injection forming is used, and have obtained certain effect.Yet, because the aperture of porous ceramics mould is less, cause the draining of slip casting later stage slower, especially when slip casing by pressure, also can produce excessive pressure drop, cause the slip casting inefficiency.
Summary of the invention
In order to solve the problems that existing mold exists, the invention discloses a kind of multi-gradient porous ceramic mold for ceramic injection forming, be specially adapted to the advanced ceramics injection forming.
The structure of porous ceramics mould of the present invention comprises carrier layer 3 (also claiming supporting layer), intermediate layer 2 and surface isolation layer 1 as shown in Figure 1.The aperture is successively reduced to the surface isolation layer by carrier layer, forms asymmetric gradient and distributes.The effect of carrier layer is a mechanical strength of keeping mould, and absorbs and discharge the moisture of separating from superficial layer.It is definite that the thickness of carrier layer is looked actual needs, is not less than 1mm usually; The pore-size distribution of carrier layer is between 1-100 μ m.The intermediate layer is actual to be exactly transition zone between carrier layer and the surface isolation layer, its thickness≤500 μ m.The intermediate layer can be made up of one or more layers; Also can have only carrier layer and surface isolation layer, and not have the intermediate layer.The surface isolation layer is separated moisture by capillarity and osmotic pressure from slurry, enter carrier layer by the intermediate layer, and forms semi-harden ceramic particle accumulation horizon, the biscuit that obtains wetting on its surface.The pore-size distribution of surface isolation layer can either increase capillarity less than 1 μ m, can guarantee good separating effect again; The thickness of surface isolation layer should be controlled at≤100 mu m ranges, and the resistance when discharging to reduce moisture reduces the pressure drop that acts on the separating layer.
The making of a kind of multi-gradient porous ceramics mould that the present invention proposes realizes by following steps:
1) preparation cellular ceramic substrate layer.Described carrier layer can be but be not limited to the technology preparation of general porous ceramics, as adding between pore creating material, the particle not exclusively sintering, directly foaming etc.The size of carrier layer and profile are looked grouting process and are required to determine.
2) if necessary, can carry out machining, reach the appearance and size of slip casting requirement the carrier layer after burning till.
3) working surface in prepared carrier layer covers the intermediate layer.Described intermediate layer is actually the intermediate zone of carrier layer and surface isolation layer.The pore in intermediate layer is formed by the particle packing of incomplete sintering, and intermediate layer thickness is below 500 μ m.
The preparation section in intermediate layer comprises coating, drying, burns till etc.The used ceramic raw material particle size in preparation intermediate layer should be between the particle size of carrier layer and superficial layer.Raw material (comprising ceramic powder, water, dispersant and binding agent etc.) is prefabricated into the working surface that slurry evenly is coated in carrier layer, utilizes the moisture in the water absorbing properties separating slurry of carrier layer, and obtain the semi-harden wet base substrate of one deck on the surface.Burn till after the drying, obtain in conjunction with firmly, cover uniform intermediate layer.In order not destroy the structure of carrier layer, the sintering temperature in intermediate layer should be lower than carrier layer.When the feed particles of carrier layer and surface isolation layer differs less than 10 times, can not have the intermediate layer, and have only carrier layer and surface isolation layer, aperture forms asymmetric gradient by carrier layer to the surface isolation layer and distributes.When differing by more than 200 times, the feed particles of carrier layer and surface isolation layer can consider to increase one deck intermediate layer, to reduce the otherness between each layer.
The coating processes in intermediate layer can be atomizing spray, high pressure painting, electrostatic spraying, dipping or brushing method coating etc.
4) in prepared interlayer surfaces covering surfaces separating layer.The surface isolation layer directly contacts with slurry when injection forming, moisture in the separating slurry and ceramic particle, so the aperture must be less than the ceramic particle in the slurry, the ceramic particle for preparing the surface isolation layer usually is less than 1 μ m.The preparation method of surface isolation layer is similar to the intermediate layer.Feed particles should be less than the intermediate layer, and sintering temperature should be less than the intermediate layer.
