CN110357589A - A kind of Aqueous injection moulding process of structural ceramics - Google Patents
A kind of Aqueous injection moulding process of structural ceramics Download PDFInfo
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- CN110357589A CN110357589A CN201910643076.9A CN201910643076A CN110357589A CN 110357589 A CN110357589 A CN 110357589A CN 201910643076 A CN201910643076 A CN 201910643076A CN 110357589 A CN110357589 A CN 110357589A
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- ceramic
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- injection
- ceramics
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- 239000000919 ceramic Substances 0.000 title claims abstract description 135
- 238000001746 injection moulding Methods 0.000 title claims abstract description 24
- 238000002347 injection Methods 0.000 claims abstract description 52
- 239000007924 injection Substances 0.000 claims abstract description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000000843 powder Substances 0.000 claims abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 238000005245 sintering Methods 0.000 claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 13
- 239000004615 ingredient Substances 0.000 claims abstract description 10
- 239000013008 thixotropic agent Substances 0.000 claims abstract description 9
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 8
- 239000003054 catalyst Substances 0.000 claims abstract description 7
- 239000002270 dispersing agent Substances 0.000 claims abstract description 7
- 239000003999 initiator Substances 0.000 claims abstract description 7
- 238000002360 preparation method Methods 0.000 claims abstract description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 87
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 56
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 22
- 238000007711 solidification Methods 0.000 claims description 20
- 230000008023 solidification Effects 0.000 claims description 20
- JIGUICYYOYEXFS-UHFFFAOYSA-N 3-tert-butylbenzene-1,2-diol Chemical compound CC(C)(C)C1=CC=CC(O)=C1O JIGUICYYOYEXFS-UHFFFAOYSA-N 0.000 claims description 12
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 12
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 11
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims description 11
- 239000002994 raw material Substances 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 10
- 229920000193 polymethacrylate Polymers 0.000 claims description 10
- 239000004952 Polyamide Substances 0.000 claims description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-O ammonium group Chemical group [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 9
- 238000002844 melting Methods 0.000 claims description 9
- 230000008018 melting Effects 0.000 claims description 9
- 229920002647 polyamide Polymers 0.000 claims description 9
- 238000007670 refining Methods 0.000 claims description 9
- KWYHDKDOAIKMQN-UHFFFAOYSA-N N,N,N',N'-tetramethylethylenediamine Chemical compound CN(C)CCN(C)C KWYHDKDOAIKMQN-UHFFFAOYSA-N 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 239000003112 inhibitor Substances 0.000 claims description 7
- 238000006116 polymerization reaction Methods 0.000 claims description 7
- KFIGICHILYTCJF-UHFFFAOYSA-N n'-methylethane-1,2-diamine Chemical compound CNCCN KFIGICHILYTCJF-UHFFFAOYSA-N 0.000 claims description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 3
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 3
- 229910052574 oxide ceramic Inorganic materials 0.000 claims description 2
- 239000011224 oxide ceramic Substances 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 23
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000000605 extraction Methods 0.000 abstract description 4
- 238000000465 moulding Methods 0.000 abstract description 4
- 239000005416 organic matter Substances 0.000 abstract description 4
- 239000000178 monomer Substances 0.000 abstract description 3
- 230000001681 protective effect Effects 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000004132 cross linking Methods 0.000 abstract description 2
- 238000012797 qualification Methods 0.000 abstract description 2
- 238000004898 kneading Methods 0.000 abstract 1
- 230000007547 defect Effects 0.000 description 7
- 238000005238 degreasing Methods 0.000 description 7
- 239000007787 solid Substances 0.000 description 6
- 239000001993 wax Substances 0.000 description 6
- 239000011230 binding agent Substances 0.000 description 5
- 238000000280 densification Methods 0.000 description 5
- 239000004033 plastic Substances 0.000 description 5
- 229920003023 plastic Polymers 0.000 description 5
- 239000002202 Polyethylene glycol Substances 0.000 description 3
- 229920001223 polyethylene glycol Polymers 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000005453 pelletization Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 229910017083 AlN Inorganic materials 0.000 description 1
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 231100000481 chemical toxicant Toxicity 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000000462 isostatic pressing Methods 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- -1 methylene-bisacrylamide lead Chemical compound 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010345 tape casting Methods 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 229910052845 zircon Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B1/00—Producing shaped prefabricated articles from the material
- B28B1/24—Producing shaped prefabricated articles from the material by injection moulding
-
- 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
