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 PDFInfo
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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
Technical field
The present invention relates to the Zirconium powder casting slurry of a kind of powder granule grading method and a kind of high useful load and its
Preparation method belongs to materials processing technology field.
Background technique
The casting technique of ceramic powder is a kind of critically important prototyping method, is widely used, especially in electronic ceramics and
There are many applications in function ceramics field.Zirconium oxide flake or multi-layer ceramics product mainly use tape casting, and organic carrier contains
Amount is lower, and useful load is higher, and sintered intensity is also higher.However, there are many factor for influencing useful load, organic carrier content mistake
The defects of low processing performance that will lead to is affected, and stress cracking is generated especially in later processing operation, reduces burn instead
At the intensity of product.
Therefore, it is necessary to be studied in terms of the characteristic of Zirconium powder itself, under the premise of guaranteeing processing performance to the greatest extent
Useful load may be improved, to improve the intensity of casting molding processes zirconia ceramic product.
Summary of the invention
The object of the present invention is to provide a kind of powder granule grading method and a kind of Zirconium powder casting slurry and its systems
Preparation Method is improved the useful load of Zirconium powder casting slurry by powder granule gradation, and then improves casting molding processes oxygen
Change the intensity of zircon ceramic product, is encountered under processing performance because improving zirconium oxide casting slurry useful load in the prior art to break through
The technical bottleneck of drop.
The present invention provides a kind of powder granule grading methods, comprising: the particle of basic diameter of particle d is pressed close to cubic crystal
Face-centred cubic accumulation mode in system, on the basis of basic diameter of particle d, a certain amount of granularity of gradation is vertical less than or equal to the center of area
The particle of sphenoid and/or octahedra maximal clearance partial size, is filled in it in tetrahedron and/or octahedral interstice.
One according to the present invention specific but non-limiting embodiment, the grain diameter and its volume or weight of gradation
Number are as follows:
Basic 100 parts of d of diameter of particle,
Fill partial size d in tetrahedral interstice4≤ 0.225d≤2.3 part,
Octahedral interstice fills partial size d8≤ 0.414d≤7.1 part.
One according to the present invention specific but non-limiting embodiment, the powder granule grading method are used for oxygen
Change the grain composition of zirconium powder body, silica powder or alumina powder.
One according to the present invention specific but non-limiting embodiment, for the grain composition of Zirconium powder, institute
State diameter of particle d, d4, d8Within the 0.2~1.0um of powder granularity range for being suitble to curtain coating.
One according to the present invention specific but non-limiting embodiment, the grain diameter and its volume or weight of gradation
Number are as follows:
Basic 100 parts of d of diameter of particle,
Fill partial size d in tetrahedral interstice42.3 parts of=0.225d,
Octahedral interstice fills partial size d87.1 parts of=0.414d；
Wherein, the diameter of particle d, d4, d8Within the 0.2~1.0um of powder granularity range for being suitble to curtain coating.
On the other hand, the present invention provides a kind of Zirconium powder casting slurries of high useful load, which is characterized in that described
Zirconium powder pass through such as above-mentioned powder granule grading method gradation.
One according to the present invention specific but non-limiting embodiment, the Zirconium powder casting slurry,
Main component and its parts by weight are as follows:
Wherein, the diameter of particle d, d4, d8Within the scope of 0.2~1.0um.
One according to the present invention specific but non-limiting embodiment, wherein solvent be in toluene or ethyl alcohol at least
It is a kind of；Dispersing agent is triethanolamine；Adhesive is polyvinyl butyral；Plasticiser is BBP(Butyl Benzyl Phthalate；Lubricant
It is polyethylene glycol.
One according to the present invention specific but non-limiting embodiment, the Zirconium powder casting slurry,
Main component and its parts by weight are as follows:
Wherein, the diameter of particle d, d4, d8Within the scope of 0.2~1.0um.
On the other hand, the present invention also provides a kind of preparation method of the Zirconium powder casting slurry of high useful load, institutes
The Zirconium powder stated passes through such as above-mentioned powder granule grading method gradation.
The beneficial effects are mainly reflected as follows:
1. the present invention proposes powder granule grading method according to accumulation mode face-centred cubic in crystallography cubic system,
It is embedded in the particle that granularity is less than or equal to maximal clearance partial size in its tetrahedron and octahedral interstice, is not increasing accumulation body volume
In the case where increase bulk density, and then in subsequent zirconium oxide casting technique, under the premise of guaranteeing processing performance, mention
The high useful load of zirconium oxide casting slurry.
