CN110078497A - Black zirconia feeding and preparation method thereof for ceramic injection forming - Google Patents
Black zirconia feeding and preparation method thereof for ceramic injection forming Download PDFInfo
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- CN110078497A CN110078497A CN201910194969.XA CN201910194969A CN110078497A CN 110078497 A CN110078497 A CN 110078497A CN 201910194969 A CN201910194969 A CN 201910194969A CN 110078497 A CN110078497 A CN 110078497A
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- feeding
- black zirconia
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- zirconia ceramics
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 140
- 239000000919 ceramic Substances 0.000 title claims abstract description 83
- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- 238000002347 injection Methods 0.000 title claims abstract description 26
- 239000007924 injection Substances 0.000 title claims abstract description 26
- 239000000843 powder Substances 0.000 claims abstract description 41
- 238000000034 method Methods 0.000 claims abstract description 34
- 238000002156 mixing Methods 0.000 claims abstract description 27
- 238000001746 injection moulding Methods 0.000 claims abstract description 17
- 239000002002 slurry Substances 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- 239000004200 microcrystalline wax Substances 0.000 claims description 24
- 235000019808 microcrystalline wax Nutrition 0.000 claims description 24
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 21
- 230000003647 oxidation Effects 0.000 claims description 21
- 238000007254 oxidation reaction Methods 0.000 claims description 21
- 230000008569 process Effects 0.000 claims description 21
- 238000010438 heat treatment Methods 0.000 claims description 19
- 239000004793 Polystyrene Substances 0.000 claims description 18
- HVUMOYIDDBPOLL-XWVZOOPGSA-N Sorbitan monostearate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O HVUMOYIDDBPOLL-XWVZOOPGSA-N 0.000 claims description 18
- 229920005606 polypropylene copolymer Polymers 0.000 claims description 18
- 229920002223 polystyrene Polymers 0.000 claims description 18
- -1 sorbitan fatty acid Chemical class 0.000 claims description 17
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 16
- 229930195729 fatty acid Natural products 0.000 claims description 16
- 239000000194 fatty acid Substances 0.000 claims description 16
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 15
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 15
- DQXBYHZEEUGOBF-UHFFFAOYSA-N but-3-enoic acid;ethene Chemical compound C=C.OC(=O)CC=C DQXBYHZEEUGOBF-UHFFFAOYSA-N 0.000 claims description 13
- 239000005038 ethylene vinyl acetate Substances 0.000 claims description 13
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 claims description 13
- 239000002245 particle Substances 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 11
- 238000000227 grinding Methods 0.000 claims description 11
- 229920003023 plastic Polymers 0.000 claims description 11
- 239000004033 plastic Substances 0.000 claims description 11
- 238000001694 spray drying Methods 0.000 claims description 9
- 230000015572 biosynthetic process Effects 0.000 claims description 8
- 239000000049 pigment Substances 0.000 claims description 8
- 238000003786 synthesis reaction Methods 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000002844 melting Methods 0.000 claims description 7
- 230000008018 melting Effects 0.000 claims description 7
- 238000003860 storage Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 6
- 239000012188 paraffin wax Substances 0.000 claims description 6
- 229920001169 thermoplastic Polymers 0.000 claims description 5
- 239000004416 thermosoftening plastic Substances 0.000 claims description 5
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 4
- 239000005977 Ethylene Substances 0.000 claims description 4
- 150000001336 alkenes Chemical class 0.000 claims description 4
- JNYAEWCLZODPBN-JGWLITMVSA-N (2r,3r,4s)-2-[(1r)-1,2-dihydroxyethyl]oxolane-3,4-diol Chemical compound OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O JNYAEWCLZODPBN-JGWLITMVSA-N 0.000 claims description 3
- 238000001125 extrusion Methods 0.000 claims description 3
- 230000008676 import Effects 0.000 claims description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 2
- 230000035611 feeding Effects 0.000 claims 16
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims 3
- 229920005862 polyol Polymers 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 8
- 238000005245 sintering Methods 0.000 abstract description 3
- 238000005469 granulation Methods 0.000 abstract 1
- 230000003179 granulation Effects 0.000 abstract 1
- 229910010293 ceramic material Inorganic materials 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 229910052573 porcelain Inorganic materials 0.000 description 4
- 238000013001 point bending Methods 0.000 description 3
- 238000000889 atomisation Methods 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 229910052845 zircon Inorganic materials 0.000 description 2
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 2
- UPZFLZYXYGBAPL-UHFFFAOYSA-N 2-ethyl-2-methyl-1,3-dioxolane Chemical compound CCC1(C)OCCO1 UPZFLZYXYGBAPL-UHFFFAOYSA-N 0.000 description 1
- 229920000265 Polyparaphenylene Polymers 0.000 description 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000320 mechanical mixture Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63496—Bituminous materials, e.g. tar, pitch
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9646—Optical properties
- C04B2235/9661—Colour
Abstract
The present invention relates to a kind of preparation methods of black zirconia feeding for ceramic injection forming, including the preparation to nanoscale black zirconia ceramics powder and organic carrier, then nanoscale black zirconia ceramics powder and organic carrier are subjected to mixing and prepare black zirconia ceramics feeding presoma, last black zirconia ceramics feeding presoma obtains the feeding of black zirconia ceramics injection moulding after the granulation of ceramic facility for granulating.It is sintered using the temperature that the feeding of the nanoscale black zirconia ceramics material injection molding of above method preparation can be used in 1400 DEG C or more, and injection property is good, thermal debinding is had excellent performance, the black zirconia ceramics color articles that sintering comes out are uniform, and product surface does not have stomata generation.