- C04B35/10—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 aluminium oxide
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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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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- 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
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- 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
- C04B35/62605—Treating the starting powders individually or as mixtures
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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
- C04B35/622—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
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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
- C04B35/622—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
- C04B35/63448—Polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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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
- C04B35/622—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
- C04B35/63448—Polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C04B35/63468—Polyamides
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/602—Making the green bodies or pre-forms by moulding
- C04B2235/6022—Injection moulding
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
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- Manufacturing & Machinery (AREA)
- Structural Engineering (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Mechanical Engineering (AREA)
- Composite Materials (AREA)
- Producing Shaped Articles From Materials (AREA)
Abstract
A kind of Aqueous injection moulding process of structural ceramics, overcome prior art high organic content, it needs to carry out extraction removing with water, production cycle is long, product qualification rate is low, and lead to the problem of polluting environment, it is characterized in a certain proportion of pure water, ceramic powder, dispersing agent, thixotropic agent and forming agent, which are added in vacuum kneading machine, to be kneaded, obtain ingredient uniformly and the not ceramic aqueous creme of bubbles, ceramic aqueous creme is injected in mold by injection (mo(u)lding) machine, elevated cure molding, obtain ceramic blank injection member, then ceramic blank injection member is demoulded, it is dry, sintering, beneficial effect be using in forming agent monomer and crosslinking agent occur under the action of catalyst and initiator gel chemistries cross-linking reaction be cured as ceramic body provide intensity, it is conducive to be injected into using the plasticity that thixotropic agent improves ceramic aqueous creme simultaneously Type, organic matter is few, does not need skimming processes, shortens the production cycle, and the environmentally protective preparation of structural ceramics may be implemented.
Description
Technical field
The invention belongs to structural ceramics preparation technical field, in particular to the Aqueous injection of a kind of structural ceramics forms work
Skill.
Background technique
Traditional structural ceramics moulding process is divided into dry-press process, Plastic Forming and wet forming, this be from raw material and at
What the state that type process is showed was divided.Wherein:
The advantages of dry-press process raw material is pelletizing, including dry-pressing formed and isostatic pressing, dry-press process is: (1) technique letter
It is single, easy to operate, the period is short, high-efficient；(2) blank density is big, accurate size, shrinks small, high mechanical strength, good electrical property；
But dry-press process has that difficult to the production of large-scale and complicated shape green body, die wear is big, processing is complicated and at high cost lacks
Point.
In plastic forming process, ceramic batch keeps Plastic Flow, including tape casting, extrusion molding and injection moulding.
The advantages of Plastic Forming, can be achieved on batch-automated molding, and injection moulding can produce complicated shape product, still, existing
In technology, the disadvantage is that high organic content, degreasing time is long for Plastic Forming, is easy to produce defect, qualification rate is caused to reduce, degreasing
The problem of pollution environment is also resulted in while process organic emission.
Wet forming includes injection forming and gel casting forming, can prepare the ceramic product of complicated shape, and sintering produces
Product consistency is high, but since the degree of automation is not high, it is difficult to realize mass production.
Application publication number is that the application for a patent for invention of 103833373 A of CN discloses the " ring of a kind of nanometer of superfine ceramic
Protect production method ", this method comprises the following steps: (1) polyvinyl butyral and polyethylene glycol being kneaded at uniform mixed
Object is closed, water base forming agent is obtained；(2) water base forming agent is mixed with ceramic powders, is heated up, mixing is at uniform mud in mixer
Material；(3) by the pug of mixing is broken or extruding pelletization at single-size feeding；(4) feeding is injected and injection molding machine is added, infused
Injection molding in mould obtains ceramic member injection base；(5) into the water by ceramic member injection base, heating and thermal insulation removes poly- second two
Alcohol；(6) by water ceramic member injection base sintering extracted；(7) Aqueous Solutions of Polyethylene Glycol of extraction is cooled down, also centrifugal dehydration.