In addition, the surface isolation layer can adopt other special process preparations, as vapour deposition, plasma spraying, plating etc.
A kind of multi-gradient porous ceramics mould that the present invention proposes will be selected different types according to the granularity of the ceramic powder that will pour into a mould in actual use.Carrier layer mainly is to keep the mechanical strength of mould, thus should select cheap ceramic raw material for use as far as possible, as aluminium oxide, carborundum or the like.Guarantee the size of the aperture of surface isolation layer, prevent from that ceramic particle from entering in the hole of mould to cause plug-hole less than ceramic particle in the slurry.
Multi-gradient porous ceramics mould strength height of the present invention, phenomenons such as when in use can image-stone cream mould not peeling off like that, stick is polluted so can not produce the ceramic body of cast.The present invention is applicable to multiple advanced ceramics injection forming, such as aluminium oxide, yittrium oxide, magnesium aluminate spinel, yttrium-aluminium-garnet, zirconia or the like.
Mould of the present invention has the following advantages: 1. rupture strength height, can reach 100MPa, and can fully stand high-pressure slip-casting; 2. the surface is difficult for impairedly, can not produce the product of slip casting and pollute; 3. surface isolation layer aperture is little, can even the slip particle is very thin, also can not block less than 0.05 μ m, is highly suitable for the injection forming of nanometer, sub-micron ceramic size; 4. the surface isolation layer thickness is thin, and resistance was little when moisture was discharged; Especially when slip casing by pressure, the pressure drop of generation is very little, slip casting efficient height; 5. good heat resistance can use under higher temperature; 6. wearability is good, long service life.Though this mould cost substantially exceeds plaster mold service life than the plaster mold height, do not need frequent die change and repair a die, significantly reduce producing cost.Therefore, this invention provides a kind of high-quality durable mould for the advanced ceramics injection forming.
Description of drawings
Fig. 1 is the structural representation of the multi-gradient porous ceramics mould of the present invention's proposition.
Fig. 2 is embodiment 2 described carrier layer vertical views.
Fig. 3 is the carrier layer side view of embodiment 2.
Among the figure: 1. surface isolation layer, 2. intermediate layer, 3. carrier layer, 4. mating surface, 5. working surface.
The specific embodiment
Introduce embodiments of the invention below
Embodiment 1:
Carrier layer adopts average grain diameter 50 μ m electric smelting Al
2O
3Powder is a raw material, adds 1wt%MgO-Al
2O
3-SiO
2As sintering aid, be pressed into the tabular sample with press, fire at 1600 ℃ and obtained the cellular ceramic substrate layer that the porosity is about 35vol% in 2 hours.Observe through SEM, pore-size distribution is mainly at 10～50 μ m.With grinding machine working surface is polished.
The intermediate layer selects for use average grain diameter to be about the Al of 2 μ m
2O
3Powder as dispersant, adds 1wt%MgO as sintering aid with the ammonium polyacrylate of 0.1wt%.Described raw material is mixed with 2wt%PVA solution, and the preparation solid content is the suspension of 10wt%.The carrier layer working surface is immersed in the described suspension takes out air-dryly after about 3 minutes, slowly be warming up to 600 ℃ of organic matters of removing wherein after the drying, continue to be warming up to 1500 ℃ of insulations 2 hours, obtain covering uniform intermediate layer.
Selecting average grain diameter for use is high-purity Al of 0.5 μ m
2O
3Powder is as the raw material of surface isolation layer, and the ammonium polyacrylate that adds 0.5wt% is mixed with the suspension of 1wt% as dispersant.The gained intermediate layer is immersed in taking-up after about 10 minutes in the described suspension, and natural air drying slowly is warming up to 600 ℃ of organic matters of removing wherein after the drying, continues to be warming up to 1300 ℃ of insulations 2 hours, obtains the surface isolation layer of even structure.The surface isolation layer thickness is about 10 μ m, and average pore size is about 0.1 μ m.
