CN110028319A - Powder granule grading method and Zirconium powder casting slurry and preparation method thereof - Google Patents

Powder granule grading method and Zirconium powder casting slurry and preparation method thereof Download PDF

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CN110028319A
CN110028319A CN201910242183.0A CN201910242183A CN110028319A CN 110028319 A CN110028319 A CN 110028319A CN 201910242183 A CN201910242183 A CN 201910242183A CN 110028319 A CN110028319 A CN 110028319A
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zirconia
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邢长生
侯令涛
童双龙
周伟
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Hubei Xi Tian Science And Technology Ltd
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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    • C04B2235/6025—Tape casting, e.g. with a doctor blade
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Abstract

A kind of powder granule grading method, the particle of basic diameter of particle d presses the face-centred cubic accumulation mode close in cubic system, on the basis of basic diameter of particle, a certain amount of granularity of gradation is less than or equal to the particle of face-centered cubic tetrahedron and octahedra maximal clearance partial size, is filled in it in its tetrahedron and octahedral interstice.Specifically, the grain diameter of gradation and its volume or weight number are as follows: partial size d is filled in basic d100 parts of diameter of particle, tetrahedral interstice4≤ 0.225d and≤2.3 part, octahedral interstice fills partial size d8≤ 0.414d and≤7.1 part.Diameter of particle d, d4, d8Within the 0.2~1.0um of powder granularity range for being suitble to zirconium oxide curtain coating.The grading method does not increase accumulation body volume, only increases bulk density, in subsequent oxidation zirconium casting technique, under the premise of guaranteeing processing performance, improves the useful load of casting slurry, and the ceramic dense degree and intensity after firing are improved.

Description

Powder particle grading method, zirconia powder tape-casting slurry and preparation method thereof
Technical Field
The invention relates to a powder particle grading method, high-loading-capacity zirconia powder tape-casting slurry and a preparation method thereof, belonging to the technical field of material processing.
Background
The casting process of ceramic powder is an important forming means, has wide application, and particularly has a plurality of applications in the fields of electronic ceramics and functional ceramics. The zirconia flake or multilayer ceramic product is mainly formed by tape casting, and the lower the content of the organic carrier is, the higher the loading capacity is, and the higher the strength after sintering is. However, the loading is affected by many factors, and the process performance is affected by the content of the organic vehicle being too low, and particularly, stress cracking and other defects are generated in the subsequent process operation, which in turn reduces the strength of the fired product.
Therefore, it is necessary to research the characteristics of the zirconia powder itself, and to increase the loading as much as possible while ensuring the process performance, so as to improve the strength of the zirconia ceramic product by the tape casting process.
Disclosure of Invention
The invention aims to provide a powder particle composition method, zirconia powder casting slurry and a preparation method thereof, wherein the loading capacity of the zirconia powder casting slurry is improved through the powder particle composition, so that the strength of a zirconia ceramic product in a casting process is improved, and the technical bottleneck that the process performance is reduced due to the improvement of the loading capacity of the zirconia casting slurry in the prior art is broken through.
The invention provides a powder particle grading method, which comprises the following steps: the particles with the basic powder particle size d are graded into certain amount of particles with the particle size less than or equal to the maximum gap particle size of face-centered cubic tetrahedron and/or octahedron according to the stacking mode close to face-centered cubic in a cubic system on the basis of the basic powder particle size d, and the particles are filled in the tetrahedral and/or octahedral gaps.
According to a particular but non-limiting embodiment of the invention, the particle size of the graded particles and their volume or weight fraction are:
the particle diameter d of the basic powder is 100 portions,
tetrahedral gap filling particle size d4Not less than 0.225d and not more than 2.3 parts,
octahedral gap-filling particle diameter d8Not less than 0.414d not more than 7.1 portions.
According to a particular but non-limiting embodiment of the invention, the powder size grading process is used for size grading of zirconia, silica or alumina powders.