2. Zirconium powder casting slurry of the invention and preparation method thereof can get high useful load using grain composition
Zirconium oxide cast sheet, ceramic dense degree and intensity after firing are improved, and breach in the prior art because improving zirconium oxide stream
Prolong the technical bottleneck that slurry useful load encounters processing performance decline.
Detailed description of the invention
Fig. 1 is the face-centered cubic body Model of powder closest packing.
Fig. 2 is the face-centered cube schematic diagram of powder closest packing.
Fig. 3 is an abstract face-centered cube schematic diagram.
Fig. 4 is a positive tetrahedron ABCD in Fig. 3.
Fig. 5 is the top view of bottom surface DBC in Fig. 4.
Fig. 6 is a regular octahedron DBCEFG in Fig. 3.
Fig. 7 is the top view of face BCEF in Fig. 6.
Fig. 8 is the top view of face AIJK in Fig. 3 face-centered cube.
Specific embodiment
Provided hereinafter specific embodiments to further illustrate the present invention, but the present invention is not limited only to implementation below
Mode.
The present invention proposes a kind of powder granule grade formula according to accumulation mode face-centred cubic in crystallography cubic system
Method.
Basic diameter of particle d, under the closestpacking state in various accumulations, the face-centered cubic close in cubic system
Accumulation mode, close to the virtual condition of face-centered cubic packing, Fig. 3 is an abstract face-centered cube signal by Fig. 1 and Fig. 2
Figure.As shown in figure 3, the particle that granularity is less than or equal to maximal clearance partial size is embedded in its tetrahedron and octahedral interstice, it can be with
Increase bulk density in the case where not increasing accumulation body volume.
According to the solid geometry relationship in crystallography about face-centered cubic lattice structure, tetrahedron and octahedral can be derived
The largest particles partial size that can be filled in body space.
Assuming that dot matrix particle is that rigid ball contacts with adjacent particle.Tetrahedral interstice is vertex particle adjacent with the vertex three
The center of area particle in face forms, and is all rigid ball contact between this four particles if the ABCD in Fig. 3 forms a tetrahedron,
There are gaps at the center of this positive tetrahedron, are put into a filler particles in the gap, and the maximum filler particles that can be put into can
It is contacted with four particle rigid balls.
Fig. 4 is a positive tetrahedron ABCD in Fig. 3, and a filler particles are put into the positive tetrahedron, make the filling
Grain is contacted with four vertex particle rigid balls, and wherein O is the centre of sphere of filler particles, and the radius of filler particles is r4, powder granule
Partial size be d, then AO=OD=1/2d+r4；
Fig. 5 is the top view of bottom surface DBC in Fig. 4, the side length DC=d of equilateral triangle DBC,
Such as Fig. 4, A O1It is the extended line that A point passes through centre of sphere O, perpendicular to the face BCD, in right angled triangle AO1In D,
Then
Such as Fig. 4, in right angled triangle OO1In D,
According to (OO1)2+(DO1)2=(OD)2, OO1=AO1- AO, if AO=OD=l
Then
Then
Then d4=2r4=0.225d.
As a result, according to face-centred cubic accumulation mode, calculating the largest particles partial size filled in tetrahedral interstice is
0.225d。
Next, deriving the largest particles partial size filled in octahedral interstice first.
The octahedron that octahedral interstice is made of six center of area particles, each particle are that rigid ball connects with adjacent particle
Touching, and be not that rigid ball contacts with relative particle, if the DBCEFG in Fig. 3 forms an octahedron, in this regular octahedron
There are gaps at center, are put into a filler particles in the gap, and the maximum filler particles that can be put into can be with six particle rigidity
Ball contact.
Fig. 6 is a regular octahedron DBCEFG in Fig. 3, and a filler particles are put into the regular octahedron, make the filling
Particle is contacted with six vertex particle rigid balls, and wherein O is the centre of sphere of filler particles, and the radius of filler particles is r8, powder
The partial size of grain is d, then DE=d；
Fig. 7 is the top view of face BCEF in Fig. 6, the side length EF=d of square BCEF, the distance OH of centre of sphere O to EF midpoint H
=d/2, EH=d/2,
Such as Fig. 6, in right angled triangle DEH, (DH)2=(DE)2-(EH)2=d2-(d/2)2=3/4d2
Then
Such as Fig. 6, in right angled triangle DOH,
Then
Then d8=0.414d.