Description
Technical field
The invention belongs to new material production technical fields, and in particular to a kind of black zirconia for ceramic injection forming
Feeding and preparation method thereof.
Background technique
The injection molding technology and technique of ceramic material are the injection molding technologies via thermoplastic to metal powder
Injection molding technology arrive the injection molding technologies of ceramic powders again and develop, be that a kind of novel ceramic material forms skill only
Art.How using the performance advantage of ceramic material itself consumer electronics product (usually described 3C electronic product) institute is prepared
The ceramic part of the various precisions needed is the project that last decade carrys out ceramic material field primary study.
And the feeding for being used to prepare ceramic material is then one of key technology, and it is wide to prepare ceramic injection forming feeding at present
It is general using color zirconium oxide feeding, the process of feeding preparation be added after binder to be heated to molten condition ceramic powders into
The method of row mechanical mixture.This method operation temperature is high, and uniformity is less desirable, and binder cannot be coated on pottery well
The surface of porcelain powder is easy to leave hole after degreasing sintered, it is difficult to meet the needs of high-quality ceramics appearance member.
Summary of the invention
The present invention for the technical problems in the prior art, provide one kind can be directly used for carry out ceramic injection at
Type and with excellent thermal debinding performance and the black zirconia feeding with environmental protection characteristic and preparation method thereof.
The technical scheme to solve the above technical problems is that
A kind of preparation method of the black zirconia feeding for ceramic injection forming, specifically includes following processing step:
A, the preparation of nanoscale black zirconia ceramics powder:
By high temperature resistant black pigment and Zirconium oxide powder according to (2~5): 100 ratio mixes；
By mixture and deionized water according to (45~65) after mixing: 100 ratio is put into tumbling ball mill, is turned
30~45 revs/min, pre-grinding 2~8 hours of speed；The slurry of pre- milled is transferred in high-speed grinder again, setting grinder turns
600~900 revs/min of speed is ground 2~8 hours；
Slurry after grinding is transferred in vacuum storage tank, slurry is spray-dried, prepares black zirconia pottery
Porcelain powder；
B, organic carrier is synthetically prepared:
Paraffin is added with thermoplastic a variety of low-molecular-weight organic matters in the case where vacuum degree is the vacuum state of 0~1Mpa
Temperature is to 100~200 DEG C and is sufficiently stirred 30~90 minutes, the organic carrier synthesized；
Organic carrier will be synthesized to be transferred in plastics facility for granulating, prepare the circle of 1~5mm of diameter, 1~5mm of thickness
Column organic carrier particle；
C, the preparation of black zirconia ceramics feeding presoma:
By the nanoscale black oxidation zirconium powder after exhausted water process with organic carrier particle according to (70-85): (30-15's)
Ratio, which is put into mixing equipment, carries out mixing processing, and 100-200 DEG C of mixing processing temperature, the operating pressure of mixing equipment is arranged
10-100kgf, setting mixing duration 45-90min, prepare black zirconia ceramics feeding forerunner after multiple mixing operation
Body；
D, the black zirconia ceramics injection moulding preparation of feeding:
The black zirconia ceramics feeding presoma that will be prepared, set temperature is in 80-120 on ceramic facility for granulating
DEG C, setting extrusion pressure 50-150kgf/cm2, setting 60-120 revs/min of cutter rotating velocity, prepare black zirconia ceramics note
Penetrate molding feeding.
As the preferred of the embodiment of the present invention, in the preparation process of nanoscale black zirconia ceramics powder, spraying
When dry, it is arranged 160~240 DEG C of spray drying device inlet temperature, 80~150 DEG C of outlet temperature, vacuum tank atomizing disk is set
6000~9000 revs/min of revolving speed.