According to a particular but non-limiting embodiment of the invention, for the granulometric composition of the zirconia powder, the particle size d, d of said powder4，d8The particle size of the powder suitable for casting is within 0.2-1.0 um.
According to a particular but non-limiting embodiment of the invention, the particle size of the graded particles and their volume or weight fraction are:
the particle diameter d of the basic powder is 100 portions,
tetrahedral gap filling particle size d40.225d 2.3 portions,
octahedral gap-filling particle diameter d80.414d 7.1 portion;
wherein the particle diameter d, d of the powder4，d8The particle size of the powder suitable for casting is within 0.2-1.0 um.
In another aspect, the present invention provides a high-loading cast slurry of zirconia powder, wherein the zirconia powder is graded by the powder particle grading method as described above.
According to a specific but non-limiting embodiment of the present invention, the zirconia powder casting slurry comprises the following main components in parts by weight:
wherein the particle diameter d, d of the powder4，d8Within the range of 0.2-1.0 um.
According to a specific but non-limiting embodiment of the invention, wherein the solvent is at least one of toluene or ethanol; the dispersant is triethanolamine; the binder is polyvinyl butyral; the plasticizer is butyl benzyl phthalate; the lubricant is polyethylene glycol.
According to a specific but non-limiting embodiment of the present invention, the zirconia powder casting slurry comprises the following main components in parts by weight:
wherein the particle diameter d, d of the powder4，d8Within the range of 0.2-1.0 um.
On the other hand, the invention also provides a preparation method of the high-loading-capacity zirconia powder casting slurry, and the zirconia powder is graded by the powder particle grading method.
The invention has the following beneficial effects:
1. the invention provides a powder particle grading method according to the accumulation mode of face-centered cubic in a crystallographic cubic system, particles with the particle size less than or equal to the maximum gap particle size are embedded in the gaps of a tetrahedron and an octahedron, the accumulation density is increased under the condition of not increasing the volume of an accumulation body, and further, in the subsequent zirconia casting process, the loading capacity of zirconia casting slurry is improved on the premise of ensuring the process performance.
2. According to the zirconia powder tape-casting slurry and the preparation method thereof, the high-loading-capacity zirconia tape-casting sheet can be obtained by utilizing the particle grading, the density and the strength of the sintered ceramic are improved, and the technical bottleneck that the technological performance is reduced due to the improvement of the loading capacity of the zirconia tape-casting slurry in the prior art is broken through.
Drawings
FIG. 1 is a face centered cubic model of the closest packing of powders.
FIG. 2 is a schematic view of a face-centered cube in which the powders are most densely packed.
FIG. 3 is a schematic diagram of an abstract face-centered cube.
Fig. 4 is a regular tetrahedron ABCD of fig. 3.
Fig. 5 is a top view of the bottom surface DBC of fig. 4.
FIG. 6 is a regular octahedron DBCEFG of FIG. 3.
Fig. 7 is a top view of the face BCEF of fig. 6.
FIG. 8 is a top view of face AIJK in the face-centered cube of FIG. 3.
Detailed Description
The following specific embodiments are provided to further illustrate the present invention, but the present invention is not limited to only the following embodiments.
The invention provides a powder particle grading method according to the accumulation mode of face-centered cubic in a crystallographic cubic system.
The basic powder particle diameter d is close to the mode of face-centered cubic stacking in the cubic system in the closest stacking state among various types of stacking, and fig. 1 and 2 are close to the actual state of face-centered cubic stacking, and fig. 3 is an abstract face-centered cubic schematic diagram. As shown in fig. 3, embedding particles having a particle size of not more than the maximum interstitial particle size in the tetragonal and octahedral gaps thereof makes it possible to increase the bulk density without increasing the volume of the stack.
According to the solid geometry relation of face-centered cubic lattice structure in crystallography, the maximum particle size that can be filled in the tetrahedral and octahedral gaps can be deduced.