Injection-molded product described in the invention, organic binder, which still needs, carries out extraction removing with water, and the production cycle is long, and process
In be easy to produce cracking defect.
It is " a kind of for ceramic injection forming that application publication number is that the application for a patent for invention of 108947545 A of CN discloses
Water base degreasing binder ", the invention water base degreasing binder contain a large amount of water-soluble constituent elements, including polyethylene glycol, poly- first
Aldehyde, solid paraffin, polymethacrylates, stearic acid, plasticizer and antioxidant, the invention water base degreasing binder with
Ceramic powder is soaked well, is bundled together, and has good mobility, and mold filling when conducive to injection moulding can make
It uses water to remove binder as degreasing solvent, avoids carrying out degreasing using toxic chemical, greatly reduce to operation
The murder by poisoning of personnel and pollution to environment, it is economic and environment-friendly；But the invention causes to give birth to there is still a need for special extraction skimming processes
Produce the defects of period is long, and skimming processes are difficult to avoid that cracking caused by reducing because of green strength.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the deficiencies in the prior art place and defects, in conjunction with aqueous gelcasting
The characteristics of mould moulding process and injection moulding, provides ceramic slurry solid content height, and organic matter is low with respect to ceramic powder content, and not
Skimming processes are needed, sintering can directly be dried and a kind of Aqueous injection moulding process of environmentally protective structural ceramics, especially
It is the Aqueous injection moulding process of fine and close 95 aluminium oxide ceramics and the Aqueous injection moulding process of densification 3Y zirconia ceramics.
The technical solution that a kind of Aqueous injection moulding process of structural ceramics of the present invention is taken includes the following steps:
Step 1, ceramic aqueous creme is equipped with:
Ceramic paste material outfit is carried out according to following weight percent:
Pure water 10 ~ 15%,
Ceramic powder 85 ~ 90%,
Following raw material is additional based on ceramic powder weight percent:
Dispersing agent 0.1 ~ 0.5%,
Thixotropic agent 0.05 ~ 0.5%,
Forming agent 1 ~ 2%,
The ceramic powder be 95 aluminium oxide or 3Y zirconium oxide,
The dispersing agent is ammonium polymethacrylate；
The thixotropic agent is aqueous polyamide wax；
The forming agent contains monomeric acrylamide, crosslinking agent methylene-bisacrylamide, initiator ammonium persulfate, catalyst four
Methyl ethylenediamine and polymerization inhibitor tert-butyl catechol；
Step 2, vacuum temp control mud refining:
Above-mentioned material investment vacuum pugmill is kneaded, melting temperature sets 5~20 DEG C, and mixing time is 1~3 hour,
Vacuum degree is set as -0.01MPa (vacuum meter registration), obtains ingredient uniformly and the not ceramic aqueous creme of bubbles；
Step 3, it is injection moulded
The ceramic aqueous creme is injected into mold elevated cure by injection (mo(u)lding) machine to form, injection pressure is 3~
12MPa, mold temperature control between 60 DEG C ~ 90 DEG C, pressure maintaining 5~10 minutes, make ceramic aqueous creme that gel solidification occur anti-
It answers, obtains ceramic blank injection member；
Step 4, it demoulds:
Pressure release demoulding can be carried out after the reaction was completed to gel solidification；
Step 5, dry:
Obtained ceramic blank injection member is dried and dehydrated in an oven, 120 DEG C drying 2 hours；
Step 6, it is sintered:
Dried ceramic blank injection member is sintered in sintering furnace, sintering temperature is 1520 DEG C~1650 DEG C.