As the preferred of the embodiment of the present invention, the partial size of the nanoscale black zirconia ceramics powder prepared is 100~
150 nanometers, specific surface area are as follows: 6~12g/m2.
As the preferred of the embodiment of the present invention, the paraffin is microcrystalline wax.
As the preferred of the embodiment of the present invention, a variety of low-molecular-weight organic matters poly-, ethylene -- acetic acid by polypropylene copolymer
Ethylene rouge, low-molecular-weight polystyrene, Span 60, sorbitan fatty acid composition.
As the preferred of the embodiment of the present invention, polypropylene copolymer is poly-, ethylene -- vinyl acetate, low molecular weight polyphenylene second
Alkene, Span 60, the proportion of sorbitan fatty acid are denoted as by weight percentage: (40-50): (5-15): (30-40): (1-
5): (1-5).
As the preferred of the embodiment of the present invention, microcrystalline wax, polypropylene copolymer be poly-, ethylene -- vinyl acetate, low point
Son amount polystyrene, Span 60, its sour synthetic ratio of sorbitan fatty are denoted as (15-25): (40- by weight percentage
50): (5-15): (30-40): (1-5): (1-5).
First microcrystalline wax is added to during carrying out organic carrier synthesis as the preferred of the embodiment of the present invention
In vacuum tank with heating, setting 100 DEG C of heating temperature or more, after the microcrystalline wax in tank all melting, then by polypropylene
Copolymer is poly-, ethylene -- vinyl acetate, low-molecular-weight polystyrene, Span 60, sorbitan fatty acid are all added to
In the vacuum tank.
As the preferred of the embodiment of the present invention, in the process for carrying out exhausted water process to nanoscale black oxidation zirconium powder are as follows:
Nanoscale black oxidation zirconium powder is put into vacuum microwave drying case, the vacuum degree being arranged in vacuum microwave drying case is 0-
0.1Mpa, setting temperature are 45~85 DEG C, and the setting time is to carry out exhausted water process in 30~60 minutes.
The embodiment of the present invention provides a kind of black oxidation for ceramic injection forming prepared according to aforementioned preparation step
Zirconium feeding.
The beneficial effects of the present invention are:
1, the black zirconia feeding for ceramic injection forming of the invention will be by that will prepare nanoscale black oxidation
Zircon ceramic powder and the organic carrier synthesized carry out mixing in mixing equipment and obtain black zirconia ceramics feeding presoma,
Finally black zirconia ceramics feeding presoma is pelletized obtain on plastics facility for granulating can injection moulding it is black
Color zirconia ceramics feeding enables the black zirconia ceramics feeding prepared directly to be injection moulded and had excellent
Different thermal debinding performance and the ceramic raw material with environmental protection characteristic.
2, the present invention uses black zirconia feeding by what the above method was prepared, can be used in 1400 DEG C or more of temperature
It is sintered, and injection property is good, thermal debinding is had excellent performance, the black zirconia ceramics color articles for being sintered out are uniform, system
Product surface does not have stomata generation, and the four-point bending intensity of product is up to 1200kgf/cm2More than.
Detailed description of the invention
Fig. 1 is the present invention in the process flow chart of the black zirconia feeding preparation method of ceramic injection forming.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Shown in Figure 1, the embodiment of the present invention provides a kind of system of black zirconia feeding for ceramic injection forming
Preparation Method specifically includes tetra- processing steps of A, B, C, D, wherein technique A and technique B can be carried out successively according to the actual situation
The adjustment of sequence.We are respectively described in detail four techniques (tetra- processing steps of A, B, C, D) below.
A, the preparation of nanoscale black zirconia ceramics powder:
1. by high temperature resistant black pigment and Zirconium oxide powder in (2~5): 100 ratio mixes, in the present embodiment
In, the preferred TYSZ-FS/FS-SD Zirconium oxide powder of Zirconium oxide powder aoxidizes high temperature resistant black pigment and TYSZ-FS/FS-SD
Zirconium powder is put into blender and is uniformly mixed.
After 2. high temperature black colorant and Zirconium oxide powder mix, by the mixture and deionized water according to (45~
65): 100 ratio is put into tumbling ball mill, and the revolving speed of setting drum ball mill is 30-45 revs/min, and pre-grinding 2~8 is small
When, then the slurry of pre- milled is transferred in high-speed grinder, it is arranged 600~900 revs/min of grinder rotating speed, grinding 2~8
Hour, stop after measuring slurry partial size less than 150 nanometers, then releases slurry.
