CN113698225B - Ceramic load bearing board and preparation method thereof - Google Patents

Ceramic load bearing board and preparation method thereof Download PDF

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CN113698225B
CN113698225B CN202110988490.0A CN202110988490A CN113698225B CN 113698225 B CN113698225 B CN 113698225B CN 202110988490 A CN202110988490 A CN 202110988490A CN 113698225 B CN113698225 B CN 113698225B
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ceramic
slurry
powder
layer
pore
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CN113698225A (en
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詹海林
陈初升
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Chen Chusheng
University of Science and Technology of China USTC
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Abstract

The invention provides a ceramic setter plate and a preparation method thereof. The invention provides a ceramic setter plate, wherein a plate body comprises a gradient straight hole layer; the gradient straight hole layer comprises a plurality of gradient straight holes distributed in a honeycomb shape, the axial direction of the hole channel is the thickness direction of the plate body, and the aperture of each straight hole is changed along the axial direction in a gradient manner. The ceramic setter plate with the structure provided by the invention has the advantages of high porosity, good air permeability and mechanical strength meeting the application requirements.

Description

Ceramic load bearing board and preparation method thereof
Technical Field
The invention relates to the field of ceramics, in particular to a ceramic load bearing plate and a preparation method thereof.
Background
The co-fired ceramic technology which rises in recent years, including LTCC, MLCC and HTCC, is widely applied to the field of a plurality of military and civil ceramic functional devices due to the characteristics of low cost, multi-layer layout, light weight, high performance, high integration and the like of products. The porous backing plate is a base material which must be used in the co-firing and post-firing processes of the co-fired ceramic, and the porous backing plate is required to have high air permeability, small surface roughness and sufficient mechanical strength.
At present, the preparation process of the setter plate mainly comprises dry pressing molding (CN 101767991A), tape casting molding (CN 110330358A), casting molding (CN 103086737A) and the like. The preparation methods mainly provide pores in the setter plate by particle accumulation or adding pore-forming agents, pores produced by the method are difficult to ensure communication, so that the effect of high air permeability is difficult to achieve, and in addition, a large amount of pore-forming agents are added, so that the sintering difficulty of the product is increased, and the setter plate is not suitable for mass production. In order to meet the performance requirements, only special raw materials such as ceramic fibers can be selected, the characteristics of basic fibers are adopted, and the porosity of the fiber board is high, so that the air permeability is good, but the price of the fiber raw materials is high, and the mass production is not facilitated.
Disclosure of Invention
In view of this, the invention provides a ceramic setter plate and a method for manufacturing the same. The ceramic setter plate provided by the invention can effectively improve the porosity and mechanical strength of the setter plate.
The invention provides a ceramic setter plate, wherein a plate body comprises a gradient straight hole layer;
the gradient straight hole layer comprises a plurality of gradient straight holes distributed in a honeycomb shape, the axial direction of the hole channel is the thickness direction of the plate body, and the aperture of each straight hole is changed along the axial direction in a gradient manner.
Preferably, in the gradient straight hole, the size of each straight hole is independently selected from: the aperture of the thin end is 0.1-10 μm, the aperture of the thick end is 50-500 μm, and the length of the pore channel is 0.1-5 mm.
Preferably, the plate body comprises a gradient straight hole layer and a capillary hole layer;
the capillary hole layer comprises a plurality of capillary holes.
Preferably, in the capillary hole layer, the pore diameters of the plurality of capillaries are independently selected from: 0.1-80 μm.
Preferably, the plate body comprises a first plate body and a second plate body which are superposed and compounded;
the first plate body comprises a gradient straight hole layer;
the second plate body comprises a gradient straight hole layer and a capillary hole layer;
wherein the thin end surface in the gradient straight hole layer of the first plate body is in contact with the thin end surface in the gradient straight hole layer of the second plate body;
the thin end surface refers to the surface of the gradient straight hole layer close to the thin end of the straight hole.
The invention also provides a preparation method of the ceramic setter plate in the technical scheme, which comprises the following steps:
a) Preparing ceramic slurry A and sacrificial slurry XS;
the ceramic slurry A comprises the following components:
a ceramic raw material, wherein the ceramic raw material,
the mass of the binder accounts for 3-10 wt% of the mass of the ceramic raw material;
a dispersant, wherein the mass of the dispersant accounts for 0.5wt% -5 wt% of the mass of the ceramic raw material;
the pore-forming agent accounts for 5-30% of the volume of the ceramic raw material;
the mass of the solvent accounts for 30-60 wt% of the sum of the mass of the ceramic raw material and the mass of the pore-forming agent;
mixing a ceramic raw material, a binder, a dispersant, a pore-forming agent and a solvent to obtain ceramic slurry A;
the sacrificial slurry XS comprises the following components:
Figure BDA0003231506650000021
the sacrificial material is a powder material which can be discharged by sintering and is insoluble in the solvent;
mixing a sacrificial material, a binder, a dispersant and a solvent to obtain sacrificial slurry XS;
b) Tape casting:
carrying out double-layer tape casting on the ceramic slurry A and the sacrificial slurry XS to obtain a material belt
Figure BDA0003231506650000022
c) And (3) curing:
the material belt is
Figure BDA0003231506650000023
Placing in water for curing to obtain wet blank
Figure BDA0003231506650000024
d) Wet blank treatment:
for the wet blank
Figure BDA0003231506650000031
Drying and maintaining to obtain green body
Figure BDA0003231506650000032
e) And (3) sintering:
to the green body
Figure BDA0003231506650000033
Sintering to obtain a ceramic setter plate A;
in the obtained ceramic setter plate A, the plate body comprises a gradient straight hole layer.
The invention also provides a preparation method of the ceramic setter plate in the technical scheme, which comprises the following steps:
a) Preparing ceramic slurry A and ceramic slurry B;
the ceramic slurry B comprises the following components:
the ceramic raw material is prepared from a ceramic raw material,
the mass of the binder accounts for 3-10 wt% of the mass of the ceramic raw material;
a dispersant, wherein the mass of the dispersant accounts for 0.5-5 wt% of the mass of the ceramic raw material;
the volume of the pore-forming agent accounts for 5-30% of the volume of the ceramic raw material;
the mass of the solvent accounts for 30-60 wt% of the sum of the mass of the ceramic raw material and the mass of the pore-forming agent;
mixing a ceramic raw material, a binder, a dispersant, a pore-forming agent and a solvent to obtain ceramic slurry B;
b) Tape casting:
carrying out double-layer tape casting on the ceramic slurry A and the ceramic slurry B to obtain a material belt
Figure BDA0003231506650000034
c) And (3) curing:
the material belt is
Figure BDA0003231506650000035
Placing in water for curing to obtain wet blank
Figure BDA0003231506650000036
d) Wet blank treatment:
for the wet blank
Figure BDA0003231506650000037
Drying and maintaining to obtain green body
Figure BDA0003231506650000038
e) And (3) sintering:
to the green body
Figure BDA0003231506650000039
Sintering to obtain the ceramic setter plate
Figure BDA00032315066500000310
The obtained ceramic setter plate
Figure BDA00032315066500000311
The plate body comprises a gradient straight hole layer and a capillary hole layer.
Preferably, in the ceramic slurry a:
the ceramic raw material is ceramic powder and/or ceramic fiber;
the ceramic material is selected from one or more of alumina, zirconia, silica, titania, magnesia, kaolin, calcium carbonate, silicon carbide, talc, feldspar, cordierite, diatomite, mullite and boehmite;
the binder is selected from one or more of PESF, PES and PVB;
the dispersing agent is PVP and/or DSP;
the pore-forming agent is one or more of starch, graphite and wood chips;
the solvent is one or more selected from NMP, DMAc and DMSO.
Preferably, in the ceramic slurry B:
the ceramic raw material is ceramic powder and/or ceramic fiber;
the ceramic material is selected from one or more of alumina, zirconia, silica, titania, magnesia, kaolin, calcium carbonate, silicon carbide, talc, feldspar, cordierite, diatomite, mullite and boehmite;
the binder is selected from one or more of PESF, PES and PVB;
the dispersing agent is PVP and/or DSP;
the pore-forming agent is one or more of starch, graphite and wood chips;
the solvent is one or more selected from NMP, DMAc and DMSO.
Preferably, in the sacrificial slurry XS:
the sacrificial material is selected from one or more of graphite, starch and wood chips;
the binder is selected from one or more of PESF, PES and PVB;
the dispersing agent is PVP and/or DSP;
the solvent is one or more selected from NMP, DMAc and DMSO.
The ceramic setter plate provided by the invention has the advantages that the gradient straight holes distributed in a honeycomb shape are formed in the plate body, the axial direction of the pore channel is the thickness direction of the plate body, and the aperture of the straight holes changes along the axial gradient. The ceramic setter plate with the structure provided by the invention can effectively improve the porosity of the setter plate, the special pore structure can increase the air permeability of the setter plate, and the mechanical strength can meet the application requirements.
Experimental results show that the ceramic setter plate provided by the invention has the porosity of more than 55% and the air permeability of 8500m 3 /m 2 H.bar or more, and the three-point bending strength is 9.5MPa or more.
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In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a schematic cross-sectional structural view of a first ceramic setter plate according to the present invention;
FIG. 2 is a schematic perspective view of a first ceramic setter plate according to the present invention;
FIG. 3 is a schematic cross-sectional view of a second ceramic setter plate according to the present invention;
FIG. 4 is a schematic perspective view of a second ceramic setter plate according to the present invention;
FIG. 5 is a schematic cross-sectional view of a third ceramic setter plate according to the present invention;
FIG. 6 is a schematic perspective view of a third ceramic setter plate according to the present invention;
FIG. 7 is an optical microscope photograph of a cross section of the ceramic setter obtained in example 3;
FIG. 8 is a schematic view of the honeycomb surface of the ceramic setter plate obtained in example 3;
FIG. 9 is a schematic view of the smooth surface of the ceramic setter plate obtained in example 3;
FIG. 10 is a schematic cross-sectional view of a graded straight hole layer in a ceramic setter plate.
Detailed Description
The invention provides a ceramic setter plate, wherein a plate body comprises a gradient straight hole layer;
the gradient straight hole layer comprises a plurality of gradient straight holes distributed in a honeycomb shape, the axial direction of the hole channel is the thickness direction of the plate body, and the pore diameters of the straight holes are changed in a gradient manner along the axial direction.
Regarding the first ceramic setter plate provided by the present invention:
the invention provides a first ceramic setter plate, which comprises: a gradient straight orifice layer.