Embodiment 2:
Carrier layer adopts average grain diameter 50 μ m electric smelting Al
2O
3Powder is a raw material, and adding the 10wt% granularity is the Al of 0.5 μ m
2O
3Powder is as sintering aid,, adds 10wt% water and mixes as dispersant with the ammonium polyacrylate of 0.1wt%.Adopt the way of vibrating casting, the gained batch is injected rectangular mould, open wide the loam cake natural air drying.Thoroughly the oven dry back obtains the rectangle carrier layer 1600 ℃ of insulations 2 hours.
Carrier layer is processed into as Fig. 2, shape shown in Figure 3.Two is a pair, is cooperated by mating surface (4), forms columniform working surface (5).
It is the Al of 0.5 μ m that granularity is selected in the intermediate layer for use
2O
3Powder is as raw material, adds the 0.7wt% ammonium polyacrylate as dispersant, is hybridly prepared into the suspension that solid content is 5wt% with the PVA solution of 1wt%.According to 0.6ml/cm
2Consumption, gained suspension evenly is coated in the carrier layer working surface, utilize the suction separating property of carrier layer, form one deck granulation mass lamination on its surface.Dry back exists, and slowly is warming up to 600 ℃ to discharge PVA wherein, is warming up to 1400 ℃ and be incubated 2 hours again, obtains covering uniform intermediate layer.
It is high-purity Al of 0.3 μ m that the surface isolation layer adopts granularity
2O
3Powder is a raw material, and the ammonium polyacrylate that adds 1wt% adds the suspension that water is mixed with 1wt% as dispersant.With described suspension according to 0.2ml/cm
2Consumption, be coated in above-mentioned intermediate layer working surface, rely on the suction separating property of himself, obtain the granulation mass lamination of uniform surface isolation layer.Dry back obtains the mould of complete three-decker at 1200 ℃ of sintering.
Embodiment 3:
Carrier layer selects for use average grain diameter to be about the Al of 2 μ m
2O
3Powder adds the 0.7wt% ammonium polyacrylate as dispersant, adds 1wt%MgO as sintering aid, and the starch that adds 10wt% is mixed with the slurry that total solid content is 75wt% as pore creating material with suitable quantity of water.After described slurry cast, heating is solidified starch gelatinization in 75 ° of baking ovens.Dried base substrate slowly is heated to 700 ℃ and discharges starch in Muffle furnace, be warming up to 1500 ℃ and be incubated 2 hours again, obtains carrier layer.
Carrier layer does not cover the intermediate layer, and direct coating surface separating layer.It is high-purity Al of 0.3 μ m that the surface isolation layer adopts granularity
2O
3Powder is a raw material, and the ammonium polyacrylate that adds 1wt% adds the suspension that water is mixed with 1wt% as dispersant.With described suspension according to 0.2ml/cm
2Consumption, be coated in above-mentioned carrier layer surface, rely on the suction separating property of himself, obtain the granulation mass lamination of uniform surface isolation layer.Dry back obtains the mould of complete double-layer structure at 1200 ℃ of sintering.
Embodiment 4:
Carrier layer adopts average grain diameter 50 μ m electric smelting Al
2O
3Powder is a raw material, adds 1wt%MgO-Al
2O
3-SiO
2As sintering aid, be pressed into the tabular sample with press, fire at 1600 ℃ and obtained the cellular ceramic substrate layer that the porosity is about 35vol% in 2 hours.
The intermediate layer is made up of two-layer, at twice preparation.Ground floor selects for use average grain diameter to be about the Al of 2 μ m
2O
3Powder as dispersant, adds 1wt%MgO as sintering aid with the ammonium polyacrylate of 0.1wt%.Described raw material is mixed with 2wt%PVA solution, and the preparation solid content is the suspension of 10wt%.Ground floor is immersed in the described suspension takes out air-dryly after about 3 minutes, slowly be warming up to 600 ℃ of organic matters of removing wherein after the drying, continue to be warming up to 1500 ℃ of insulations cooling after 2 hours.It is high-purity Al of 0.5 μ m that the second layer is selected average grain diameter for use
2O
3Powder is as raw material, and the ammonium polyacrylate that adds 0.5wt% is mixed with the suspension of 1wt% as dispersant.Above-mentioned first interbed is immersed in taking-up after about 10 minutes in the described suspension, and natural air drying slowly is warming up to 600 ℃ of organic matters of removing wherein after the drying, continues to be warming up to 1300 ℃ of insulations cooling after 2 hours.