3. the slurry after grinding is transferred in vacuum storage tank, it is sprayed after slurry bubble is removed in vacuum, then to slurry
It is dry, when spray drying, 160~240 DEG C of temperature of setting spray drying device import, it is arranged 80~150 DEG C of outlet temperature, if
6000~9000 revs/min of disk rotating speed of atomization is set, black zirconia ceramics powder is finally obtained.In the present embodiment, by upper
Stating step makes the partial size for the nanoscale black zirconia ceramics powder prepared remain 100~150nm, specific surface area are as follows: 6
~12g/m2。
B, organic carrier is synthetically prepared:
1. by paraffin and having thermoplastic a variety of low-molecular-weight organic matters in the case where vacuum degree is the vacuum state of 0~1Mpa
It is heated up to 100~200 DEG C and is sufficiently stirred 30~90 minutes, synthesize organic carrier.
In the present embodiment, the preferred microcrystalline wax of paraffin.A variety of low-molecular-weight organic matters poly-, second by polypropylene copolymer
Alkene -- vinyl acetate, low-molecular-weight polystyrene, Span 60, sorbitan fatty acid composition, above-mentioned low molecular weight are organic
Object it is as follows by weight ratio: (40-50): (5-15): (30-40): (1-5): (1-5).Wherein, microcrystalline wax, poly- third
Alkene copolymer is poly-, ethylene -- its sour synthesis of vinyl acetate, low-molecular-weight polystyrene, Span 60, sorbitan fatty is matched
Than being denoted as (15-25) by weight percentage: (40-50): (5-15): (30-40): (1-5): (1-5).
In the present embodiment, during carrying out organic carrier synthesis, first microcrystalline wax is added to the true of heating
In slack tank, 100 DEG C of heating temperature of setting or more, after the microcrystalline wax in tank all melting, then the poly-, second by polypropylene copolymer
Alkene -- vinyl acetate, low-molecular-weight polystyrene, Span 60, sorbitan fatty acid are all added to according to said ratio
In the vacuum tank, then vacuum tank is extracted under vacuum degree to the vacuum state of 0-1Mpa, 100-200 DEG C is heated up to and sufficiently stirs
It mixes 30-90 minutes and synthesizes required organic carrier.
2. organic carrier will be synthesized to be transferred in plastics facility for granulating, by the temperature setting of plastics facility for granulating in 90-
180 DEG C, prepare the cylindric organic carrier particle of 1~5mm of diameter, 1~5mm of thickness.
C, the preparation of black zirconia ceramics feeding presoma:
1. by the nanoscale black oxidation zirconium powder prepared in technique A and technique B and organic carrier (specially airborne body
Particle) by weight ratio (70-85): the ratio of (30-15) is configured.In the present embodiment, nanoscale black oxidation zirconium powder
Nanoscale black oxidation zirconium powder is first put into vacuum microwave drying case before configuration and carries out exhausted water process by end.
Specific exhausted water treatment procedure are as follows: nanoscale black oxidation zirconium powder is put into vacuum microwave drying case, is arranged
Vacuum degree in vacuum microwave drying case is -0.1Mpa, and setting temperature is 50~75 DEG C, and the setting time is to carry out for 30~60 minutes
Moisture solution in powder is down to the state of 0-0.2% by exhausted water process.
2. the nanoscale black oxidation zirconium powder after exhausted water process and aforementioned organic carrier particle will be carried out according to (70-
85): the ratio of (30-15) be put into can Self-pressurizing agri and heating hermetic type it is intracavitary, 100-200 DEG C of setting type chamber processing temperature,
Operating pressure 10-100kgf, setting mixing duration 45-90 minutes is set, it is (close in the present embodiment after multiple mixing operation
Refining 1-5 times) it prepares with good fluidity and thermoplastic black zirconia ceramics feeding presoma.
D, the black zirconia ceramics injection moulding preparation of feeding:
By the aforementioned made black zirconia ceramics feeding presoma got ready, set temperature exists on ceramic facility for granulating
80-120 DEG C, setting extrusion pressure 50-150kgf/cm2, setting 60-120 revs/min of revolving speed of cutter, to prepare particle
Size are as follows: the feeding of the black zirconia ceramics material injection molding of diameter 3-5mm, length 1-3mm.