Referring to fig. 1 and fig. 2, fig. 1 is a schematic cross-sectional structure diagram of a first ceramic setter plate provided by the present invention, and fig. 2 is a schematic perspective structure diagram of the first ceramic setter plate provided by the present invention; the first ceramic setter plate structure is marked as type A. Wherein, 1 is a plate body, 101 is a gradient straight hole (101 a is a thin end, 101b is a thick end), 102 is a capillary hole, 103 is a first surface, and 104 is a second surface.
In the invention, the plate body of the ceramic setter plate comprises a gradient straight hole layer, and the gradient straight hole layer comprises a plurality of gradient straight holes which are distributed in a honeycomb shape. The gradient straight hole is a hollow tube structure (namely a communicating hole), the axial direction of the pore channel is the thickness direction of the plate body, and the aperture of the straight hole is changed along the axial gradient. The number of the gradient straight holes can be more than 1.
Wherein:
the gradient straight holes are distributed in a honeycomb shape, the axial direction of the pore channel is the thickness direction of the plate body, and the aperture of the straight holes changes along the axial gradient. In fig. 1-2, the gradient straight hole is only used to show the general shape of the gradient straight hole, and the sidewall thereof is relatively smooth, and in the actual product, the sidewall of the gradient straight hole is not completely smooth due to the straight hole structure formed by the reaction of the raw materials. Distribution of gradient straight holes referring to fig. 10, fig. 10 is a schematic cross-sectional view of a gradient straight hole layer in a ceramic setter plate, wherein black circles represent each gradient straight hole, and the gradient straight holes are distributed in a honeycomb shape.
In the plurality of gradient straight holes, the aperture of each straight hole changes in a gradient manner along the axial direction of the pore channel (namely the thickness direction of the plate body), namely, the aperture of each straight hole changes in a gradient manner from the upper surface to the lower surface of the plate body (the upper surface and the lower surface are not limited by special directions, one surface is the upper surface, and the other surface is naturally the lower surface). The gradient can be gradually increased or decreased, for example, the aperture diameter of each straight hole is gradually increased from the first surface to the second surface along the thickness direction of the plate body; if the direction from the second surface to the first surface is reversed, the aperture of each straight hole is gradually reduced.
The gradient straight holes have gradient pore diameters, so that each gradient straight hole comprises a thin end and a thick end, which is shown in fig. 1, wherein 101a is the thin end, and 101b is the thick end. In the present invention, the size of each of the plurality of gradient straight holes is independently selected from: the aperture of the thin end is 0.1-10 μm, the aperture of the thick end is 50-500 μm, and the length of the pore channel is 0.1-5 mm. In the invention, the plate body of the ceramic setter plate comprises a first surface and a second surface, wherein the gradient straight hole penetrates through the two surfaces, but the gradient straight hole penetrates through the two surfaces in a microscopic view because the aperture of the gradient straight hole is smaller, but holes cannot be seen by naked eyes on the upper surface and the lower surface of the plate body in a macroscopic view, and the plate body is still a compact plate body.
In the present invention, the gradient straight-hole layer further includes a plurality of capillary holes, see fig. 1 and 2, wherein 102 is a capillary hole. The capillary holes are distributed in the matrix space except for the gradient straight holes, such as being sandwiched between the gradient straight holes. In the invention, the pore diameter of each capillary pore is independently selected from 0.1-80 μm.
In the invention, the thickness of the plate body of the first ceramic setter plate is preferably 0.5-5 mm.
Regarding the second ceramic setter plate provided by the present invention:
the invention provides a second ceramic setter plate, which comprises: gradient straight pore layer and capillary pore layer.
Referring to fig. 3 and 4, fig. 3 is a schematic cross-sectional structure diagram of a second ceramic setter plate provided by the present invention, and fig. 4 is a schematic perspective structure diagram of the second ceramic setter plate provided by the present invention; the second ceramic setter plate structure is marked as
Figure BDA0003231506650000061
And (4) molding. Wherein 2 is a plate body, 2-z is a gradient straight hole layer, 2-m is a capillary hole layer, 201 is a gradient straight hole, 202z and 202m are capillary holes, 203 is a first surface, and 204 is a second surface.
In fig. 3-4, the dashed line is used as a boundary, the gradient straight pore layer is above the dashed line, and the capillary pore layer is below the dashed line. Wherein, the structure and the straight hole size of the gradient straight hole layer 2-z are the same as those in the first ceramic setter plate in the above technical solution, and are not described herein again.
In the present invention, the capillary-type pores 2-m are only contained, and gradient straight-hole-type pores are not contained. In the invention, in the capillary hole layers 2-m, the pore diameters of a plurality of capillary holes 202m are independently selected from: 0.1-80 μm.
In the invention, in the second ceramic setter plate, the total thickness of the plate body is 0.5-5 mm; wherein, the thickness of the gradient straight hole layer accounts for 10 to 90 percent of the total thickness of the plate body.
Regarding the third ceramic setter plate provided by the present invention:
the third ceramic setter plate provided by the invention comprises: the first plate body and the second plate body.
Referring to fig. 5 and 6, fig. 5 is a schematic cross-sectional structure diagram of a third ceramic setter plate provided by the present invention, and fig. 6 is a schematic perspective structure diagram of the third ceramic setter plate provided by the present invention; the third ceramic setter plate structure is marked as
Figure BDA0003231506650000071
And (4) molding. 1 is a first plate body, 101 is a gradient straight hole, 102 is a capillary hole, 103 is a first surface of the first plate body, and 104 is a second surface of the first plate body; 2 is a second plate body, 2-z is a gradient straight hole layer, 2-m is a capillary hole layer, 201 is a gradient straight hole, 202z and 202m are capillary holes, 203 is a first surface of the second plate body, and 204 is a second surface of the second plate body.
In the present invention, the first plate body includes a graded straight bore layer. The structure, the size of the straight hole, the thickness of the plate body and the like of the gradient straight hole layer are the same as those of the first ceramic setter plate in the technical scheme, and are not described in detail herein.
In the invention, the second plate body comprises a gradient straight hole layer and a capillary hole layer. The structures, the sizes and the like of the gradient straight hole layer and the capillary hole layer in the second plate body are consistent with those of the second ceramic setter plate in the technical scheme, and are not described again.
In the invention, the thin end surface in the gradient straight hole layer of the first plate body is contacted with the thin end surface in the gradient straight hole layer of the second plate body; wherein, the thin end surface refers to the side of the gradient straight hole layer close to the thin end of the straight hole. Referring to fig. 5-6, the first surface 103 of the first plate is in contact with the first surface 203 of the second plate.
With respect to other ceramic setter plates provided by the present invention:
the invention also provides another ceramic setter plate, comprising: two first ceramic setter plates; wherein the thin end surfaces in the gradient straight hole layers of the two first ceramic setter plates are in contact.
The invention also provides another ceramic setter plate, comprising: two second ceramic setter plates; wherein the thin end surfaces in the gradient straight hole layers of the two second ceramic burning bearing plates are contacted.
The invention also provides other ceramic setter plates, comprising: at least one of the two plate bodies comprises a gradient straight hole layer; the structure of the gradient straight hole layer is the same as that in the foregoing technical solution, and is not described herein again.
The ceramic setter plate provided by the invention has the advantages that a gradient straight hole structure is formed in the plate body, a plurality of gradient straight holes are distributed in a honeycomb shape, the axial direction of a pore passage is the thickness direction of the plate body, and the pore diameter of each straight hole is changed along the axial direction in a gradient manner. The ceramic setter plate with the structure provided by the invention can effectively improve the porosity of the setter plate, and the special hole structure is an effective hole capable of increasing the air permeability, so that the air permeability of the setter plate can be effectively improved, and the mechanical strength of the ceramic setter plate can be improved.
The invention provides a preparation method of a first ceramic setter plate (namely, A type) in the technical scheme, which comprises the following steps:
a) Preparing ceramic slurry A and sacrificial slurry XS;
the sacrificial slurry XS comprises the following components:
Figure BDA0003231506650000081
the sacrificial material is a powder material which can be discharged by sintering and is insoluble in the solvent;
mixing a sacrificial material, a binder, a dispersant and a solvent to obtain sacrificial slurry XS;
b) Tape casting:
carrying out double-layer tape casting on the ceramic slurry A and the sacrificial slurry XS to obtain a material belt
Figure BDA0003231506650000082
c) And (3) curing:
the material belt is
Figure BDA0003231506650000083
Placing in water for curing to obtain wet blank
Figure BDA0003231506650000084
d) Wet blank treatment:
for the wet blank
Figure BDA0003231506650000085
Curing to obtain a green body
Figure BDA0003231506650000086
e) And (3) sintering:
to the green body
Figure BDA0003231506650000087
Sintering to obtain a ceramic setter plate A;
in the obtained ceramic setter plate A, the plate body comprises a gradient straight hole layer.
With respect to step a): ceramic slurry a and sacrificial slurry XS were prepared.
The raw material composition and the preparation method of the ceramic slurry a are the same as those in the foregoing technical solutions, and are not described in detail here.
The sacrificial slurry XS comprises the following components: sacrificial materials, binders, dispersants, and solvents.
Wherein:
the sacrificial material is a powder material which can be discharged through sintering and is insoluble in the solvent, and the powder material is organic powder and/or inorganic powder. The sacrificial material is preferably one or more of graphite, starch and wood chips. The content of the sacrificial material is 30wt% -60 wt%.
The binder is preferably one or more of PESF (i.e., polyphenylene ether sulfone), PES (i.e., polyether sulfone) and PVB (i.e., polyvinyl butyral). In the invention, the content of the binder is 3-10 wt%.
The dispersant is preferably PVP (i.e. polyvinylpyrrolidone) and/or DSP (i.e. modified fish oil). In the invention, the content of the dispersant is 1wt% -5 wt%.
The solvent is selected from NMP (i.e., N-methylpyrrolidone), DMAc (i.e., dimethyl ethyl phthalein amine)
) And DMSO (i.e., dimethyl sulfoxide), more preferably NMP (i.e., N-methylpyrrolidone). In the invention, the content of the solvent is 30-60 wt%.
The invention is not particularly limited in the manner of making the above components into slurry, and it is sufficient to make the slurry according to the conventional pulping manner in the art, specifically, the sacrificial material, the binder, the dispersant and the solvent are mixed to obtain the sacrificial slurry XS. In the present invention, the mixing is preferably performed by ball milling. The rotation speed of the ball mill is preferably 25-50 rpm. The time for ball milling is preferably 10 to 20 hours. And (4) carrying out mixing treatment to obtain uniform sacrificial slurry XS.