As a result, according to face-centred cubic accumulation mode, calculating the largest particles partial size filled in octahedral interstice is
0.414d。
The largest body product that calculating tetrahedral interstice and octahedral interstice can be filled below.If the powder of basic diameter of particle d
Body volume is V, then
The fillable maximum volume V in tetrahedral interstice4max=tetrahedral interstice maximum filler particles volume/face-centred cubic
Stacking volume V；
The fillable maximum volume V of octahedral interstice8max=octahedral interstice maximum filler particles volume/face-centred cubic
Stacking volume V；
Tetrahedral interstice number is 8 in single face-centered cubic body, and octahedral interstice number is 4, then
Tetrahedral interstice maximum filler particles volume=8 × (4/3) π (d4/2)3=8 (1/6) π (0.225d)3=
0.0477d3,
Octahedral interstice maximum filler particles volume=4 × (4/3) π (d8/2)3=4 (1/6) π (0.414d)3=
0.149d3,
As shown in figure 3, face centered cubic side length is a, face-centered cube volume=a3, according to face centered cubic accumulation
Density is 0.74, then face-centred cubic stacking volume=0.74a3,
Fig. 8 is the top view of face AIJK in Fig. 3 face-centered cube, (AI)2+(JI)2=(AJ)2, AJ=2d, 2a2=(2d)2,
Then
The then fillable maximum volume V in tetrahedral interstice4max=tetrahedral interstice maximum filler particles volume/face-centered cubic
Stacking volume V=0.0477d3/2.09d3V=0.023V,
The fillable maximum volume V of octahedral interstice8max=octahedral interstice maximum filler particles volume/face-centred cubic
Stacking volume V=0.149d3/2.09d3V=0.071V.
Calculating the fillable maximum volume in tetrahedral interstice as a result, is 0.023V；The fillable maximum of octahedral interstice
Volume is 0.071V.
In the practical application of Zirconium powder, such as in practical casting slurry system, Zirconium powder particle is being starched
The random collision of Material system has certain probability to form above-mentioned face-centred cubic closestpacking, if grain composition meet it is above-mentioned
The rule of tetrahedron and octahedral interstice filling will play the effect for increasing curtain coating useful load under the premise of guaranteeing casting technique performance
Fruit.
Therefore the present invention proposes a kind of powder granule grading method, comprising: the particle of basic diameter of particle d presses close cube
Face-centred cubic accumulation mode in crystallographic system, on the basis of basic diameter of particle d, a certain amount of granularity of gradation is less than or equal to the center of area
The particle of cube tetrahedron and/or octahedra maximal clearance partial size, is filled in it in tetrahedron and/or octahedral interstice.It is logical
Gradation is crossed, the bulk density of powder is increased in the case where not increasing accumulation body volume.
Specifically, the grain diameter of gradation and its volume or weight number are as follows:
Basic 100 parts of d of diameter of particle,
Fill partial size d in tetrahedral interstice4≤ 0.225d≤2.3 part,
Octahedral interstice fills partial size d8≤ 0.414d≤7.1 part.
Because basic powder and filling powder are same powders, so being indicated with volume parts and parts by weight.
Powder granule grading method of the invention is other than being suitable for Zirconium powder, some other spherical powder such as oxygen
SiClx powder, alumina powder etc. are applicable in.
The Zirconium powder partial size d of curtain coating generally is suitable in 0.2~1.0um, specific surface area is in 6~16m2/ g, therefore, on
State diameter of particle d, d4, d8It should also be within the 0.2~1.0um of powder granularity range for being suitble to curtain coating.
By the Zirconium powder of gradation, in terms of the basic powder of 100 parts by weight, the solvent of 30-60 parts by weight is added, adds
Enter the lubricant of the dispersing agent of 0.1-2 parts by weight, the adhesive of 4-9 parts by weight, the plasticiser of 2-3 parts by weight and 2-3 parts by weight,
The zirconium oxide casting slurry of high useful load is made up of ball grinding method.
Wherein, common substance in casting technique can be used in solvent, dispersing agent, adhesive, plasticiser and lubricant, such as molten
Agent can be toluene, ethyl alcohol etc.；Dispersing agent can be triethanolamine etc.；Adhesive can be polyvinyl butyral etc.；Plasticizing
Agent can be BBP(Butyl Benzyl Phthalate etc.；Lubricant can be polyethylene glycol etc..
It is demonstrated experimentally that the cast sheet by gradation is burnt into tile compared with the cast sheet without gradation is burnt into tile, relatively
Density improves 1.5% or more, and breaking strength improves 5% or more.Therefore, powder granule grading method through the invention, can be with
The zirconium oxide cast sheet of the higher useful load obtained, the ceramic dense degree and intensity after firing are higher.