The technical solution that the Aqueous injection moulding process of fine and close 95 aluminium oxide ceramics of the present invention is taken includes following step
It is rapid:
Step 1, the water base creme of 95 aluminium oxide ceramics is equipped with:
The water base creme of 95 aluminium oxide ceramics is carried out according to following weight percent to be equipped with:
Pure water 10%,
95 aluminium oxide formula powders 90%,
Following raw material is additional based on 95 alumina powder weight percent:
Ammonium polymethacrylate 0.2%,
Aqueous polyamide wax 0.1%,
Acrylamide: 1.5%,
Methylene-bisacrylamide: 0.15%,
10% ammonium persulfate aqueous solution: 0.001%,
Tetramethylethylenediamine: 0.001%,
Tert-butyl catechol 0.001%,
Step 2, vacuum temp control mud refining:
Above-mentioned material investment vacuum pugmill is kneaded, melting temperature is set as 5 DEG C, and mixing time is 1 hour, vacuum degree
It is set as -0.01MPa, obtains ingredient uniformly and the not water base creme of 95 aluminium oxide ceramics of bubbles；
Step 3, it is injection moulded:
The water base creme of aluminium oxide ceramics is injected into mold, injection pressure 12MPa, mold temperature is 60 DEG C, and pressure maintaining 5 divides
Clock makes ceramic aqueous creme that gel solidification reaction occur；Obtain 95 aluminium oxide ceramics base injection members；
Step 4, it demoulds:
Pressure release demoulding can be carried out after the reaction was completed to gel solidification；
Step 5, dry:
By obtained ceramic blank injection member 120 DEG C drying 2 hours in an oven；
Step 6, it is sintered:
Then fine and close 95 aluminium oxide ceramics, density 3.85g/cm are obtained in 1650 DEG C of sintering3。
The Aqueous injection moulding process of densification 3Y zirconia ceramics of the present invention includes the following steps:
Step 1, the water base creme preparation of 3Y zirconia ceramics:
The water base creme of 3Y zirconia ceramics is carried out according to following weight percent to be equipped with:
Pure water 10%,
3Y zirconia powder 90%,
Following raw material is additional based on 3Y zirconia powder quality:
Ammonium polymethacrylate 0.4%,
Aqueous polyamide wax 0.2%,
Acrylamide: 2.0%,
Methylene-bisacrylamide: 0.2%,
10% ammonium persulfate aqueous solution: 0.001%,
Tetramethylethylenediamine: 0.001%,
Tert-butyl catechol 0.001%,
Step 2, vacuum temp control mud refining:
Above-mentioned material investment vacuum pugmill is kneaded, melting temperature is set as 20 DEG C, and mixing time is 3 hours, vacuum
Degree is set as -0.01MPa, obtains ingredient uniformly and the not water base creme of 3Y zirconia ceramics of bubbles；
Step 3, it is injection moulded:
Then the water base creme of 3Y zirconia ceramics is injected into mold, injection pressure 3MPa, mold temperature is 90 DEG C, pressure maintaining
10 minutes, makes ceramic aqueous creme that gel solidification reaction occur, obtain 3Y zirconia ceramics base injection member；
Step 4, it demoulds:
Pressure release demoulding can be carried out after the reaction was completed to gel solidification；
Step 5, dry:
By obtained ceramic blank injection member 120 DEG C drying 2 hours in an oven；
Step 6, it is sintered:
Then compact zirconia ceramics, density 6.05g/cm are obtained in 1520 DEG C of sintering3。
Compared with prior art, the beneficial effects of the present invention are:
(1) present invention combines the characteristics of water-base gel casting technique and injection moulding, develops advantage, overcomes the deficiency, and is formed
A kind of completely new ceramic aqueous injection molding technique, core of the invention principle are to utilize the monomer and crosslinking agent in forming agent
Gel chemistries cross-linking reaction occurs under the action of catalyst and initiator, ceramic body offer intensity is provided, while utilizing touching
Become agent and improve the plasticity of ceramic aqueous creme and be conducive to injection moulding, the characteristics of ceramic aqueous creme be with high solids content,
Mass percent is more than 90%, and organic matter is lower than 3% with respect to ceramic powder content, and the solid content of slurry is high, then ceramic density is high,
It is unlikely to deform in later period drying and sintering process, organic matter is few, does not need skimming processes, and sintering can directly be dried, and reduces
Various defects caused by skimming processes, shorten the production cycle, the environmentally protective preparation of structural ceramics may be implemented；