With respect to step b): and (4) tape casting.
Carrying out double-layer tape casting on the ceramic slurry A and the sacrificial slurry XS to obtain a material belt
Figure BDA0003231506650000091
In the double-layer casting, the height of a front cutter and the height of a rear cutter of a casting cutter are respectively adjusted, and then slurry is added for casting forming. In the invention, preferably, the ceramic slurry A is added between the front and back parts and the back knife, and the sacrificial slurry XS is added behind the back knife, so as to obtain the composite material belt with the ceramic slurry layer A on the upper part and the sacrificial slurry XS on the lower part
Figure BDA0003231506650000092
The height between the front cutter and the rear cutter corresponds to the thickness of the ceramic slurry layer A, and the height of the rear cutter corresponds to the thickness of the sacrificial slurry layer XS.
In the present invention, the thickness of the ceramic A layer is preferably 2 to 3mm, and the thickness of the XS layer (i.e., the sacrificial layer) is preferably 0.1 to 0.5mm.
With respect to step c): and (5) curing.
The material belt is
Figure BDA0003231506650000093
Placing in water for curing to obtain wet blank
Figure BDA0003231506650000094
The invention has no special limit on the using amount of the water and can completely submerge the material belt
Figure BDA0003231506650000095
And (4) finishing. The time for curing in water is preferably 5 to 20 hours. The principle of forming the gradient straight-hole structure by solidification in water is consistent with the foregoing description, and is not repeated herein. Wherein, the material belt
Figure BDA0003231506650000096
The invention controls the compositions of the slurry to be the ceramic slurry A and the sacrificial slurry XS shown in the specification, and simultaneously controls the curing process and parameters as follows: the material belt is arranged along the thickness direction of the plate body
Figure BDA0003231506650000097
Vertically and stably put into water until the material belt is put into
Figure BDA0003231506650000101
Completely immersed in water, wherein the sacrificial layer XS is arranged below and the slurry A layer is arranged above (namely the depth of the sacrificial layer XS in the water is deeper), the temperature of the water is 5-30 ℃, and the curing time is 5-20 h. Preferably, the temperature of the water is 15 ℃. In some embodiments, the volume ratio of water to all solvent contained in the tape is 80: 1, but is not so limited.
After the solidification treatment, the upper part of the plate body (corresponding to the layer A of the ceramic slurry) forms a straight hole structure, and the aperture changes in a gradient manner from one end of the straight hole to the other end; the lower part of the plate body corresponds to the sacrificial layer XS, and the internal structure of the sacrificial layer is porous and spongy. Curing and forming to obtain a wet blank
Figure BDA0003231506650000102
In the ceramic layer A, one surface far away from the sacrificial slurry XS layer corresponds to the thin end of the gradient straight hole, and the surface in contact with the sacrificial slurry XS layer corresponds to the thick end of the gradient straight hole.
With respect to step d): and (5) wet blank treatment.
For the wet blank
Figure BDA0003231506650000103
Drying and maintaining to obtain green body
Figure BDA0003231506650000104
In the invention, before airing and maintaining, the target product is preferably cut into a certain shape and size, and then airing and maintaining are carried out. In the present invention, the conditions for drying and maintaining are preferably as follows: the temperature is 10-35 ℃, the relative humidity is 20-80%, and the time is 10-40 h. By the above treatment, a green compact is obtained
Figure BDA0003231506650000105
With respect to step e): and (5) sintering.
To the green body
Figure BDA0003231506650000106
Sintering to obtain the ceramic setter plate A. In the present invention, the sintering preferably includes: the first heating, the glue discharging and the second heating. The first temperature raising condition is preferably: the heating rate is preferably 1-5 ℃/min, the target temperature is preferably 600-800 ℃, and the heat preservation time is preferably 1-5 h. After the first temperature rise treatment, the glue is discharged, and then the second temperature rise treatment is carried out. The second temperature rise condition is preferably: the heating rate is preferably 3-10 ℃/min, the target temperature is preferably 1300-1500 ℃, and the heat preservation time is preferably 2-10 h. After the sintering treatment, the sacrificial layer (i.e., XS layer) is sintered away, and the ceramic setter plate A is obtained.
In the ceramic setter plate a, the plate body includes the gradient straight hole layer, corresponding to the structure of the first ceramic setter plate in the above technical solution, as shown in fig. 1-2, wherein the gradient straight hole penetrates through the two surfaces, but the gradient straight hole penetrates through the two surfaces microscopically because the aperture of the gradient straight hole is small, but the holes cannot be seen by naked eyes on the upper and lower surfaces of the plate body from a macroscopic product, but the plate body is compact, but in the second preparation method, the sacrificial layer is introduced first and then sintered, so that a rough surface is formed on the sacrificial layer removal surface (i.e., the surface where the coarse end of the gradient straight hole is located in the ceramic setter plate a), that is, the surface where the coarse end of the straight hole is located is a rough honeycomb surface in appearance (see fig. 8), and the surface where the fine end of the straight hole is located is a smooth surface in appearance (see fig. 9).
The invention also provides a second ceramic setter plate (namely, the second ceramic setter plate) in the technical scheme
Figure BDA0003231506650000107
Form (b) comprising the steps of:
a) Preparing ceramic slurry A and ceramic slurry B;
the ceramic slurry B comprises the following components:
the ceramic raw material is prepared from a ceramic raw material,
the mass of the binder accounts for 3-10 wt% of the mass of the ceramic raw material;
a dispersant, wherein the mass of the dispersant accounts for 0.5wt% -5 wt% of the mass of the ceramic raw material;
the pore-forming agent accounts for 5-30% of the volume of the ceramic raw material;
the mass of the solvent accounts for 30-60 wt% of the sum of the mass of the ceramic raw material and the mass of the pore-forming agent;
mixing a ceramic raw material, a binder, a dispersant, a pore-forming agent and a solvent to obtain ceramic slurry B;
b) Tape casting:
carrying out double-layer tape casting on the ceramic slurry A and the ceramic slurry B to obtain a material belt
Figure BDA0003231506650000111
c) And (3) curing:
the material belt is
Figure BDA0003231506650000112
Placing in water for curing to obtain wet blank
Figure BDA0003231506650000113
d) Wet blank treatment:
for the wet blank
Figure BDA0003231506650000114
Drying and maintaining to obtain green body
Figure BDA0003231506650000115
e) And (3) sintering:
to the green body
Figure BDA0003231506650000116
Sintering to obtain the ceramic setter plate
Figure BDA0003231506650000117
The obtained ceramic setter plate
Figure BDA0003231506650000118
In, the plate body includes gradient straight hole layer and capillary pore layer.
With respect to step a): ceramic slurry a and ceramic slurry B were prepared.
The raw material composition and the preparation method of the ceramic slurry a are the same as those in the foregoing technical solutions, and are not described in detail here.
In the invention, the ceramic slurry B comprises the following components: ceramic raw materials, a binder, a dispersant, a pore-forming agent and a solvent.
Wherein:
the ceramic raw material is ceramic powder and/or ceramic fiber. Wherein, the ceramic material is preferably one or more of alumina, zirconia, silica, titania, magnesia, kaolin, calcium carbonate, silicon carbide, talc, feldspar, cordierite, diatomite, mullite and boehmite.
The binder is preferably one or more of PESF (i.e., polyphenylene ether sulfone), PES (i.e., polyether sulfone), and PVB (i.e., polyvinyl butyral). In the present invention, the binder is preferably present in an amount of 3 to 10wt% based on the mass of the ceramic raw material.
The dispersant is preferably PVP (i.e. polyvinylpyrrolidone) and/or DSP (i.e. modified fish oil). In the present invention, the dispersant preferably accounts for 0.5wt% to 5wt% of the mass of the ceramic raw material.
The pore-forming agent is preferably one or more of starch, graphite and wood chips. In the present invention, it is preferable that the volume of the pore-forming agent is 5% to 30% of the volume of the ceramic raw material.
The solvent is selected from NMP (i.e., N-methylpyrrolidone), DMAc (i.e., dimethyl ethyl phthalein amine)
) And DMSO (i.e., dimethyl sulfoxide), more preferably NMP (i.e., N-methylpyrrolidone). In the present invention, the solvent preferably accounts for 30wt% to 60wt% of the mass of the ceramic raw material.
The invention has no special limitation on the mode of preparing the components into the slurry, and the ceramic slurry B can be obtained by mixing the ceramic raw material, the binder, the dispersant, the pore-forming agent and the solvent according to the conventional pulping mode in the field. Preferably, the ceramic raw material, the dispersant, the pore-forming agent and the solvent are uniformly mixed, and then the binder is added and continuously and uniformly mixed. In the present invention, the mixing is preferably performed by ball milling. The rotation speed of the ball mill is preferably 25-50 rpm. The ball milling time is preferably 14-30 h, wherein the ball milling time is preferably 4-10 h before the binder is added, and the ball milling time is preferably 10-20 h after the binder is added. And (3) carrying out mixing treatment to obtain uniform ceramic slurry B.
According to the component introduction, the component types and specific selection ranges of the components of the ceramic slurry A and the ceramic slurry B are the same, and when the ceramic slurry A and the ceramic slurry B are simultaneously adopted, the components of the same type are independently selected from the corresponding selection ranges, namely the ceramic slurry A and the ceramic slurry B can be the same or different. When the ceramic slurry A and the ceramic slurry B are the same (namely, only one slurry is adopted), a single-layer tape casting can be carried out to prepare the material belt, and a structure comprising a gradient straight hole layer and a capillary hole layer can be formed in subsequent solidification.
With respect to step b): and (4) tape casting.
Carrying out double-layer tape casting on the ceramic slurry A and the ceramic slurry B to obtain a material belt
Figure BDA0003231506650000121
In the double-layer casting, the height of a front cutter and the height of a rear cutter of a casting cutter are respectively adjusted, and then slurry is added for casting forming. In the present invention, it is preferable that the ceramic slurry A is fed between the front and rear blades and the rear blade, and the ceramic slurry B is fed behind the rear blade, thereby obtaining a composite tape in which the ceramic slurry layer A is on the upper side and the ceramic slurry layer B is on the lower side
Figure BDA0003231506650000122
Wherein, the height between the front cutter and the rear cutter corresponds to the thickness of the ceramic A layer, and the height of the rear cutter corresponds to the thickness of the ceramic B layer.
In the present invention, the thickness of the ceramic layer A is preferably 2 to 4mm, and the thickness of the ceramic layer B is preferably 0.1 to 0.5mm.
With respect to step c): and (5) curing.