The lattice particles are assumed to be in rigid ball contact with adjacent particles. The tetrahedral gap is formed by the vertex particle and the face center particle of the three adjacent sides of the vertex, for example, ABCD in figure 3 forms a tetrahedron, all four particles are in rigid ball contact, a gap exists in the center of the regular tetrahedron, a filling particle is placed in the gap, and the largest filling particle capable of being placed can be in rigid ball contact with the four particles.
FIG. 4 is a regular tetrahedron ABCD of FIG. 3, wherein a filler particle is placed in the regular tetrahedron such that the filler particle is in rigid ball contact with four vertex particles, wherein O is the center of the filler particle and the radius of the filler particle is r4When the particle diameter of the powder particle is d, AO-OD-1/2 d + r4；
Fig. 5 is a top view of the base surface DBC in fig. 4, the side length DC of the equilateral triangle DBC being d,
as shown in fig. 4, A O1Is the extension line of the point A passing through the sphere center O, is perpendicular to the BCD surface and is positioned in a right triangle AO1In the step D, the step (c),
then
In the right triangle OO as shown in FIG. 41In the step D, the step (c),
according to (OO)1)2+(DO1)2＝(OD)2，OO1＝AO1-AO, provided that AO ═ OD ═ l
Then
Then
Then d4＝2r4＝0.225d。
From this, the maximum particle diameter of the particles filled in the tetrahedral gap was calculated to be 0.225d in accordance with the face centered cubic packing.
Next, the maximum particle size filled in the octahedral gap is first deduced.
An octahedral gap is an octahedron of six face-centered particles, each particle being in rigid ball contact with an adjacent particle and not with an opposing particle, such as DBCEFG in fig. 3, forming an octahedron, there being a gap in the center of the octahedron, into which gap a filler particle is placed, the largest filler particle that can be placed being in rigid ball contact with six particles.
FIG. 6 is a octahedron DBCEFG of FIG. 3, into which a filler particle is placed in rigid ball contact with six vertex particles, where O is the spherical center of the filler particle and the radius of the filler particle is r8If the particle size of the powder particles is d, DE is d;
fig. 7 is a top view of the plane BCEF of fig. 6, where the side length EF of the square BCEF is d, the distance OH from the center O to the center point H of EF is d/2, EH is d/2,
as in FIG. 6, in the right triangle DEH, (DH)2＝(DE)2-(EH)2＝d2-(d/2)2＝3/4d2
Then
As in fig. 6, in the right triangle DOH,
then
Then d8＝0.414d。
From this, the maximum particle diameter of the particles filled in the octahedral gap was calculated to be 0.414d in accordance with the face-centered cubic packing manner.
The maximum volume number that tetrahedral gaps and octahedral gaps can fill is calculated below. Assuming that the volume of the powder of the basic powder particle diameter d is V, then
Maximum volume V of tetrahedral gap fillable4maxThe volume of the tetrahedral interstitial maximum filling particles/the packing volume of the face centered cubic · V;
maximum volume V of octahedral gap fillable8maxThe octahedral interstitial maximum filling particle volume/face-centered cubic packing volume · V;
the number of tetrahedral gaps in a single face-centered cube is 8, and the number of octahedral gaps is 4, then
Maximum tetrahedral interstitial filling particle volume of 8 × (4/3) pi (d)4/2)3＝8(1/6)π(0.225d)3＝0.0477d3,
Octahedral interstitial maximum filling particle volume 4 × (4/3) pi (d)8/2)3＝4(1/6)π(0.414d)3＝0.149d3,
As shown in fig. 3, the side length of the face-centered cube is a, and the volume of the face-centered cube is a3When the packing density of the face-centered cubic is 0.74, the packing volume of the face-centered cubic is 0.74a3，
FIG. 8 is a top view of the face-centered cubic middle plane AIJK of FIG. 3, (AI)2+(JI)2＝(AJ)2，AJ＝2d，2a2＝(2d)2Then, then
The maximum volume V that the tetrahedral gap can be filled with4maxVolume of maximum filling particle per face-centered cubic (fee) of tetrahedral gap V0.0477 d3/2.09d3·V＝0.023V，
Maximum volume V of octahedral gap fillable8maxVolume of octahedral interstitial maximum filling particles/face-centered cubic packing volume. V is 0.149d3/2.09d3·V＝0.071V。
Thus, the maximum fillable volume of the tetrahedral gap is calculated to be 0.023V; the maximum volume that the octahedral gap can be filled with is 0.071V.