The present invention is further elaborated combined with specific embodiments below, but the present invention is not limited to following embodiments.
Above and experimental method used in following embodiments is conventional method unless otherwise specified.
Above and the materials, reagents and the like used in the following examples, is commercially available unless otherwise specified.
Embodiment 1
The zirconium oxide casting slurry of high useful load is prepared with following powder grading methods:
The gradation that basic Zirconium powder partial size d is 0.5um calculates d according to above-mentioned powder grading method8=0.207um,
Additional amount is the 7.1% of basic powder；d4=0.113um is not added not in the powder 0.2~1.0um of range for being suitble to curtain coating.Institute
It is 100 parts of powder score of partial size d for 0.5um, partial size d with the optimal powder gradation of the system8For the powder score of 0.207um
7.1 part.The powder that 100 parts of partial size d are 0.5um is replaced to make casting slurry the powder of the gradation.
Casting slurry is the preparation method comprises the following steps: take the Zirconium powder and 7.1 parts by weight that the partial size of 100 parts by weight is 0.5um
Partial size be 0.207um Zirconium powder, be added 40 parts by weight solvent toluene, ethyl alcohol it is fifty-fifty, be added 0.5 parts by weight point
Powder triethanolamine, the adhesive polyethylene butyral of 8 parts by weight, 3 parts by weight plasticiser BBP(Butyl Benzyl Phthalate and 3
The lubricant polyethylene glycol of parts by weight, is made casting slurry by ball grinding method.
The partial size for comparing 100 parts by weight without gradation is the Zirconium powder of 0.5um, and the molten of above-mentioned same component is added
Casting slurry is made by ball grinding method in agent, dispersing agent, adhesive, plasticiser and lubricant.
Above-mentioned casting slurry is made into cast sheet on casting machine, by lambda sensor cast sheet be placed in program-controlled sintering furnace into
Row abjection organic matter and sintering, first dumping before sintering, heating rate control at this time is in 0.2 DEG C/min, and temperature range is at 200 DEG C
~800 DEG C, sintering temperature is set in 1500 DEG C.
Cast sheet firing tile Jing Guo gradation and the cast sheet firing tile without gradation are subjected to consistency and fracture
Intensity contrast.Tile density without gradation is 5.7g/cm3, intensity 1200Mpa；Tile density by gradation is 5.8g/
cm3, intensity 1265Mpa；Tile relative density by gradation improves 1.8%, and intensity improves 5% or more.
Embodiment 2
The zirconium oxide casting slurry of high useful load is prepared with following powder grading methods:
The gradation that basic Zirconium powder partial size d is 0.6um calculates d according to above-mentioned powder grading method8=0.248um,
Additional amount is the 7.1% of basic powder；d4=0.135um is not added not in the powder 0.2~1.0um of range for being suitble to curtain coating.Institute
It is 100 parts of powder score of partial size d for 0.6um, partial size d with the optimal powder gradation of the system8For the powder score of 0.248um
7.1 part.The powder that 100 parts of partial size d are 0.6um is replaced to make casting slurry the powder of the gradation.
Casting slurry is the preparation method comprises the following steps: take the Zirconium powder and 7.1 parts by weight that the partial size of 100 parts by weight is 0.6um
Partial size be 0.248um Zirconium powder, be added 40 parts by weight solvent toluene, ethyl alcohol it is fifty-fifty, be added 0.5 parts by weight point
Powder triethanolamine, the adhesive polyethylene butyral of 8 parts by weight, 3 parts by weight plasticiser BBP(Butyl Benzyl Phthalate and 3
The lubricant polyethylene glycol of parts by weight, is made casting slurry by ball grinding method.
The partial size for comparing 100 parts by weight without gradation is the Zirconium powder of 0.6um, and the molten of above-mentioned same component is added
Casting slurry is made by ball grinding method in agent, dispersing agent, adhesive, plasticiser and lubricant.
Firing process is the same as embodiment 1.Cast sheet firing tile Jing Guo gradation and the cast sheet without gradation are burnt into porcelain
Piece carries out consistency and breaking strength comparison.Tile density without gradation is 5.6g/cm3, intensity 1180Mpa；By grade
The tile density matched is 5.7g/cm3, intensity 1240Mpa；Tile relative density by gradation improves 1.8%, and intensity mentions
It is high by 5%.