The material belt is
Figure BDA0003231506650000131
Placing in water for curing to obtain wet blank
Figure BDA0003231506650000132
The invention has no special limit on the using amount of the water and can completely submerge the material belt
Figure BDA0003231506650000133
And (4) finishing. The time for curing in water is preferably 10 to 20 hours. The principle of forming gradient straight hole layer and capillary hole layer by solidification in water and the above-mentioned oneDuring the process of curing the material belt in water, the phase-inversion slurry is contacted with water, the water enters the slurry to generate a viscosity finger-entering phenomenon, and the entry of the water simultaneously causes the thermodynamic equilibrium of a binder and a solvent in the slurry to be greatly broken, so that phase separation is generated; the finger-like pore layer is formed when viscous fingering dominates, and the capillary structure dominates when phase separation dominates. Specifically, in the phase inversion process, water exchanges with the solvent in the slurry, the binder gradually precipitates from the solvent, the ceramic powder in the slurry is driven to rearrange, meanwhile, the slurry gradually gels, the gelling time is short, the advancing speed of the gel front is high, the concentration of the polymer (namely the binder in the slurry) is low, the membrane tends to form a finger-shaped macroporous structure, and in the later curing period, the gelling time is long, the advancing speed of the gel front is low, the concentration of the polymer is high, and the membrane tends to form a spongy structure with only capillary pores.
For the material belt
Figure BDA0003231506650000134
The invention controls the compositions of the slurry to be the ceramic slurry A and the ceramic slurry B shown in the specification, and simultaneously controls the curing process and parameters as follows: the material belt is arranged along the thickness direction of the plate body
Figure BDA0003231506650000135
Vertically and stably put into water until the material belt is put into
Figure BDA0003231506650000136
Completely immerging in water, wherein the slurry B layer is below and the slurry A layer is above (namely the depth of the slurry B layer in the water is deeper), the temperature of the water is 5-30 ℃, and the curing time is 5-20 h. Preferably, the temperature of the water is 15 ℃. In some embodiments, the volume ratio of water to all solvent contained in the tape is 80: 1, but is not so limited. After the curing treatment, the upper part of the plate body (corresponding to the layer A of the ceramic) forms a straight hole structure, and the aperture changes in a gradient manner from one end of the straight hole to the other end; the lower part of the plate body (i.e. corresponding to the ceramic layer B) forms a capillary structure. Curing and forming to obtain a wet blank
Figure BDA0003231506650000137
In the ceramic layer A, one surface far away from the ceramic layer B corresponds to the thin end of the gradient straight hole, and the surface in contact with the ceramic layer B corresponds to the thick end of the gradient straight hole.
If a plurality of material belts are simultaneously cured (namely, a batch of material belts are simultaneously cured) in the same container, when a plurality of material belts are required to be stacked, the distance between two adjacent material belts is required to be controlled to be not less than 20mm; specifically, multiple layers of partition plates can be arranged in the container, the material belts are arranged on the partition plates on different layers, and the distance between the different material belts is controlled through the installation height of the partition plates.
With respect to step d): and (5) wet blank treatment.
For the wet blank
Figure BDA0003231506650000138
Drying and maintaining to obtain green body
Figure BDA0003231506650000139
In the invention, before airing and maintaining, the target product is preferably cut into a certain shape and size, and then airing and maintaining are carried out. In the present invention, the conditions for drying and maintaining are preferably as follows: the temperature is 10-35 ℃, the relative humidity is 20-80%, and the time is 10-40 h. By the above treatment, a green compact is obtained
Figure BDA00032315066500001310
With respect to step e): and (4) sintering.
To the green body
Figure BDA00032315066500001311
Sintering to obtain the ceramic setter plate
Figure BDA00032315066500001312
In the present invention, the sintering preferably includes: the first heating, the glue discharging and the second heating. The first temperature raising condition is preferably: the heating rate is preferably 1-3 ℃/min, the target temperature is preferably 600-800 ℃, and the heat preservation time is preferably 1-5 h.After the first temperature rise treatment, the glue is discharged, and then the second temperature rise treatment is carried out. The second temperature rise condition is preferably: the heating rate is preferably 3-10 ℃/min, the target temperature is preferably 1300-1500 ℃, and the heat preservation time is preferably 2-10 h. After the sintering treatment, the ceramic setter plate is obtained
Figure BDA0003231506650000141
Namely a composite plate body with a ceramic layer A at the upper part and a ceramic layer B at the lower part
Figure BDA0003231506650000142
In the ceramic layer A, one surface far away from the ceramic layer B corresponds to the thin end of the gradient straight hole, and the surface in contact with the ceramic layer B corresponds to the thick end of the gradient straight hole.
The ceramic load bearing plate
Figure BDA0003231506650000143
In, the plate body includes straight hole layer of gradient and capillary pore layer, corresponds the structure of the second kind of pottery bearingburning board among the above-mentioned technical scheme.
The invention also provides a third ceramic load bearing plate (namely, a third ceramic load bearing plate) in the technical scheme
Figure BDA0003231506650000144
Form (la) comprising the steps of:
a) Preparation of Wet Green A and Wet Green A, respectively
Figure BDA0003231506650000145
b) Green body treatment:
mixing the wet blank A and the wet blank
Figure BDA0003231506650000146
Stacking and pressing to obtain a composite green body
Figure BDA0003231506650000147
Wherein, during the stacking process, the fine in the gradient straight hole layer in the wet blank AEnd surface and the wet blank
Figure BDA0003231506650000148
The thin end surfaces in the middle gradient straight hole layer are contacted;
c) And (3) sintering:
to the composite green body
Figure BDA0003231506650000149
Sintering to obtain the ceramic setter plate
Figure BDA00032315066500001410
With respect to step a):
in the present invention, a wet green A and a wet green are prepared
Figure BDA00032315066500001411
The preparation method is the same as that in the above technical scheme, and is not described in detail herein.
With respect to step b):
before stacking, preferably, the two wet blanks are cut, dried and maintained. Wherein, the conditions of the drying and maintenance are the same as those in the above technical scheme, and are not repeated herein. After the above treatment, the two wet blanks are stacked.
During the stacking process, the thin end surface in the gradient straight hole layer in the wet blank A and the wet blank
Figure BDA00032315066500001412
The thin end surfaces in the middle gradient straight hole layer are contacted; in practice, two wet blanks are stacked in contact with the surfaces facing upward in the flow time (i.e., the side of the wet blank a in contact with the doctor blade front and the side of the wet blank a in contact with the doctor blade rear).
And pressing after the overlapping. In the invention, the pressing temperature is preferably 50-80 ℃. The pressure of the pressing is preferably 500 to 1000Psi. The pressure maintaining time of the pressing is preferably 0.5-5 min. And pressing to obtain the composite green body.
With respect to step c):
in the present invention, the sintering preferably includes: the first heating, the glue discharging and the second heating. The first temperature raising condition is preferably: the heating rate is preferably 1-3 ℃/min, the target temperature is preferably 600-800 ℃, and the heat preservation time is preferably 1-5 h. After the first temperature rise treatment, the glue is discharged, and then the second temperature rise treatment is carried out. The second temperature rise condition is preferably: the heating rate is preferably 3-10 ℃/min, the target temperature is preferably 1300-1500 ℃, and the heat preservation time is preferably 2-10 h. After the sintering treatment, the ceramic setter plate is obtained
Figure BDA0003231506650000151
Namely a first plate body (ceramic A) on the upper and a second plate body (ceramic)
Figure BDA0003231506650000152
) Composite plate body under
Figure BDA0003231506650000153
Wherein, one surface of the first plate body (ceramic A) corresponding to the thin end of the gradient straight hole is corresponding to the second plate body (ceramic
Figure BDA0003231506650000154
) The surfaces corresponding to the thin ends of the middle gradient straight holes are contacted.
The ceramic load bearing plate
Figure BDA0003231506650000155
The ceramic setter plate comprises a first plate body and a second plate body, and corresponds to the structure of the third ceramic setter plate in the technical scheme.
The invention also provides a preparation method of other ceramic setter plates in the technical scheme, which is carried out on the basis of the preparation methods of the first ceramic setter plate to the third ceramic setter plate, and the preparation process of the ceramic setter plates is referred to, and the individual steps are correspondingly adjusted according to the structural composition of the target ceramic setter plate.
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the invention, and not to limit the scope of the claims. In the following examples, the particle size of the ceramic powder was 1 to 100. Mu.m.
Example 1: preparing a ceramic setter plate A (as shown in figure 1-2)
S1, preparing ceramic slurry A and sacrificial layer slurry XS:
(1) Ceramic slurry A raw material:
ceramic powder: 80wt% of alumina fine powder, 10wt% of silica fine powder, 5wt% of kaolin fine powder and 5wt% of titanium oxide fine powder;
adhesive: polyvinyl butyral (PVB) accounting for 7.5wt% of the ceramic powder;
dispersing agent: polyvinylpyrrolidone accounting for 1.5wt% of the ceramic powder;
pore-forming agent: graphite with a median particle size D50 of 35 μm, the volume of which accounts for 15% of the volume of the ceramic powder;
solvent: n-methyl-2-pyrrolidone NMP accounts for 48wt% of the total mass of the ceramic powder and the pore-forming agent.
Preparation of ceramic slurry A: mixing and ball-milling the ceramic powder, the pore-forming agent, the dispersing agent and the solvent for 5 hours, adding the binder, and continuing ball-milling for 15 hours to obtain ceramic slurry A.
(2) Sacrificial layer slurry XS raw material:
Figure BDA0003231506650000156
Figure BDA0003231506650000161
preparation of sacrificial slurry XS: and mixing the sacrificial material, the dispersing agent, the binder and the solvent, and performing ball milling for 20 hours to obtain sacrificial slurry XS.
S2, tape casting:
double-layer casting: the height of the front cutter of the casting cutter is adjusted to 2.5mm, the height of the rear cutter is adjusted to 0.3mm, sacrificial slurry XS is added behind the rear cutter,adding ceramic slurry A between the front cutter and the rear cutter, and performing casting to obtain the material belt
Figure BDA0003231506650000162
S3, curing:
feeding belt
Figure BDA0003231506650000163
Placing in water for curing for 15h, specifically: the material belt is arranged along the thickness direction of the plate body
Figure BDA0003231506650000164
Vertically and stably put into water until the material belt is put into
Figure BDA0003231506650000165
Completely immersed in water with the sacrificial layer XS layer below and the slurry A layer above (i.e., deeper depth of the sacrificial layer XS in water), the temperature of the water being 15 deg.C, the water and the tape
Figure BDA0003231506650000166
The volume ratio of all solvents contained in the mixture is 80: 1, and the mixture is solidified for 15 hours to obtain a wet blank
Figure BDA0003231506650000167
S4, green body treatment:
the wet blank is processed
Figure BDA0003231506650000168
Cutting into certain shape and size, air drying at 30 deg.C and 60% relative humidity for 30 hr to obtain green body
Figure BDA0003231506650000169
S5, sintering:
mixing the green body
Figure BDA00032315066500001610
Heating to 800 deg.C at a rate of 1 deg.C/min, maintaining for 2 hr, removing glue, and heating to 3 deg.CAnd heating to 1450 ℃ at a rate of/min, and preserving the temperature for 5h, wherein the sacrificial layer XS is burnt off, so as to obtain the ceramic setter plate A. The structure of the resulting product is shown in fig. 1-2.