(2) the polymerization inhibitor tert-butyl catechol that uses of the present invention is a kind of polymerization inhibitor of Thermo-sensitive, can be with when being lower than 60 DEG C
Effectively prevent monomeric acrylamide and crosslinking agent methylene-bisacrylamide that Raolical polymerizable, ceramic aqueous creme occurs
There is no gel chemistries to react cured risk；And when being higher than 60 DEG C, polymerization inhibitor tert-butyl catechol fails, monomer third
Acrylamide and crosslinking agent methylene-bisacrylamide lead under the action of initiator ammonium persulfate and catalyst tetramethylethylenediamine
It crosses Raolical polymerizable and forms three-dimensional netted gel solidification；Simultaneously because reaction temperature is set as 60~90 DEG C, Ke Yiyou
Effect prevents water from becoming gas hole defect caused by vapor volatilization at 100 DEG C；
(3) fine and close 95 aluminium oxide ceramics prepared by the present invention, density is up to 3.85g/cm3, densification 3Y oxidation prepared by the present invention
Zircon ceramic, density is up to 6.05g/cm3, fine and close 95 aluminium oxide ceramics prepared by the present invention and densification 3Y zirconia ceramics can be extensive
Applied to industrial circles such as space flight, chemical industry, the energy and environmental protection.
(4) heretofore described ceramic powder is the ceramic powder not hydrolyzed, including but not limited to aluminium oxide and oxygen
Change zirconium, silicon carbide or silicon nitride and be easy to water and the ceramic powder of hydrolysis occurs after the cladding hydrophobic processing of surface
It can be used, including but not limited to aluminium nitride, magnesia, calcium oxide or yttrium oxide.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
It elaborates below by specific embodiment to the present invention.
Specific embodiment 1
A kind of Aqueous injection moulding process of structural ceramics of the present invention includes the following steps:
Step 1: ceramic aqueous creme is equipped with
Ceramic aqueous creme outfit is carried out according to following weight percent:
Pure water 10 ~ 15%,
Ceramic powder 85 ~ 90%,
Following raw material is additional based on ceramic powder weight percent:
Dispersing agent 0.1 ~ 0.5%,
Thixotropic agent 0.05 ~ 0.5%,
Forming agent 1 ~ 2%,
The ceramic powder be 95 aluminium oxide or 3Y zirconium oxide,
The dispersing agent is ammonium polymethacrylate, which can improve the dispersibility of ceramic powder and improve ceramic paste material
Solid content；
The thixotropic agent is aqueous polyamide wax, and the effect of the thixotropic agent is to be effectively improved the plasticity of aqueous-based ceramic creme, in height
It is conducive to injection under the conditions of solid content；
The forming agent contains monomeric acrylamide, crosslinking agent methylene-bisacrylamide, initiator ammonium persulfate, catalyst four
Methyl ethylenediamine and polymerization inhibitor tert-butyl catechol；
Step 2, vacuum temp control mud refining
Above-mentioned material investment vacuum pugmill is kneaded, melting temperature sets 5~20 DEG C, and mixing time is 1~3 hour,
Vacuum degree is set as -0.01MPa (vacuum meter registration), obtains ingredient uniformly and the not ceramic aqueous creme of bubbles；
Step 3, it is injection moulded
Then the ceramic aqueous creme is injected into elevated cure in mold by injection (mo(u)lding) machine to form, injection pressure 3
~12MPa, mold temperature control between 60 DEG C ~ 90 DEG C, pressure maintaining 5~10 minutes, make ceramic aqueous creme that gel solidification occur
Reaction, obtains ceramic blank injection member；
In this step, since polymerization inhibitor tert-butyl catechol is being higher than 60 DEG C i.e. failure, forming agent in ceramic aqueous creme
In monomeric acrylamide, crosslinking agent methylene-bisacrylamide, initiator ammonium persulfate and catalyst tetramethylethylenediamine it is logical
It crosses Raolical polymerizable and forms three-dimensional netted gel solidification, simultaneously because the reaction is exothermic reaction, to prevent water at 100 DEG C
Become vapor volatilization and generate gas hole defect, so reaction temperature should be lower than 90 DEG C；
Step 4, it demoulds:
Pressure release demoulding can be carried out after the reaction was completed to gel solidification；
Step 5, dry:
Obtained ceramic blank injection member is dried and dehydrated in an oven, 120 DEG C drying 2 hours；
Step 6, it is sintered:
Then dried ceramic blank injection member is sintered in sintering furnace, sintering temperature is 1520 DEG C~1650 DEG C.