We are by specific embodiment part (following embodiment unless otherwise specified, then without containing except inevitable below
Impurity other than other the components pointed out are not known) present invention is further described in detail:
Embodiment one:
1. high temperature resistant black pigment and TYSZ-FS/FS-SD Zirconium oxide powder are mixed in the ratio of 2:100, then
It is put into drum ball mill according to the ratio and deionized water of 45:100, the revolving speed that tumbling ball mill is arranged is 35 revs/min,
Pre-grinding 8 hours, then the slurry of pre- milled is transferred in high-speed grinder, while being arranged 800 revs/min of grinder rotating speed, it grinds
Mill 2.5 hours after measuring slurry partial size less than 150 nanometers, then slurry is transferred in vacuum storage tank, slurry gas is removed in vacuum
After bubble, then slurry is spray-dried, when spray drying, setting out temperature is respectively as follows: 180 DEG C and 90 DEG C, setting mist
Change 6000 revs/min of disk rotating speed, so that preparing powder diameter is 150 nanometers, specific surface area are as follows: 10g/m2Black zirconia
Ceramic powders.
2. by microcrystalline wax, polypropylene copolymer, ethylene -- vinyl acetate, Span 60, loses low-molecular-weight polystyrene
Water sorbitan fatty acid, the by weight percentage proportional arrangement of 20:40:5:30:1:4 are good, then, are first added to microcrystalline wax
In vacuum tank with heating, it is arranged 120 DEG C of heating temperature, after the microcrystalline wax in tank all melting, then by Polypropylene copolymer
Object is poly-, ethylene -- vinyl acetate, low-molecular-weight polystyrene, Span 60, sorbitan fatty acid are all added to this very
In slack tank, vacuum degree is extracted to -0.1Mpa, required for setting heating temperature synthesizes after being 120 DEG C, strong stirring 80 minutes
Organic carrier.Then, the organic carrier of the synthesis is transferred in plastics facility for granulating, the temperature of plastics facility for granulating is set
It is 100 DEG C, prepares the columned organic carrier particle of diameter 5mm, thickness 1mm.
3. the ratio of nanoscale black oxidation zirconium powder and the organic carrier 70:30 by weight percentage prepared is carried out
Configuration, meanwhile, configured nanoscale black oxidation zirconium powder be arranged in vacuum microwave drying case vacuum degree for-
0.1Mpa, setting temperature are 50 DEG C, and the setting time is to carry out exhausted water process in 60 minutes, then will carry out the black after exhausted water process
Zirconium oxide powder is gone in mixing equipment, and pressure 40kgf is arranged, when setting in 30 revs/min of revolving speed of setting, 150 DEG C of temperature of setting
Between 60 minutes, configured organic carrier is also added to the equipment again after the setting temperature in equipment is consistent with observed temperature
It is interior, mixing is carried out after closed, to prepare presoma needed for feeding.
4. the presoma needed for prepared by feeding goes to set temperature on dedicated ceramic facility for granulating and squeezes out in 80 DEG C, setting
Pressure 80kgf/cm2, setting 100 revs/min of cutter rotating velocity, to prepare granular size are as follows: diameter 3mm, length 2mm's is black
The feeding of color zirconia ceramics material injection moulding.
Embodiment two:
1. high temperature resistant black pigment and TYSZ-FS/FS-SD Zirconium oxide powder are mixed in the ratio of 3:100, then
It is put into drum ball mill according to the ratio and deionized water of 50:100, the revolving speed that tumbling ball mill is arranged is 40 revs/min,
Pre-grinding 6 hours, then the slurry of pre- milled is transferred in high-speed grinder, while being arranged 600 revs/min of grinder rotating speed, it grinds
Mill 7 hours after measuring slurry partial size less than 150 nanometers, then slurry is transferred in vacuum storage tank, through slurry bubble is removed in vacuum
Afterwards, then to slurry it is spray-dried, when spray drying, setting out temperature is respectively as follows: 200 DEG C and 100 DEG C, and setting is atomized
7000 revs/min of disk rotating speed, so that preparing powder diameter is 150 nanometers, specific surface area are as follows: 10g/m2Black zirconia pottery
Porcelain powder.
2. by microcrystalline wax, polypropylene copolymer, ethylene -- vinyl acetate, Span 60, loses low-molecular-weight polystyrene
Water sorbitan fatty acid, the by weight percentage proportional arrangement of 15:42:8:32:1:2 are good, then, are first added to microcrystalline wax
In vacuum tank with heating, it is arranged 130 DEG C of heating temperature, after the microcrystalline wax in tank all melting, then by Polypropylene copolymer
Object is poly-, ethylene -- vinyl acetate, low-molecular-weight polystyrene, Span 60, sorbitan fatty acid are all added to this very
In slack tank, vacuum degree is extracted to -0.1Mpa, setting heating temperature is 150 DEG C, required for strong stirring synthesizes after sixty minutes
Organic carrier.Then, the organic carrier of the synthesis is transferred in plastics facility for granulating, the temperature of plastics facility for granulating is set
It is 120 DEG C, prepares the columned organic carrier particle of diameter 3mm, thickness 2mm.