Example 2: preparing ceramic load bearing board
Figure BDA00032315066500001611
(as shown in FIGS. 3-4)
S1, preparing ceramic slurry A and ceramic slurry B;
(1) Ceramic slurry A raw material:
ceramic powder: 60wt% of mullite fine powder, 20wt% of white corundum powder, 15wt% of boehmite fine powder, 3.5wt% of kaolin fine powder and 1.5wt% of calcium carbonate powder;
adhesive: polyvinyl butyral PVB accounting for 7.5wt% of the ceramic powder;
dispersing agent: polyvinylpyrrolidone accounting for 1.7wt% of the mass of the ceramic powder;
pore-forming agent: graphite with a median particle size D50 of 35 μm, the volume of which accounts for 10% of the volume of the ceramic powder;
solvent: n-methyl-2-pyrrolidone NMP accounts for 40wt% of the total mass of the ceramic powder and the pore-forming agent.
Preparation of ceramic slurry A: mixing and ball-milling the ceramic powder, the pore-forming agent, the dispersing agent and the solvent for 5 hours, adding the binder, and continuing ball-milling for 15 hours to obtain ceramic slurry A.
(2) Ceramic slurry B raw materials:
ceramic powder: 80wt% of alumina fine powder, 10wt% of silica fine powder, 5wt% of kaolin fine powder and 5wt% of titanium oxide fine powder;
adhesive: polyvinyl butyral PVB accounting for 7.5wt% of the ceramic powder;
dispersing agent: polyvinylpyrrolidone accounting for 1.5wt% of the ceramic powder;
pore-forming agent: graphite, wherein the median particle size D50 is 35 mu m, and the volume of the graphite accounts for 15 percent of the volume of the ceramic powder;
solvent: n-methyl-2-pyrrolidone NMP accounts for 48wt% of the total mass of the ceramic powder and the pore-forming agent.
Preparation of ceramic slurry B: mixing and ball-milling the ceramic powder, the pore-forming agent, the dispersing agent and the solvent for 5 hours, adding the binder, and continuing ball-milling for 15 hours to obtain ceramic slurry B.
S2, tape casting:
double-layer casting: adjusting the height of a front cutter of a casting cutter to 3mm, adjusting the height of a rear cutter to 0.3mm, adding ceramic slurry B behind the rear cutter, adding ceramic slurry A between the front cutter and the rear cutter, and casting to obtain the material belt
Figure BDA0003231506650000171
S3, curing:
feeding belt
Figure BDA0003231506650000172
Placing in water for curing for 10 hours, specifically: the material belt is arranged along the thickness direction of the plate body
Figure BDA0003231506650000173
Vertically and stably put into water until the material belt is put into
Figure BDA0003231506650000174
Completely immersed in water, wherein slurry B layer is below and slurry A layer is above (i.e. the depth of slurry B layer in water is deeper), the temperature of water is 15 ℃, and water and the material belt
Figure BDA0003231506650000175
The volume ratio of all solvents contained in the mixture is 80: 1, and the mixture is solidified for 10 hours to obtain a wet blank
Figure BDA0003231506650000176
S4, green body treatment:
the wet blank is processed
Figure BDA0003231506650000177
Cutting into certain shape and size, air drying at 20 deg.C and 60% relative humidity for 30 hr to obtain green body
Figure BDA0003231506650000178
S5, sintering:
mixing the green body
Figure BDA0003231506650000179
Heating to 800 deg.C at a rate of 1 deg.C/min, maintaining for 2 hr, removing glue, heating to 1450 deg.C at a rate of 3 deg.C/min, and maintaining for 5 hr to obtain ceramic setter plate
Figure BDA00032315066500001710
The structure of the resulting product is shown in fig. 3-4.
Example 3: preparation of ceramic setter plate A-A
S1, preparing ceramic slurry A and sacrificial layer slurry XS:
(1) Ceramic slurry A raw material:
ceramic powder: 80wt% of alumina fine powder, 10wt% of silica fine powder, 5wt% of kaolin fine powder and 5wt% of titanium oxide fine powder;
adhesive: polyvinyl butyral PVB accounting for 7.5wt% of the ceramic powder;
dispersing agent: polyvinylpyrrolidone accounting for 1.5wt% of the ceramic powder;
pore-forming agent: graphite with a median particle size D50 of 35 μm, the volume of which accounts for 15% of the volume of the ceramic powder;
solvent: n-methyl-2-pyrrolidone NMP accounts for 48wt% of the total mass of the ceramic powder and the pore-forming agent.
Preparation of ceramic slurry A: mixing and ball-milling the ceramic powder, the pore-forming agent, the dispersing agent and the solvent for 5 hours, adding the binder, and continuing ball-milling for 15 hours to obtain ceramic slurry A.
(2) Sacrificial layer slurry XS raw material:
Figure BDA0003231506650000181
preparation of sacrificial slurry XS: and mixing the sacrificial material, the dispersing agent, the binder and the solvent, and performing ball milling for 20 hours to obtain sacrificial slurry XS.
S2, tape casting:
(1) Single-layer casting: the height of the casting knife is adjusted to 2.0mm, and a ceramic slurry material belt A with the thickness of about 2.0mm is cast.
(2) Double-layer casting: adjusting the height of a front cutter of a tape casting cutter to 2.5mm, adjusting the height of a rear cutter to 0.3mm, adding sacrificial slurry XS behind the rear cutter, adding ceramic slurry A between the front cutter and the rear cutter, and performing tape casting to obtain a material tape
Figure BDA0003231506650000182
S3, curing:
respectively arranging the material belt A and the material belt
Figure BDA0003231506650000183
And (3) placing the material strip A in water for curing for 15h, wherein the curing of the material strip A is as follows: vertically putting the material belt A into water along the thickness direction of the plate body and stably putting the material belt A into the water until the material belt A is completely immersed into the water, wherein the temperature of the water is 15 ℃, the volume ratio of the water to the solvent contained in the material belt A is 80: 1, and curing for 15h. Material belt
Figure BDA0003231506650000184
The curing of (a) is as follows: taking another container filled with water, and placing the material belt along the thickness direction of the plate body
Figure BDA0003231506650000185
Vertically and stably put into water until the material belt is put into
Figure BDA0003231506650000186
Completely immersed in water, wherein the sacrificial layer XS is below and the slurry A is above (i.e., the sacrificial layer XS is deeper in the water), the temperature of the water is 15 ℃, and the water and the material belt are
Figure BDA0003231506650000187
The volume ratio of all solvents contained in the resin is 80: 1, and the curing time is 15 hours. Respectively obtaining a wet blank A and a wet blank through the treatment
Figure BDA0003231506650000188
S4, green body treatment:
mixing the wet blank A and the wet blank
Figure BDA0003231506650000189
Cutting into certain shape and size, air drying at 30 deg.C and 60% relative humidity for 30 hr to obtain green body A and green body
Figure BDA0003231506650000191
Thereafter, green body A and green body
Figure BDA0003231506650000192
Stacking, specifically stacking the upward surfaces of the two blanks during casting, and pressing at 65 ℃ under 700Psi and 3min of pressure maintaining to obtain a composite green blank with a thickness of about 3.3mm
Figure BDA0003231506650000193
S5, sintering:
compounding the green body
Figure BDA0003231506650000194
Heating to 800 ℃ atbase:Sub>A speed of 1 ℃/min, preserving heat for 2 hours, then removing glue, heating to 1450 ℃ atbase:Sub>A speed of 3 ℃/min, preserving heat for 5 hours, wherein the sacrificial layer XS is burnt off, and the ceramic setter plate A-A is obtained. Wherein, the one side that the thin end of straight hole corresponds in the gradient straight hole layer in two plate bodies A contacts each other.
Example 4: preparing ceramic load bearing board
Figure BDA0003231506650000195
(as shown in FIGS. 5-6)
S1, preparing ceramic slurry A, ceramic slurry B and sacrificial slurry XS;
(1) Ceramic slurry A raw material:
ceramic powder: 60wt% of mullite fine powder, 20wt% of white corundum powder, 15wt% of boehmite fine powder, 3.5wt% of kaolin fine powder and 1.5wt% of calcium carbonate powder;
adhesive: polyvinyl butyral PVB accounting for 7.5wt% of the ceramic powder;
dispersing agent: polyvinylpyrrolidone accounting for 1.7wt% of the mass of the ceramic powder;
pore-forming agent: graphite with a median particle size D50 of 35 μm, the volume of which accounts for 10% of the volume of the ceramic powder;
solvent: n-methyl-2-pyrrolidone NMP accounts for 40wt% of the total mass of the ceramic powder and the pore-forming agent.
Preparation of ceramic slurry A: mixing and ball-milling the ceramic powder, the pore-forming agent, the dispersing agent and the solvent for 5 hours, adding the binder, and continuing ball-milling for 15 hours to obtain ceramic slurry A.
(2) Ceramic slurry B raw material:
ceramic powder: 80wt% of alumina fine powder, 10wt% of silica fine powder, 5wt% of kaolin fine powder and 5wt% of titanium oxide fine powder;
adhesive: polyvinyl butyral PVB accounting for 7wt% of the ceramic powder;
dispersing agent: polyvinylpyrrolidone accounting for 1.5wt% of the ceramic powder;
pore-forming agent: graphite with a median particle size D50 of 35 μm, the volume of which accounts for 15% of the volume of the ceramic powder;
solvent: n-methyl-2-pyrrolidone NMP accounts for 48wt% of the total mass of the ceramic powder and the pore-forming agent.
Preparation of ceramic slurry B: mixing and ball-milling the ceramic powder, the pore-forming agent, the dispersing agent and the solvent for 5 hours, adding the binder, and continuing ball-milling for 15 hours to obtain ceramic slurry B.