In the practical application of zirconia powder, for example, in the practical casting slurry system, the random collision of zirconia powder particles in the slurry system has a certain probability to form the closest packing of the face-centered cubic, and as long as the particle grading meets the rule of tetrahedral and octahedral gap filling, the effect of increasing the casting loading capacity on the premise of ensuring the casting process performance can be achieved.
The invention therefore provides a powder particle grading method, which comprises the following steps: the particles with the basic powder particle size d are graded into certain amount of particles with the particle size less than or equal to the maximum gap particle size of face-centered cubic tetrahedron and/or octahedron according to the stacking mode close to face-centered cubic in a cubic system on the basis of the basic powder particle size d, and the particles are filled in the tetrahedral and/or octahedral gaps. By the gradation, the bulk density of the powder is increased without increasing the volume of the bulk.
Specifically, the particle size and volume or weight parts of the graded particles are as follows:
the particle diameter d of the basic powder is 100 portions,
tetrahedral gap filling particle size d4Not less than 0.225d and not more than 2.3 parts,
octahedral gap-filling particle diameter d8Not less than 0.414d not more than 7.1 portions.
Since the base powder and the filler powder are the same powder, they may be expressed in terms of parts by volume and parts by weight.
The powder particle grading method of the invention is applicable to zirconia powder, and other spherical powder such as silica powder, alumina powder and the like.
The particle diameter d of the zirconia powder suitable for casting is 0.2-1.0 um, and the specific surface area is 6-16 m2G, therefore, the particle diameters d, d of the above-mentioned powders4，d8The particle size of the powder suitable for casting is within 0.2-1.0 um.
The graded zirconia powder is added with 30 to 60 weight parts of solvent, 0.1 to 2 weight parts of dispersant, 4 to 9 weight parts of adhesive, 2 to 3 weight parts of plasticizer and 2 to 3 weight parts of lubricant based on 100 weight parts of basic powder, and is prepared into high-loading zirconia casting slurry by a ball milling method.
Among them, the solvent, the dispersant, the binder, the plasticizer and the lubricant may be those commonly used in the casting process, for example, the solvent may be toluene, ethanol, etc.; the dispersant may be triethanolamine or the like; the binder may be polyvinyl butyral, or the like; the plasticizer can be butyl benzyl phthalate and the like; the lubricant may be polyethylene glycol or the like.
Experiments prove that compared with the ceramic chip fired by the casting sheet which is not graded, the ceramic chip fired by the graded casting sheet has the advantages that the relative density is improved by more than 1.5 percent, and the breaking strength is improved by more than 5 percent. Therefore, the zirconia casting sheet with higher loading capacity can be obtained by the powder particle grading method, and the density and the strength of the sintered ceramic are higher.
The present invention will be further illustrated with reference to the following specific examples, but the present invention is not limited to the following examples.
The experimental procedures used above and in the examples below are conventional unless otherwise specified.
The materials, reagents and the like used above and in the following examples are commercially available unless otherwise specified.
Example 1
Preparing high-loading zirconia tape-casting slurry by using the following powder grading method:
the basic zirconia powder particle size d is 0.5um gradation, d is calculated according to the powder gradation method80.207um, the addition amount is 7.1 percent of the basic powder; d40.113um, not in the range of 0.2 to 1.0um of powder suitable for casting. Therefore, the optimum powder composition of the system is that the powder fraction with the particle diameter d of 0.5um is 100 parts, and the particle diameter d8The powder fraction of 0.207um is 7.1 parts. The graded powder is used to replace 100 parts of powder with the grain diameter d of 0.5um to prepare casting slurry.