3. the ratio of nanoscale black oxidation zirconium powder and the organic carrier 80:20 by weight percentage prepared is carried out
Configuration, meanwhile, configured nanoscale black oxidation zirconium powder be arranged in vacuum microwave drying case vacuum degree for-
0.1Mpa, setting temperature are 60 DEG C, and the setting time is to carry out exhausted water process in 50 minutes, then will carry out the black after exhausted water process
Zirconium oxide powder is gone in mixing equipment, and pressure 25kgf is arranged, when setting in 45 revs/min of revolving speed of setting, 120 DEG C of temperature of setting
Between 70 minutes, configured organic carrier is also added to the equipment again after the setting temperature in equipment is consistent with observed temperature
It is interior, mixing is carried out after closed, to prepare presoma needed for feeding.
4. the presoma needed for prepared by feeding goes to set temperature on dedicated ceramic facility for granulating and squeezes in 100 DEG C, setting
Pressure 60kgf/cm out2, setting 60 revs/min of cutter rotating velocity, to prepare granular size are as follows: diameter 4mm, length 2.5mm
Black zirconia ceramics material injection molding feeding.
Embodiment three:
1. high temperature resistant black pigment and TYSZ-FS/FS-SD Zirconium oxide powder are mixed in the ratio of 3.5:100, so
It is put into drum ball mill according to the ratio of 55:100 and deionized water afterwards, the revolving speed that tumbling ball mill is arranged is 35 revs/min
Clock, pre-grinding 5 hours, then the slurry of pre- milled is transferred in high-speed grinder, meanwhile, it is arranged 700 revs/min of grinder rotating speed
Clock is ground 5 hours, after measuring slurry partial size less than 150 nanometers, then slurry is transferred in vacuum storage tank, slurry is removed in vacuum
After expecting bubble, then slurry being spray-dried, when spray drying, setting out temperature is respectively as follows: 220 DEG C and 120 DEG C, if
6500 revs/min of disk rotating speed of atomization is set, so that preparing powder diameter is 150 nanometers, specific surface area 10g/m2Black oxygen
Change zircon ceramic powder.
2. by microcrystalline wax, polypropylene copolymer, ethylene -- vinyl acetate, Span 60, loses low-molecular-weight polystyrene
Water sorbitan fatty acid, by weight percentage 17:43:6:30:2:2 proportional arrangement are good, then, microcrystalline wax are first added to band
In the vacuum tank of heating, it is arranged 125 DEG C of heating temperature, after the microcrystalline wax in tank all melting, then by polypropylene copolymer
Poly-, ethylene -- vinyl acetate, low-molecular-weight polystyrene, Span 60, sorbitan fatty acid are all added to the vacuum
In tank, vacuum degree is extracted to negative 0.1Mpa, it is 150 DEG C that heating temperature, which is arranged, required for strong stirring synthesizes after forty minutes
Organic carrier.Then, the organic carrier of the synthesis is transferred in plastics facility for granulating, prepares size and exist: diameter
The columned organic carrier particle of 3.5mm, thickness 2mm；
3. the ratio of nanoscale black oxidation zirconium powder and the organic carrier 75:25 by weight percentage prepared is carried out
Configuration, meanwhile, configured nanoscale black oxidation zirconium powder be arranged in vacuum microwave drying case vacuum degree for-
0.1Mpa, setting temperature are 70 DEG C, and the setting time is to carry out exhausted water process in 40 minutes, then will carry out the black after exhausted water process
Zirconium oxide powder is gone in mixing equipment, and pressure 60kgf is arranged, when setting in 45 revs/min of revolving speed of setting, 150 DEG C of temperature of setting
Between 50 minutes, configured organic carrier is also added to the equipment again after the setting temperature in equipment is consistent with observed temperature
It is interior, mixing is carried out after closed, to prepare presoma needed for feeding.
4. the presoma needed for prepared by feeding goes to set temperature on dedicated ceramic facility for granulating and squeezes out in 90 DEG C, setting
Pressure 120kgf/cm2, setting 100 revs/min of cutter rotating velocity, to prepare granular size are as follows: diameter 3.5mm, length
The feeding of the black zirconia ceramics material injection molding of 1.5mm.