(3) Sacrificial slurry XS feedstock:
Figure BDA0003231506650000196
Figure BDA0003231506650000201
preparation of sacrificial slurry XS: and mixing the sacrificial material, the dispersing agent, the binder and the solvent, and performing ball milling for 20 hours to obtain sacrificial slurry XS.
S2, tape casting:
(1) Double-layer casting of ceramic slurry: the height of the front blade of the casting blade is adjustedAdjusting the height of the rear cutter to be 0.3mm when the height of the rear cutter is 3mm, adding ceramic slurry B behind the rear cutter, adding ceramic slurry A between the front cutter and the rear cutter, and performing casting to obtain the material belt
Figure BDA0003231506650000202
(2) Double-layer tape casting of ceramic slurry and sacrificial slurry: adjusting the height of a front cutter of a casting cutter to 3mm, adjusting the height of a rear cutter to 0.3mm, adding sacrificial slurry XS behind the rear cutter, adding ceramic slurry A between the front cutter and the rear cutter, and casting to obtain the material belt
Figure BDA0003231506650000203
S3, curing:
respectively put the material belt
Figure BDA0003231506650000204
Material mixing belt
Figure BDA0003231506650000205
Curing in water for 10 hr to obtain a material belt
Figure BDA0003231506650000206
The curing of (a) is as follows: the material belt is arranged along the thickness direction of the plate body
Figure BDA0003231506650000207
Vertically and stably put into water until the material belt is put into
Figure BDA0003231506650000208
Completely immersed in water, wherein slurry B layer is below and slurry A layer is above (i.e. the depth of slurry B layer in water is deeper), the temperature of water is 15 ℃, and water and the material belt
Figure BDA0003231506650000209
The volume ratio of all solvents contained in the resin is 80: 1, and the curing time is 10 hours. Material belt
Figure BDA00032315066500002010
Is cured as follows: taking another container filled with water, and placing the material belt along the thickness direction of the plate body
Figure BDA00032315066500002011
Vertically and stably put into water until the material belt is put into
Figure BDA00032315066500002012
Completely immersed in water at 15 deg.C with the sacrificial layer XS layer below and the slurry A layer above (i.e., deeper depth of the sacrificial layer XS layer in water), and water and the tape
Figure BDA00032315066500002013
The volume ratio of all solvents contained in the resin is 80: 1, and the curing time is 10 hours. Respectively obtaining wet blanks by the treatment
Figure BDA00032315066500002014
And wet green
Figure BDA00032315066500002015
S4, green body treatment:
the wet blank is processed
Figure BDA00032315066500002016
And wet green
Figure BDA00032315066500002017
Cutting into certain shape and size, air drying at 20 deg.C and 60% relative humidity for 30 hr to obtain green bodies
Figure BDA00032315066500002018
And green compact
Figure BDA00032315066500002019
Thereafter, the green body is pressed
Figure BDA00032315066500002020
And green compact
Figure BDA00032315066500002021
Stacking the surfaces of the A layers of the two green bodies, and pressing at 65 deg.C under 700Psi for 3min to obtain a composite green body with a thickness of about 4.5mm
Figure BDA00032315066500002022
S5, sintering:
compounding the green body
Figure BDA00032315066500002023
Heating to 800 deg.C at a rate of 1 deg.C/min, maintaining for 2 hr, removing glue, heating to 1450 deg.C at a rate of 3 deg.C/min, and maintaining for 5 hr, wherein the sacrificial layer XS is burned off to obtain the ceramic setter plate
Figure BDA00032315066500002024
Wherein, the one side that the thin end of the straight hole in the gradient straight hole layer corresponds in two plate bodies contacts each other. The structure of the resulting product is shown in fig. 5-6.
Example 5:
(1) Characterization of
The microstructure test of the cross section of the ceramic setterbase:Sub>A-base:Sub>A obtained in example 3 was carried out, and the result is shown in fig. 7, and fig. 7 is an optical microscope photograph of the cross section of the ceramic setter obtained in example 3. It can be seen that a plurality of gradient straight hole structures appear inside the setter plate.
Observing the appearance of the upper and lower surfaces of the ceramic setter plate obtained in example 3, and as a result, as shown in fig. 8-9, fig. 8 is a schematic surface diagram of the honeycomb surface of the ceramic setter plate obtained in example 3, the honeycomb surface corresponds to the surface where the sacrificial layer XS is burned off, and a rough honeycomb structure is formed on the surface of the plate body due to the sintering off of the sacrificial layer XS; FIG. 9 is a schematic view of the smooth surface of the ceramic setter plate obtained in example 3.
(2) Performance testing
The ceramic setter plates obtained in examples 1 to 4 were subjected to performance tests, and the results are shown in Table 1.
TABLE 1 Properties of the ceramic setter plates obtained in examples 1 to 4
Figure BDA0003231506650000211
As can be seen from the test results in Table 1, the ceramic setter plates provided by the present invention have porosity of more than 55% and air permeability of 8500m 3 /m 2 H.bar or more, the three-point bending strength of 9.5MPa or more, higher porosity, good air permeability and mechanical strength.
The foregoing examples are provided to facilitate an understanding of the principles of the invention and their core concepts, including the best mode, and also to enable any person skilled in the art to practice the invention, including making and using any devices or systems and performing any incorporated methods. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention. The scope of the invention is defined by the claims and may include other embodiments that occur to those skilled in the art. Such other embodiments are intended to be within the scope of the claims if they have structural elements that approximate the literal language of the claims, or if they include equivalent structural elements with insubstantial differences from the literal languages of the claims.

Claims (3)

1. A ceramic load bearing plate is characterized in that,
is selected from a first ceramic load bearing board A and a second ceramic load bearing board
Figure FDA0003834507050000011
Third ceramic load bearing plate A-
Figure FDA0003834507050000012
Respectively as follows:
first ceramic setter plate a:
the plate body comprises a gradient straight hole layer; the gradient straight hole layer comprises a plurality of gradient straight holes distributed in a honeycomb shape, the axial direction of the hole channel is the thickness direction of the plate body, and the pore diameters of the straight holes are changed along the axial direction in a gradient manner; in the gradient straight hole, the size of each straight hole is independently selected from the following group: the aperture of the thin end is 0.1-10 μm, the aperture of the thick end is 50-500 μm, and the length of the pore channel is 0.1-5 mm;
the first ceramic setter plate A is prepared by the following preparation method:
s1, preparing ceramic slurry A and sacrificial layer slurry XS:
(1) Ceramic slurry A raw material:
ceramic powder: 80wt% of alumina fine powder, 10wt% of silica fine powder, 5wt% of kaolin fine powder and 5wt% of titanium oxide fine powder;
adhesive: polyvinyl butyral PVB accounting for 7.5wt% of the ceramic powder;
dispersing agent: polyvinylpyrrolidone accounting for 1.5wt% of the ceramic powder;
pore-forming agent: graphite with a median particle size D50 of 35 μm, the volume of which accounts for 15% of the volume of the ceramic powder;
solvent: n-methyl-2-pyrrolidone NMP, which accounts for 48wt% of the total mass of the ceramic powder and the pore-forming agent;
preparation of ceramic slurry A: mixing ceramic powder, a pore-forming agent, a dispersing agent and a solvent, carrying out ball milling for 5 hours, adding a binder, and continuing ball milling for 15 hours to obtain ceramic slurry A;
(2) Sacrificial layer slurry XS raw material:
Figure FDA0003834507050000013
preparation of sacrificial slurry XS: mixing and ball-milling the sacrificial material, the dispersing agent, the binder and the solvent for 20 hours to obtain sacrificial slurry XS;
s2, tape casting:
double-layer casting: adjusting the height of a front cutter of a casting cutter to 2.5mm, adjusting the height of a rear cutter to 0.3mm, adding sacrificial slurry XS behind the rear cutter, adding ceramic slurry A between the front cutter and the rear cutter, and casting to obtain the material belt
Figure FDA0003834507050000021
S3, curing:
feeding belt
Figure FDA0003834507050000022
Placing in water for curing for 15 hours, specifically: the material belt is arranged along the thickness direction of the plate body
Figure FDA0003834507050000023
Vertically and stably put into water until the material belt is put into
Figure FDA0003834507050000024
Completely immersed in water, wherein the sacrificial layer XS is below and the slurry A is above, the temperature of the water is 15 ℃, and the water and the material belt are
Figure FDA0003834507050000025
The volume ratio of all solvents contained in the mixture is 80: 1, and the mixture is solidified for 15 hours to obtain a wet blank
Figure FDA0003834507050000026
S4, green body treatment:
the wet blank is processed
Figure FDA0003834507050000027
Cutting into certain shape and size, air drying at 30 deg.C and relative humidity of 60% for 30 hr to obtain green body
Figure FDA0003834507050000028
S5, sintering:
mixing the green body
Figure FDA0003834507050000029
Heating to 800 deg.C at 1 deg.C/min, maintaining for 2 hr, discharging glue, and heating at 3 deg.C/minHeating to 1450 ℃, and preserving the temperature for 5h, wherein the sacrificial layer XS is burnt off to obtain a ceramic setter plate A;
or
Second ceramic load bearing plate
Figure FDA00038345070500000210
The plate body comprises a gradient straight hole layer and a capillary hole layer; the gradient straight hole layer comprises a plurality of gradient straight holes distributed in a honeycomb shape, the axial direction of the hole channel is the thickness direction of the plate body, and the aperture of each straight hole is changed along the axial direction in a gradient manner; in the gradient straight hole, the size of each straight hole is independently selected from the following group: the aperture of the thin end is 0.1 to 10 mu m, the aperture of the thick end is 50 to 500 mu m, and the length of the pore canal is 0.1 to 5mm; the capillary hole layer comprises a plurality of capillary holes;