The preparation method of the casting slurry comprises the following steps: 100 parts by weight of zirconia powder with the particle size of 0.5um and 7.1 parts by weight of zirconia powder with the particle size of 0.207um are taken, 40 parts by weight of solvent toluene and half of ethanol are added, 0.5 part by weight of dispersant triethanolamine, 8 parts by weight of adhesive polyvinyl butyral, 3 parts by weight of plasticizer butyl benzyl phthalate and 3 parts by weight of lubricant polyethylene glycol are added, and casting slurry is prepared by a ball milling method.
Compared with 100 parts by weight of ungraded zirconia powder with the grain diameter of 0.5um, the same amount of solvent, dispersant, adhesive, plasticizer and lubricant are added to prepare the casting slurry by a ball milling method.
And preparing the casting slurry into a casting sheet on a casting machine, placing the oxygen sensor casting sheet in a program-controlled sintering furnace for removing organic matters and sintering, wherein glue is discharged before sintering, the temperature rise speed is controlled to be 0.2 ℃/min, the temperature range is 200-800 ℃, and the sintering temperature is set at 1500 ℃.
And comparing the density and the breaking strength of the ceramic chip sintered by the graded casting sheet with the ceramic chip sintered by the non-graded casting sheet. The density of the ceramic chip without grading is 5.7g/cm3The strength is 1200 Mpa; the ceramic chip density after grading is 5.8g/cm3Strength 1265 MPa; the relative density of the ceramic chip after grading is improved by 1.8%, and the strength is improved by more than 5%.
Example 2
Preparing high-loading zirconia tape-casting slurry by using the following powder grading method:
the grading that the particle diameter d of the basic zirconia powder is 0.6um is calculated according to the powder grading method80.248um, the addition amount is 7.1 percent of the basic powder; d40.135um, not in the range of 0.2-1.0 um of powder suitable for casting. Therefore, the optimum powder composition of the system is that the powder fraction with the particle diameter d of 0.6um is 100 parts, and the particle diameter d8The powder fraction is 7.1 parts of 0.248 um. The graded powder is used to replace 100 parts of powder with the grain diameter d of 0.6um to prepare casting slurry.
The preparation method of the casting slurry comprises the following steps: 100 parts by weight of zirconia powder with the particle size of 0.6um and 7.1 parts by weight of zirconia powder with the particle size of 0.248um are taken, 40 parts by weight of solvent toluene and half of ethanol are added, 0.5 part by weight of dispersant triethanolamine, 8 parts by weight of adhesive polyvinyl butyral, 3 parts by weight of plasticizer butyl benzyl phthalate and 3 parts by weight of lubricant polyethylene glycol are added, and casting slurry is prepared by a ball milling method.
Compared with 100 parts by weight of ungraded zirconia powder with the grain diameter of 0.6um, the same amount of solvent, dispersant, adhesive, plasticizer and lubricant are added to prepare the casting slurry by a ball milling method.
The firing process was the same as in example 1. And comparing the density and the breaking strength of the ceramic chip sintered by the graded casting sheet with the ceramic chip sintered by the non-graded casting sheet. The density of the ceramic chip without grading is 5.6g/cm3The strength is 1180 Mpa; the ceramic chip density after grading is 5.7g/cm3The strength is 1240 MPa; the relative density of the ceramic chip after grading is improved by 1.8%, and the strength is improved by 5%.
Example 3
Preparing high-loading zirconia tape-casting slurry by using the following powder grading method:
grading with the particle diameter d of the basic zirconia powder being 1.0um, and calculating d according to the powder grading method80.414um, the addition amount is 7.1%; d40.225um, 2.3% was added. Therefore, the optimum powder composition of the system is that the powder fraction with the particle diameter d of 1.0um is 100 parts, and the particle diameter d8Powder fraction of 0.414um is 7.1 parts, and powder fraction of 0.225um particle diameter d is 2.3 parts. The graded powder is used to replace 100 parts of powder with the grain diameter d of 1.0um to prepare casting slurry.