Example IV:
1. high temperature resistant black pigment and TYSZ-FS/FS-SD Zirconium oxide powder are mixed in the ratio of 4.5:100, so
It is put into drum ball mill according to the ratio of 65:100 and deionized water afterwards, setting drum drum's speed of rotation is 40 revs/min,
Pre-grinding 6 hours, then the slurry of pre- milled is transferred in high-speed grinder, meanwhile, it is arranged 500 revs/min of grinder rotating speed, grinds
Mill 6 hours after measuring slurry partial size less than 150 nanometers, then slurry is transferred in vacuum storage tank, through slurry bubble is removed in vacuum
Afterwards, then to slurry it is spray-dried, when spray drying, setting out temperature is respectively as follows: 200 DEG C and 100 DEG C, and setting is atomized
8500 revs/min of disk rotating speed, so that preparing powder diameter is 150 nanometers, specific surface area 10g/m2Black zirconia pottery
Porcelain powder.
2. by microcrystalline wax, polypropylene copolymer, ethylene -- vinyl acetate, Span 60, loses low-molecular-weight polystyrene
Water sorbitan fatty acid, the by weight percentage proportional arrangement of 18:40:6:30:4:2 are good, then, are first added to microcrystalline wax
In vacuum tank with heating, it is arranged 100 DEG C of heating temperature, after the microcrystalline wax in tank all melting, then by Polypropylene copolymer
Object is poly-, ethylene -- vinyl acetate, low-molecular-weight polystyrene, Span 60, sorbitan fatty acid are all added to this very
In slack tank, vacuum degree is extracted to -0.1Mpa, required for setting heating temperature synthesizes after being 150 DEG C, strong stirring 40 hours
Organic carrier.Then, the organic carrier of the synthesis is transferred in plastics facility for granulating, prepares size and exists: diameter 3mm,
The columned organic carrier particle of thickness 3mm；
3. the ratio of nanoscale black oxidation zirconium powder and the organic carrier 80:20 by weight percentage prepared is carried out
Configuration, meanwhile, configured nanoscale black oxidation zirconium powder be arranged in vacuum microwave drying case vacuum degree for-
0.1Mpa, setting temperature are 70 DEG C, and the setting time is to carry out exhausted water process in 40 minutes, then will carry out the black after exhausted water process
Zirconium oxide powder is gone in mixing equipment, and pressure 80kgf is arranged, when setting in 50 revs/min of revolving speed of setting, 150 DEG C of temperature of setting
Between 50 minutes, configured organic carrier is also added to the equipment again after the setting temperature in equipment is consistent with observed temperature
It is interior, mixing is carried out after closed, to prepare presoma needed for feeding.
4. the presoma needed for prepared by feeding goes to set temperature on dedicated ceramic facility for granulating and squeezes in 110 DEG C, setting
Pressure 100kgf/cm out2, setting 100 revs/min of cutter rotating velocity, to prepare granular size are as follows: diameter 3mm, length 2mm
Black zirconia ceramics material injection molding feeding.
We use the black zirconia ceramics material injection molding prepared in above-described embodiment by testing below
Feeding tested:
The feeding prepared into example IV of embodiment one is passed through subsequent injection moulding, thermal debinding and height by us
The black zirconia ceramics testing piece of 45 × 45 × 2mm is prepared after temperature sintering, to carrying out after the density of testing piece, mirror finish
SEM scanning situation and carry out testing piece is cut into the four-point bending intensity measured after the strip of 3 × 4 × 45mm
It is as shown in the table:
| Testing piece density (g/cm3) | SEM scanning | Four-point bending intensity (kgf/cm2) | |
| Embodiment one | 6.02 | Pore-free | 1342 |
| Embodiment two | 6.08 | Pore-free | 1365 |
| Embodiment three | 6.05 | Pore-free | 1358 |
| Example IV | 6.07 | Pore-free | 1326 |
Table 1
It will be seen that the subsequent injection of black zirconia feeding prepared by aforementioned preparation process from table 1
The black zirconia ceramics testing piece that 45 × 45 × 2mm is prepared after molding, thermal debinding and high temperature sintering can satisfy essence completely
The requirement of close ceramic part.