the second ceramic load bearing board
Figure FDA00038345070500000211
The preparation method comprises the following steps:
s1, preparing ceramic slurry A and ceramic slurry B;
(1) Ceramic slurry A raw material:
ceramic powder: 60wt% of mullite fine powder, 20wt% of white corundum powder, 15wt% of boehmite fine powder, 3.5wt% of kaolin fine powder and 1.5wt% of calcium carbonate powder;
adhesive: polyvinyl butyral PVB accounting for 7.5wt% of the ceramic powder;
dispersing agent: polyvinylpyrrolidone accounting for 1.7wt% of the mass of the ceramic powder;
pore-forming agent: graphite with a median particle size D50 of 35 μm, the volume of which accounts for 10% of the volume of the ceramic powder;
solvent: n-methyl-2-pyrrolidone NMP, which accounts for 40wt% of the total mass of the ceramic powder and the pore-forming agent;
preparation of ceramic slurry A: mixing ceramic powder, a pore-forming agent, a dispersing agent and a solvent, carrying out ball milling for 5 hours, adding a binder, and continuing ball milling for 15 hours to obtain ceramic slurry A;
(2) Ceramic slurry B raw materials:
ceramic powder: 80wt% of alumina fine powder, 10wt% of silica fine powder, 5wt% of kaolin fine powder and 5wt% of titanium oxide fine powder;
adhesive: polyvinyl butyral PVB accounting for 7.5wt% of the ceramic powder;
dispersing agent: polyvinylpyrrolidone accounting for 1.5wt% of the ceramic powder;
pore-forming agent: graphite, wherein the median particle size D50 is 35 mu m, and the volume of the graphite accounts for 15 percent of the volume of the ceramic powder;
solvent: n-methyl-2-pyrrolidone NMP, which accounts for 48wt% of the total mass of the ceramic powder and the pore-forming agent;
preparation of ceramic slurry B: mixing ceramic powder, a pore-forming agent, a dispersing agent and a solvent, carrying out ball milling for 5 hours, adding a binder, and continuing ball milling for 15 hours to obtain ceramic slurry B;
s2, tape casting:
double-layer casting: adjusting the height of a front cutter of a casting cutter to 3mm, adjusting the height of a rear cutter to 0.3mm, adding ceramic slurry B behind the rear cutter, adding ceramic slurry A between the front cutter and the rear cutter, and casting to obtain the material belt
Figure FDA0003834507050000031
S3, curing:
feeding belt
Figure FDA0003834507050000032
Placing in water for curing for 10 hours, specifically: the material belt is arranged along the thickness direction of the plate body
Figure FDA0003834507050000033
Vertically and stably put into water until the material belt is put into
Figure FDA0003834507050000034
Completely immersing in water, wherein the slurry B layer is below and the slurry A layer is above, the temperature of water is 15 deg.C, and water and the material belt
Figure FDA0003834507050000035
The volume ratio of all solvents contained in the composition is 801, curing for 10 hours to obtain a wet blank
Figure FDA0003834507050000036
S4, green body treatment:
the wet blank is processed
Figure FDA0003834507050000037
Cutting into certain shape and size, air drying at 20 deg.C and 60% relative humidity for 30 hr to obtain green body
Figure FDA0003834507050000038
S5, sintering:
mixing the green body
Figure FDA0003834507050000039
Heating to 800 deg.C at a rate of 1 deg.C/min, maintaining for 2 hr, removing glue, heating to 1450 deg.C at a rate of 3 deg.C/min, and maintaining for 5 hr to obtain ceramic setter plate
Figure FDA00038345070500000310
Or
Third ceramic load bearing plate A-
Figure FDA00038345070500000311
The plate body includes: the first plate body and the second plate body are superposed and compounded;
the first plate body comprises a gradient straight hole layer;
the second plate body comprises a gradient straight hole layer and a capillary hole layer;
wherein the thin end surface in the gradient straight hole layer of the first plate body is in contact with the thin end surface in the gradient straight hole layer of the second plate body;
the surface of the thin end refers to the surface, close to the thin end of the straight hole, in the gradient straight hole layer;
the gradient straight hole layer comprises a plurality of gradient straight holes distributed in a honeycomb shape, the axial direction of the hole channel is the thickness direction of the plate body, and the aperture of each straight hole is changed along the axial direction in a gradient manner;
in the gradient straight hole, the size of each straight hole is independently selected from the following group: the aperture of the thin end is 0.1-10 μm, the aperture of the thick end is 50-500 μm, and the length of the pore channel is 0.1-5 mm;
the third ceramic burning bearing plate A-
Figure FDA0003834507050000041
The preparation method comprises the following steps:
s1, preparing ceramic slurry A, ceramic slurry B and sacrificial slurry XS;
(1) Ceramic slurry A raw material:
ceramic powder: 60wt% of mullite fine powder, 20wt% of white corundum powder, 15wt% of boehmite fine powder, 3.5wt% of kaolin fine powder and 1.5wt% of calcium carbonate powder;
adhesive: polyvinyl butyral PVB accounting for 7.5wt% of the ceramic powder;
dispersing agent: polyvinylpyrrolidone accounting for 1.7wt% of the mass of the ceramic powder;
pore-forming agent: graphite with a median particle size D50 of 35 μm, the volume of which accounts for 10% of the volume of the ceramic powder;
solvent: n-methyl-2-pyrrolidone NMP, which accounts for 40wt% of the total mass of the ceramic powder and the pore-forming agent;
preparation of ceramic slurry a: mixing ceramic powder, a pore-forming agent, a dispersing agent and a solvent, carrying out ball milling for 5 hours, adding a binder, and continuing ball milling for 15 hours to obtain ceramic slurry A;
(2) Ceramic slurry B raw materials:
ceramic powder: 80wt% of alumina fine powder, 10wt% of silica fine powder, 5wt% of kaolin fine powder and 5wt% of titanium oxide fine powder;
adhesive: polyvinyl butyral PVB accounting for 7wt% of the ceramic powder;
dispersing agent: polyvinylpyrrolidone accounting for 1.5wt% of the ceramic powder;
pore-forming agent: graphite with a median particle size D50 of 35 μm, the volume of which accounts for 15% of the volume of the ceramic powder;
solvent: n-methyl-2-pyrrolidone NMP, which accounts for 48wt% of the total mass of the ceramic powder and the pore-forming agent;
preparation of ceramic slurry B: mixing ceramic powder, a pore-forming agent, a dispersing agent and a solvent, carrying out ball milling for 5 hours, adding a binder, and continuing ball milling for 15 hours to obtain ceramic slurry B;
(3) Sacrificial slurry XS feedstock:
Figure FDA0003834507050000051
preparation of sacrificial slurry XS: mixing and ball-milling the sacrificial material, the dispersing agent, the binder and the solvent for 20 hours to obtain sacrificial slurry XS;
s2, tape casting:
(1) Double-layer casting of ceramic slurry: adjusting the height of a front cutter of a casting cutter to 3mm, adjusting the height of a rear cutter to 0.3mm, adding ceramic slurry B behind the rear cutter, adding ceramic slurry A between the front cutter and the rear cutter, and casting to obtain the material belt
Figure FDA0003834507050000052
(2) Double-layer tape casting of ceramic slurry and sacrificial slurry: adjusting the height of a front cutter of a casting cutter to 3mm, adjusting the height of a rear cutter to 0.3mm, adding sacrificial slurry XS behind the rear cutter, adding ceramic slurry A between the front cutter and the rear cutter, and casting to obtain the material belt
Figure FDA0003834507050000053
S3, curing:
respectively put the material belt
Figure FDA0003834507050000054
Material mixing belt
Figure FDA0003834507050000055
Curing in water for 10h to obtain a material belt
Figure FDA0003834507050000056
Curing ofThe following were used: the material belt is arranged along the thickness direction of the plate body
Figure FDA0003834507050000057
Vertically and stably put into water until the material belt is put into
Figure FDA0003834507050000058
Completely immersing in water, wherein the slurry B layer is below and the slurry A layer is above, the temperature of water is 15 deg.C, and water and the material belt
Figure FDA0003834507050000059
The volume ratio of all solvents contained in the resin is 80: 1, and the curing time is 10 hours; material belt
Figure FDA00038345070500000510
The curing of (a) is as follows: taking another container filled with water, and placing the material belt along the thickness direction of the plate body
Figure FDA00038345070500000511
Vertically and stably put into water until the material belt is put into
Figure FDA00038345070500000512
Completely immersed in water, wherein the sacrificial layer XS is below and the slurry A is above, the temperature of the water is 15 ℃, and the water and the material belt are
Figure FDA00038345070500000513
The volume ratio of all solvents contained in the resin is 80: 1, and the curing time is 10 hours; respectively obtaining wet blanks by the treatment
Figure FDA00038345070500000514
And wet green
Figure FDA00038345070500000515
S4, green body treatment:
the wet blank is processed
Figure FDA00038345070500000516
And wet green
Figure FDA00038345070500000517
Cutting into certain shape and size, air drying at 20 deg.C and 60% relative humidity for 30 hr to obtain green bodies
Figure FDA00038345070500000518
And green compact
Figure FDA00038345070500000519
Thereafter, the green body is pressed
Figure FDA00038345070500000520
And green compact
Figure FDA00038345070500000521
Stacking the surfaces of the A layers of the two green bodies, and pressing at 65 deg.C under 700Psi for 3min to obtain a composite green body with a thickness of about 4.5mm
Figure FDA00038345070500000522
S5, sintering:
compounding the green body
Figure FDA0003834507050000061
Heating to 800 ℃ at a speed of 1 ℃/min, preserving heat for 2h, removing glue, heating to 1450 ℃ at a speed of 3 ℃/min, preserving heat for 5h, wherein the sacrificial layer XS is burnt off to obtain the ceramic setter plate A-
Figure FDA0003834507050000062
Wherein, the one side that the thin end of the straight hole in the gradient straight hole layer corresponds in two plate bodies contacts each other.
2. The ceramic setter plate of claim 1, wherein the pore size of the plurality of capillaries in the capillary layer is independently selected from the group consisting of: 0.1-80 μm.