The surface isolation layer is selected the commercial oxidation aluminium colloidal sol (average grain diameter 30nm) of 25wt% for use, is diluted to behind the 2wt% according to 0.1ml/cm
2The consumption atomizing spraying in interlayer surfaces, dry back promptly obtains covering complete surface isolation layer at 1000 ℃ of sintering.
Embodiment 5:
It is raw material that carrier layer adopts 10 μ m SiC powder, adds 5wt%MgO-Al
2O
3-SiO
2As sintering aid, add the 0.2wt% TMAH as dispersant, the starch that adds 10wt% is mixed with the batch that total solid content is 80wt% as pore creating material with suitable quantity of water.The gained batch is adopted the vibrating casting moulding, and heating is solidified starch gelatinization in 75 ° of baking ovens.Dried base substrate slowly is heated to 600 ℃ and discharges starch in Muffle furnace, put into vacuum drying oven after the cooling, is warming up to 1700 ℃ of insulations and obtains carrier layer in 2 hours.
The intermediate layer select for use granularity be the SiC powder of 0.5 μ m as raw material, add the 0.7wt% TMAH as dispersant, be hybridly prepared into the suspension that solid content is 5wt% with the PVA solution of 1wt%.According to 0.5ml/cm
2Consumption, gained suspension evenly is coated in the carrier layer working surface, dry back exists, and slowly is warming up to 600 ℃ to discharge PVA wherein, is warming up to 1600 ℃ and be incubated 2 hours then under vacuum condition, obtains covering uniform intermediate layer.
With the xylene solution of Polycarbosilane, use compressed air spraying on the intermediate layer.Dry back is at H
2Obtain porous SiC surface isolation layer in 800 ℃ of pyrolysis under the/Ar mixed atmosphere.
Embodiment 6:
With the high purity aluminium oxide powder is raw material, adds water and is configured to 55% slurry.It is watered surface isolation layer at embodiment 1 gained mould, and suction time is 5 minutes, can obtain laminar wet base.The laminar biscuit of gained does not pollute, and dry back obtains the transparent alumina ceramics sheet after burning till through 1850 ℃ in 1000 ℃ Muffle furnace after the pre-burning again under hydrogen atmosphere.And the biscuit that obtains with gypsum mold, a small amount of gypsum that need fall wherein with dissolving with hydrochloric acid after pre-burning just can obtain the transparent alumina ceramics sheet.
Embodiment 7:
Yttrium-aluminium-garnet (YAG) powder with the coprecipitation preparation is a raw material, adds water and mixes, and makes 60% slurry.Pouring procedure can obtain sheet YAG biscuit with embodiment 6.Under vacuum, can obtain transparent YAG pottery in 3 hours through 1750 ℃ of insulations.
Embodiment 8:
The preparation of slurry is described with embodiment 6.With embodiment 2 gained multi-gradient porous alumina ceramics is mould, adopts the method for slip casing by pressure to prepare earthenware.Inhaled slurry 1.5 minutes under the pressure of 1.5MPa, and continued to discharge moisture 10 minutes in the wet base with the compressed air of 0.5MPa again, the demoulding can obtain semi-humid tubulose biscuit.Phenomenon such as die surface do not have adhesion, come off.After the wet base drying, after burning till according to the burning process of embodiment 6, obtain the transparent alumina pipe.
Mould after the demoulding need not to handle the cast that can carry out next time, and does not need the processing that repairs a die.Repeatedly use the back mold performance not change.
Claims (9)
1. ceramic grout moulding porous ceramics mould is characterized in that described porous ceramics mould is any in two kinds:
A. by carrier layer, one deck intermediate layer and surface isolation layer constitute at least, aperture is successively reduced to the surface isolation layer by carrier layer, forms asymmetric gradient and distributes;
B. constitute by carrier layer and surface isolation layer; Aperture forms asymmetric gradient by carrier layer to the surface isolation layer and distributes.