The preparation method of the casting slurry comprises the following steps: 100 parts by weight of zirconia powder with the grain diameter of 1.0um, 7.1 parts by weight of zirconia powder with the grain diameter of 0.414um and 2.3 parts by weight of zirconia powder with the grain diameter of 0.225um are taken, 40 parts by weight of solvent toluene and ethanol are added respectively, 0.5 part by weight of dispersant triethanolamine, 8 parts by weight of adhesive polyvinyl butyral, 3 parts by weight of plasticizer butyl benzyl phthalate and 3 parts by weight of lubricant polyethylene glycol are added, and casting slurry is prepared by a ball milling method.
Compared with 100 parts by weight of ungraded zirconia powder with the grain diameter of 1.0um, the same amount of solvent, dispersant, adhesive, plasticizer and lubricant are added to prepare casting slurry by a ball milling method.
The firing process was the same as in example 1. And comparing the density and the breaking strength of the ceramic chip sintered by the graded casting sheet with the ceramic chip sintered by the non-graded casting sheet. The density of the ceramic chips without grading is 5.58g/cm3The strength is 1150 Mpa; the ceramic chip density after grading is 5.69g/cm3The strength is 1242 Mpa; the relative density of the ceramic chip after grading is improved by 2 percent, and the strength is improved by 8 percent.
The above is only a specific application example of the present invention, and the protection scope of the present invention is not limited in any way. All the technical solutions formed by equivalent transformation or equivalent replacement fall within the protection scope of the present invention.

Claims (10)

1. A powder particle grading method comprises the following steps: the particles with the basic powder particle size d are graded into certain amount of particles with the particle size less than or equal to the maximum gap particle size of face-centered cubic tetrahedron and/or octahedron according to the stacking mode close to face-centered cubic in a cubic system on the basis of the basic powder particle size d, and the particles are filled in the tetrahedral and/or octahedral gaps.
2. The process according to claim 1, wherein the particle size of the graded particles and the volume or weight fraction thereof are:
the particle diameter d of the basic powder is 100 portions,
tetrahedral gap filling particle size d4Not less than 0.225d and not more than 2.3 parts,
octahedral gap-filling particle diameter d8Not less than 0.414d not more than 7.1 portions.
3. The process according to claim 1 or 2, for the particle grading of zirconia, silica or alumina powders.
4. The method according to claim 2, for the particle grading of zirconia powders, the particle size d, d of said powders4，d8The particle size of the powder suitable for casting is within 0.2-1.0 um.
5. The process according to claim 2, wherein the particle size of the graded particles and the volume or weight fraction thereof are:
the particle diameter d of the basic powder is 100 portions,
tetrahedral gap filling particle size d40.225d 2.3 portions,
octahedral gap-filling particle diameter d80.414d 7.1 portion;
wherein the particle diameter d, d of the powder4，d8The particle size of the powder suitable for casting is within 0.2-1.0 um.
6. A high loading cast slurry of zirconia powder, wherein the zirconia powder is graded by the powder particle grading method of any of claims 1 to 5.
7. A zirconia powder casting slurry according to claim 6 comprising the following major components in parts by weight:
wherein,the particle diameter d, d of the powder4，d8Within the range of 0.2-1.0 um.
8. The casting slurry of zirconia powder according to claim 7, wherein the solvent is at least one of toluene or ethanol; the dispersant is triethanolamine; the binder is polyvinyl butyral; the plasticizer is butyl benzyl phthalate; the lubricant is polyethylene glycol.
9. The zirconia powder casting slurry according to claim 7, which comprises the following main components in parts by weight:
wherein the particle diameter d, d of the powder4，d8Within the range of 0.2-1.0 um.
10. A method of preparing a high loading cast slurry of zirconia powder which has been graded by the powder particle grading process of any one of claims 1 to 5.
CN201910242183.0A 2019-03-28 2019-03-28 Powder granule grading method and Zirconium powder casting slurry and preparation method thereof Pending CN110028319A (en)

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