3. A method for producing a ceramic setter plate as set forth in any one of claims 1 to 2,
the first preparation method of the ceramic setter plate A comprises the following steps:
s1, preparing ceramic slurry A and sacrificial layer slurry XS:
(1) Ceramic slurry A raw material:
ceramic powder: 80wt% of fine alumina powder, 10wt% of fine silica powder, 5wt% of fine kaolin powder and 5wt% of fine titanium oxide powder;
adhesive: polyvinyl butyral PVB accounting for 7.5wt% of the ceramic powder;
dispersing agent: polyvinylpyrrolidone accounting for 1.5wt% of the ceramic powder;
pore-forming agent: graphite with a median particle size D50 of 35 μm, the volume of which accounts for 15% of the volume of the ceramic powder;
solvent: n-methyl-2-pyrrolidone NMP, which accounts for 48wt% of the total mass of the ceramic powder and the pore-forming agent;
preparation of ceramic slurry A: mixing ceramic powder, a pore-forming agent, a dispersing agent and a solvent, performing ball milling for 5 hours, adding a binder, and continuing ball milling for 15 hours to obtain ceramic slurry A;
(2) Sacrificial layer slurry XS raw material:
Figure FDA0003834507050000063
preparation of sacrificial slurry XS: mixing and ball-milling the sacrificial material, the dispersing agent, the binder and the solvent for 20 hours to obtain sacrificial slurry XS;
s2, tape casting:
double-layer casting: adjusting the height of a front cutter of a casting cutter to 2.5mm, adjusting the height of a rear cutter to 0.3mm, adding sacrificial slurry XS behind the rear cutter, adding ceramic slurry A between the front cutter and the rear cutter, and casting to obtain the material belt
Figure FDA0003834507050000071
S3, curing:
feeding belt
Figure FDA0003834507050000072
Placing in water for curing for 15 hours, specifically: the material belt is arranged along the thickness direction of the plate body
Figure FDA0003834507050000073
Vertically and stably put into water until the material belt is put into
Figure FDA0003834507050000074
Completely immersed in water, wherein the sacrificial layer XS is below and the slurry A is above, the temperature of the water is 15 ℃, and the water and the material belt are
Figure FDA0003834507050000075
The volume ratio of all solvents contained in the mixture is 80: 1, and the mixture is solidified for 15 hours to obtain a wet blank
Figure FDA0003834507050000076
S4, green body treatment:
the wet blank is processed
Figure FDA0003834507050000077
Cutting into certain shape and size, air drying at 30 deg.C and 60% relative humidity for 30 hr to obtain green body
Figure FDA0003834507050000078
S5, sintering:
mixing the green body
Figure FDA0003834507050000079
Heating to 800 deg.C at a rate of 1 deg.C/min, maintaining for 2 hr, removing glue, heating to 1450 deg.C at a rate of 3 deg.C/min, and maintaining for 5 hr, wherein the sacrificial layer XS is burnt off to obtain the final productA ceramic setter plate A;
or
Second ceramic load bearing plate
Figure FDA00038345070500000710
The preparation method comprises the following steps:
s1, preparing ceramic slurry A and ceramic slurry B;
(1) Ceramic slurry A raw material:
ceramic powder: 60wt% of mullite fine powder, 20wt% of white corundum powder, 15wt% of boehmite fine powder, 3.5wt% of kaolin fine powder and 1.5wt% of calcium carbonate powder;
adhesive: polyvinyl butyral PVB accounting for 7.5wt% of the ceramic powder;
dispersing agent: polyvinylpyrrolidone accounting for 1.7wt% of the mass of the ceramic powder;
pore-forming agent: graphite with a median particle size D50 of 35 μm, the volume of which accounts for 10% of the volume of the ceramic powder;
solvent: n-methyl-2-pyrrolidone NMP, which accounts for 40wt% of the total mass of the ceramic powder and the pore-forming agent;
preparation of ceramic slurry A: mixing ceramic powder, a pore-forming agent, a dispersing agent and a solvent, carrying out ball milling for 5 hours, adding a binder, and continuing ball milling for 15 hours to obtain ceramic slurry A;
(2) Ceramic slurry B raw materials:
ceramic powder: 80wt% of alumina fine powder, 10wt% of silica fine powder, 5wt% of kaolin fine powder and 5wt% of titanium oxide fine powder;
adhesive: polyvinyl butyral PVB accounting for 7.5wt% of the ceramic powder;
dispersing agent: polyvinylpyrrolidone accounting for 1.5wt% of the ceramic powder;
pore-forming agent: graphite with a median particle size D50 of 35 μm, the volume of which accounts for 15% of the volume of the ceramic powder;
solvent: n-methyl-2-pyrrolidone NMP, which accounts for 48wt% of the total mass of the ceramic powder and the pore-forming agent;
preparation of ceramic slurry B: mixing ceramic powder, a pore-forming agent, a dispersing agent and a solvent, carrying out ball milling for 5 hours, adding a binder, and continuing ball milling for 15 hours to obtain ceramic slurry B;
s2, tape casting:
double-layer casting: adjusting the height of a front cutter of a casting cutter to 3mm, adjusting the height of a rear cutter to 0.3mm, adding ceramic slurry B behind the rear cutter, adding ceramic slurry A between the front cutter and the rear cutter, and casting to obtain the material belt
Figure FDA0003834507050000081
S3, curing:
feeding belt
Figure FDA0003834507050000082
Placing in water for curing for 10 hours, specifically: the material belt is arranged along the thickness direction of the plate body
Figure FDA0003834507050000083
Vertically and stably put into water until the material belt is put into
Figure FDA0003834507050000084
Completely immersed in water, wherein the slurry B layer is arranged below the slurry A layer, the temperature of the water is 15 ℃, and the water and the material belt are
Figure FDA0003834507050000085
The volume ratio of all solvents contained in the mixture is 80: 1, and the mixture is solidified for 10 hours to obtain a wet blank
Figure FDA0003834507050000086
S4, green body treatment:
the wet blank is processed
Figure FDA0003834507050000087
Cutting into certain shape and size, air drying at 20 deg.C and 60% relative humidity for 30 hr to obtain green body
Figure FDA0003834507050000088
S5, sintering:
mixing the green body
Figure FDA0003834507050000089
Heating to 800 deg.C at a rate of 1 deg.C/min, maintaining for 2 hr, removing glue, heating to 1450 deg.C at a rate of 3 deg.C/min, and maintaining for 5 hr to obtain ceramic setter plate
Figure FDA00038345070500000810
Or
Third ceramic load bearing plate A-
Figure FDA00038345070500000811
The preparation method comprises the following steps:
s1, preparing ceramic slurry A, ceramic slurry B and sacrificial slurry XS;
(1) Ceramic slurry A raw material:
ceramic powder: 60wt% of mullite fine powder, 20wt% of white corundum powder, 15wt% of boehmite fine powder, 3.5wt% of kaolin fine powder and 1.5wt% of calcium carbonate powder;
adhesive: polyvinyl butyral PVB accounting for 7.5wt% of the ceramic powder;
dispersing agent: polyvinylpyrrolidone accounting for 1.7wt% of the mass of the ceramic powder;
pore-forming agent: graphite with a median particle size D50 of 35 μm, the volume of which accounts for 10% of the volume of the ceramic powder;
solvent: n-methyl-2-pyrrolidone NMP, which accounts for 40wt% of the total mass of the ceramic powder and the pore-forming agent;
preparation of ceramic slurry A: mixing ceramic powder, a pore-forming agent, a dispersing agent and a solvent, carrying out ball milling for 5 hours, adding a binder, and continuing ball milling for 15 hours to obtain ceramic slurry A;
(2) Ceramic slurry B raw materials:
ceramic powder: 80wt% of alumina fine powder, 10wt% of silica fine powder, 5wt% of kaolin fine powder and 5wt% of titanium oxide fine powder;
adhesive: polyvinyl butyral (PVB) accounting for 7wt% of the ceramic powder;
dispersing agent: polyvinylpyrrolidone accounting for 1.5wt% of the mass of the ceramic powder;
pore-forming agent: graphite with a median particle size D50 of 35 μm, the volume of which accounts for 15% of the volume of the ceramic powder;
solvent: n-methyl-2-pyrrolidone NMP, which accounts for 48wt% of the total mass of the ceramic powder and the pore-forming agent;
preparation of ceramic slurry B: mixing ceramic powder, a pore-forming agent, a dispersing agent and a solvent, carrying out ball milling for 5 hours, adding a binder, and continuing ball milling for 15 hours to obtain ceramic slurry B;
(3) Sacrificial slurry XS feedstock:
Figure FDA0003834507050000091
preparation of sacrificial slurry XS: mixing and ball-milling the sacrificial material, the dispersing agent, the binder and the solvent for 20 hours to obtain sacrificial slurry XS;
s2, tape casting:
(1) Double-layer casting of ceramic slurry: adjusting the height of a front cutter of a tape casting cutter to 3mm, adjusting the height of a rear cutter to 0.3mm, adding a ceramic slurry B behind the rear cutter, adding a ceramic slurry A between the front cutter and the rear cutter, and performing tape casting to obtain a material belt
Figure FDA0003834507050000092
(2) Double-layer tape casting of ceramic slurry and sacrificial slurry: adjusting the height of a front cutter of a casting cutter to 3mm, adjusting the height of a rear cutter to 0.3mm, adding sacrificial slurry XS behind the rear cutter, adding ceramic slurry A between the front cutter and the rear cutter, and casting to obtain the material belt
Figure FDA0003834507050000093
S3, curing:
respectively put the material belt
Figure FDA0003834507050000101
Material mixing belt
Figure FDA0003834507050000102
Curing in water for 10h to obtain a material belt
Figure FDA0003834507050000103
The curing of (a) is as follows: the material belt is arranged along the thickness direction of the plate body
Figure FDA0003834507050000104
Vertically and stably put into water until the material belt is put into
Figure FDA0003834507050000105
Completely immersing in water, wherein the slurry B layer is below and the slurry A layer is above, the temperature of water is 15 deg.C, and water and the material belt
Figure FDA0003834507050000106
The volume ratio of all solvents contained in the resin is 80: 1, and the curing time is 10 hours; material belt
Figure FDA0003834507050000107
The curing of (a) is as follows: taking another container filled with water, and placing the material belt along the thickness direction of the plate body
Figure FDA0003834507050000108
Vertically and stably put into water until the material belt is put into
Figure FDA0003834507050000109
Completely immersed in water, wherein the sacrificial layer XS is below and the slurry A is above, the temperature of the water is 15 ℃, and the water and the material belt are
Figure FDA00038345070500001010
The volume ratio of all solvents contained in the resin is 80: 1, and the curing time is 10 hours; respectively obtaining wet blanks by the treatment
Figure FDA00038345070500001011
And wet green
Figure FDA00038345070500001012
S4, green body treatment:
the wet blank is processed
Figure FDA00038345070500001013
And wet green
Figure FDA00038345070500001014
Cutting into certain shape and size, air drying at 20 deg.C and relative humidity of 60% for 30 hr to obtain green bodies
Figure FDA00038345070500001015
And green compact
Figure FDA00038345070500001016
Thereafter, the green body is pressed
Figure FDA00038345070500001017
And green compact
Figure FDA00038345070500001018
Stacking the surfaces of the A layers of the two green bodies, and pressing at 65 deg.C under 700Psi for 3min to obtain a composite green body with a thickness of about 4.5mm
Figure FDA00038345070500001019
S5, sintering:
compounding the green body
Figure FDA00038345070500001020
Heating to 800 ℃ at a speed of 1 ℃/min, preserving heat for 2h, removing glue, heating to 1450 ℃ at a speed of 3 ℃/min, preserving heat for 5h, wherein the sacrificial layer XS is burnt off to obtain the ceramic setter plate A-
Figure FDA00038345070500001021
Wherein, the one side that the thin end of the straight hole in the gradient straight hole layer corresponds in two plate bodies contacts each other.
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