Embodiment 3
The zirconium oxide casting slurry of high useful load is prepared with following powder grading methods:
The gradation that basic Zirconium powder partial size d is 1.0um calculates d according to above-mentioned powder grading method8=0.414um,
Additional amount is 7.1%；d4=0.225um, additional amount 2.3%.So the optimal powder gradation of the system is that partial size d is
100 parts of the powder score of 1.0um, partial size d8It is 7.1 parts of powder score of 0.414um, partial size d is the powder score of 0.225um
2.3 part.The powder that 100 parts of partial size d are 1.0um is replaced to make casting slurry the powder of the gradation.
Casting slurry is the preparation method comprises the following steps: take the Zirconium powder and 7.1 parts by weight that the partial size of 100 parts by weight is 1.0um
The partial size Zirconium powder for being 0.414um and 2.3 parts by weight partial size be 0.225um Zirconium powder, be added 40 weight
The solvent toluene, ethyl alcohol of part are fifty-fifty, and the dispersing agent triethanolamine of 0.5 parts by weight, the adhesive polyethylene alcohol contracting of 8 parts by weight is added
The lubricant polyethylene glycol of butyraldehyde, the plasticiser BBP(Butyl Benzyl Phthalate of 3 parts by weight and 3 parts by weight, by ball grinding method system
At casting slurry.
The partial size for comparing 100 parts by weight without gradation is the Zirconium powder of 1.0um, and the molten of above-mentioned same component is added
Casting slurry is made by ball grinding method in agent, dispersing agent, adhesive, plasticiser and lubricant.
Firing process is the same as embodiment 1.Cast sheet firing tile Jing Guo gradation and the cast sheet without gradation are burnt into porcelain
Piece carries out consistency and breaking strength comparison.Tile density without gradation is 5.58g/cm3, intensity 1150Mpa；By grade
The tile density matched is 5.69g/cm3, intensity 1242Mpa；Tile relative density by gradation improves 2%, and intensity mentions
It is high by 8%.
The above is only specific application examples of the invention, are not limited in any way to protection scope of the present invention.All uses
Equivalent transformation or equivalent replacement and the technical solution formed, all fall within rights protection scope of the present invention.
Claims (10)
1. a kind of powder granule grading method, comprising: the particle of basic diameter of particle d is by face-centred cubic close in cubic system
Accumulation mode, on the basis of basic diameter of particle d, a certain amount of granularity of gradation be less than or equal to face-centered cubic tetrahedron and/or
The particle of octahedra maximal clearance partial size, is filled in it in tetrahedron and/or octahedral interstice.
2. the method according to claim 1, the grain diameter and its volume or weight number of gradation are as follows:
Basic 100 parts of d of diameter of particle,
Fill partial size d in tetrahedral interstice4≤ 0.225d≤2.3 part,
Octahedral interstice fills partial size d8≤ 0.414d≤7.1 part.
3. method according to claim 1 or 2, the grain composition for Zirconium powder, silica powder or alumina powder.
4. method according to claim 2, for the grain composition of Zirconium powder, the diameter of particle d, d4, d8It is being suitble to stream
Within the 0.2~1.0um of powder granularity range prolonged.
5. method according to claim 2, the grain diameter and its volume or weight number of gradation are as follows:
Basic 100 parts of d of diameter of particle,
Fill partial size d in tetrahedral interstice42.3 parts of=0.225d,
Octahedral interstice fills partial size d87.1 parts of=0.414d；
Wherein, the diameter of particle d, d4, d8Within the 0.2~1.0um of powder granularity range for being suitble to curtain coating.
6. a kind of Zirconium powder casting slurry of high useful load, which is characterized in that the Zirconium powder passes through such as right
It is required that the powder granule grading method gradation of any one of 1-5.
7. Zirconium powder casting slurry according to claim 6, main component and its parts by weight are as follows:
Wherein, the diameter of particle d, d4, d8Within the scope of 0.2~1.0um.
8. Zirconium powder casting slurry according to claim 7, wherein solvent is at least one of toluene or ethyl alcohol；Dispersion
Agent is triethanolamine；Adhesive is polyvinyl butyral；Plasticiser is BBP(Butyl Benzyl Phthalate；Lubricant is poly- second two
Alcohol.
9. Zirconium powder casting slurry according to claim 7, main component and its parts by weight are as follows:
Wherein, the diameter of particle d, d4, d8Within the scope of 0.2~1.0um.
10. a kind of preparation method of the Zirconium powder casting slurry of high useful load, the Zirconium powder passes through such as right
It is required that the powder granule grading method gradation of any one of 1-5.
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