2. by the described ceramic grout moulding porous ceramics mould of claim 1, it is characterized in that:
1. the thickness of carrier layer is not less than 1mm; Pore-size distribution is at 1-100 μ m;
2. intermediate layer thickness≤500 μ m;
3. the aperture of surface isolation layer is less than 1 μ m; The thickness of surface isolation layer≤100 μ m.
3. make the method for ceramic grout moulding as claimed in claim 1 or 2, it is characterized in that making step is with the porous ceramics mould:
1) carrier layer of making porous ceramics;
2) working surface in carrier layer covers the intermediate layer;
3) in interlayer surfaces covering surfaces separating layer;
It is raw material less than the ceramic powder of 100 μ m that particle diameter is adopted in the making of described cellular ceramic substrate layer, and interpolation pore creating material, sintering aid, blowing agent form through forming and sintering;
Described intermediate layer makes, employed ceramic raw material particle size is between the particle size of carrier layer and surface isolation layer, ceramic powder, water, dispersant or binding agent are prefabricated into slurry, be coated in the working surface of carrier layer equably, obtain the semi-harden wet base substrate of one deck, burn till after the drying; The sintering temperature in intermediate layer is lower than the sintering temperature of carrier layer;
Described making in interlayer surfaces coating surface separating layer is to use ceramic powder, and particle diameter is less than the intermediate layer, and sintering temperature is lower than the sintering temperature in intermediate layer, adopts vapour deposition, plasma spraying or electroplating technology.
4. by the preparation method of the described ceramic grout moulding of claim 3 with the porous ceramics mould, it is characterized in that the porous ceramics mould of made is made of carrier layer and surface isolation layer when the feed particles size of carrier layer and the use of surface isolation layer differs less than 10 times.
5. by the preparation method of the described ceramic grout moulding of claim 3, it is characterized in that when carrier layer and the employed feed particles size of surface isolation layer differ by more than 200 times, should increasing one deck intermediate layer with the porous ceramics mould.
6. by the preparation method of the described ceramic grout moulding of claim 3, it is characterized in that behind the cellular ceramic substrate layer that step 1 is made, carrying out machining with the porous ceramics mould.
7. by the preparation method of the described ceramic grout moulding of claim 3 with the porous ceramics mould, the coated that it is characterized in that the intermediate layer is atomizing spray, high pressure painting, electrostatic spraying, dipping or brushing.
8. use the method for ceramic grout moulding as claimed in claim 1 or 2, it is characterized in that the aperture of surface isolation layer should be less than the size of the ceramic particle in the ceramic size of made with the porous ceramics mould.
9. by the using method of the described injection forming of claim 8, it is characterized in that the porous ceramics mould that is provided is applicable to aluminium oxide, yittrium oxide, magnesium aluminate spinel, yttrium-aluminium-garnet or zirconic injection forming with the porous ceramics mould.
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|---|---|---|---|
| CNA2007101719197A CN101181798A (en) | 2007-12-07 | 2007-12-07 | Multi-gradient porous ceramic mold for ceramic injection forming and making method |
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| CN101805175A (en) * | 2010-04-06 | 2010-08-18 | 九江学院 | Yttrium aluminum garnet porous ceramics and preparation method thereof |
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| CN102020470B (en) * | 2009-09-17 | 2013-03-13 | 中国科学院上海硅酸盐研究所 | Preparation method of transparent yttria ceramics with high optical quality |
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| CN101805175A (en) * | 2010-04-06 | 2010-08-18 | 九江学院 | Yttrium aluminum garnet porous ceramics and preparation method thereof |
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| CN106476293A (en) * | 2016-10-14 | 2017-03-08 | 九牧厨卫股份有限公司 | A kind of method that utilization master mold prepares high-pressure slip-casting shaping Working mould |
| CN106476293B (en) * | 2016-10-14 | 2019-03-01 | 九牧厨卫股份有限公司 | A method of high-pressure slip-casting molding Working mould is prepared using master mold |
| CN108261928A (en) * | 2018-01-26 | 2018-07-10 | 山东理工大学 | Pure silicon carbide ceramics membrane component and preparation method thereof |
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