Each constituent component in above embodiments can be combined adjustment according to the actual situation, for simplicity of description, not
Combination all possible to each technical characteristic in above-described embodiment is all described, as long as however, these technical characteristics
Contradiction is not present in combination, all should be considered as described in this specification.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of the black zirconia feeding for ceramic injection forming, which is characterized in that including following technique,
A, the preparation of nanoscale black zirconia ceramics powder:
By high temperature resistant black pigment and Zirconium oxide powder according to (2~5): 100 ratio mixes；
By mixture and deionized water according to (45~65) after mixing: 100 ratio is put into tumbling ball mill, revolving speed 30
~45 revs/min, pre-grinding 2~8 hours；The slurry of pre- milled is transferred in high-speed grinder again, grinder rotating speed 600 is set
It~900 revs/min, grinds 2~8 hours；
Slurry after grinding is transferred in vacuum storage tank, slurry is spray-dried, prepares black zirconia ceramics powder
End；
B, organic carrier is synthetically prepared:
Paraffin is heated up to with thermoplastic a variety of low-molecular-weight organic matters in the case where vacuum degree is the vacuum state of 0~1Mpa
It 100~200 DEG C and is sufficiently stirred 30~90 minutes, the organic carrier synthesized；
Organic carrier will be synthesized to be transferred in plastics facility for granulating, prepare 1~5mm of diameter, 1~5mm of thickness it is cylindric
Organic carrier particle；
C, the preparation of black zirconia ceramics feeding presoma:
By after exhausted water process nanoscale black oxidation zirconium powder and organic carrier particle according to (70-85): the ratio of (30-15)
It is put into mixing equipment and carries out mixing processing, 100-200 DEG C of mixing processing temperature, the operating pressure 10- of mixing equipment are set
100kgf, setting mixing duration 45-90min, prepare black zirconia ceramics feeding presoma after multiple mixing operation；
D, the black zirconia ceramics injection moulding preparation of feeding:
The black zirconia ceramics feeding presoma that will be prepared, on ceramic facility for granulating set temperature 80-120 DEG C, set
Determine extrusion pressure 50-150kgf/cm2, setting 60-120 revs/min of cutter rotating velocity, prepare black zirconia ceramics and be injected into
Type feeding.
2. the preparation method of the black zirconia feeding according to claim 1 for ceramic injection forming, feature exist
In: in the preparation process of nanoscale black zirconia ceramics powder, in spray drying, spray drying device import temperature is set
160~240 DEG C of degree, 80~150 DEG C of outlet temperature, setting vacuum tank is atomized 6000~9000 revs/min of disk rotating speed.
3. the preparation method of the black zirconia feeding according to claim 1 for ceramic injection forming, feature exist
In: the partial size for the nanoscale black zirconia ceramics powder prepared is 100~150 nanometers, specific surface area are as follows: 6~12g/m2。
4. the preparation method of the black zirconia feeding according to claim 1 for ceramic injection forming, feature exist
In: the paraffin is microcrystalline wax.
5. the preparation method of the black zirconia feeding according to claim 4 for ceramic injection forming, feature exist
In: a variety of low-molecular-weight organic matters poly-, ethylene -- vinyl acetate, low-molecular-weight polystyrene, Span by polypropylene copolymer
60, sorbitan fatty acid forms.
6. the preparation method of the black zirconia feeding according to claim 5 for ceramic injection forming, feature exist
The poly-, ethylene in: polypropylene copolymer -- vinyl acetate, low-molecular-weight polystyrene, Span 60, sorbitan fatty acid
Proportion is denoted as by weight percentage: (40-50): (5-15): (30-40): (1-5): (1-5).
7. the preparation method of the black zirconia feeding according to claim 5 for ceramic injection forming, feature exist
In: microcrystalline wax, polypropylene copolymer is poly-, ethylene -- vinyl acetate, low-molecular-weight polystyrene, Span 60, Sorbitan
Its synthetic ratio of polyol fatty acid is denoted as (15-25) by weight percentage: (40-50): (5-15): (30-40): (1-5): (1-5).
8. according to the preparation method of the described in any item black zirconia feedings for ceramic injection forming of claim 4 to 7,
It is characterized by: first microcrystalline wax is added in the vacuum tank with heating during carrying out organic carrier synthesis, setting
100 DEG C of heating temperature or more, after the microcrystalline wax in tank all melting, then poly-, ethylene -- the acetic acid second by polypropylene copolymer
Alkene rouge, low-molecular-weight polystyrene, Span 60, sorbitan fatty acid are all added in the vacuum tank.
9. according to right want 1 described in for ceramic injection forming black zirconia feeding preparation method, which is characterized in that
In the process for carrying out exhausted water process to nanoscale black oxidation zirconium powder are as follows: it is micro- that nanoscale black oxidation zirconium powder is put into vacuum
In wave drying box, the vacuum degree being arranged in vacuum microwave drying case is 0-0.1Mpa, and setting temperature is 45~85 DEG C, and the time is arranged
Exhausted water process was carried out for 30~60 minutes.
10. a kind of preparation method preparation of black zirconia feeding according to claim 1 for ceramic injection forming
Black zirconia feeding for ceramic injection forming.
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