Specific embodiment 2
The Aqueous injection moulding process of fine and close 95 aluminium oxide ceramics of the present invention includes the following steps:
Step 1,95 aluminium oxide ceramics cremes are equipped with:
95 aluminium oxide ceramics cremes are carried out according to following weight percent to be equipped with:
Pure water 10%,
95 aluminium oxide formula powders 90%,
Following raw material is additional based on 95 alumina powder weight percent:
Ammonium polymethacrylate 0.2%,
Aqueous polyamide wax 0.1%,
Acrylamide: 1.5%,
Methylene-bisacrylamide: 0.15%,
10% ammonium persulfate aqueous solution: 0.001%,
Tetramethylethylenediamine: 0.001%,
Tert-butyl catechol 0.001%,
Step 2, vacuum temp control mud refining:
Above-mentioned material investment vacuum pugmill is kneaded, melting temperature is set as 5 DEG C, and mixing time is 1 hour, vacuum degree
It is set as -0.01MPa, obtains ingredient uniformly and the not water base creme of 95 aluminium oxide ceramics of bubbles；
Step 3, it is injection moulded:
Then the water base creme of aluminium oxide ceramics is injected into mold, injection pressure 12MPa, mold temperature is 60 DEG C, pressure maintaining 5
Minute, make ceramic aqueous creme that gel solidification reaction occur；Obtain 95 aluminium oxide ceramics base injection members；
Step 4, it demoulds:
Pressure release demoulding can be carried out after the reaction was completed to gel solidification.；
Step 5, dry
By obtained ceramic blank injection member 120 DEG C drying 2 hours in an oven；
Step 6, it is sintered:
Then compact aluminum oxide ceramic, density 3.85g/cm are obtained in 1650 DEG C of sintering3。
Specific embodiment 3
The Aqueous injection moulding process of densification 3Y zirconia ceramics of the present invention includes the following steps:
Step 1, the water base creme preparation of 3Y zirconia ceramics:
The water base creme of 3Y zirconia ceramics is carried out according to following weight percent to be equipped with:
Pure water 10%,
3Y zirconia powder 90%,
Following raw material is additional based on 3Y zirconia powder quality:
Ammonium polymethacrylate 0.4%,
Aqueous polyamide wax 0.2%,
Acrylamide: 2.0%,
Methylene-bisacrylamide: 0.2%,
10% ammonium persulfate aqueous solution: 0.001%,
Tetramethylethylenediamine: 0.001%,
Tert-butyl catechol 0.001%,
Step 2, vacuum temp control mud refining:
Above-mentioned material investment vacuum pugmill is kneaded, melting temperature is set as 20 DEG C, and mixing time is 3 hours, vacuum
Degree is set as -0.01MPa, obtains ingredient uniformly and the not water base creme of 3Y zirconia ceramics of bubbles；
Step 3, it is injection moulded:
Then the water base creme of 3Y zirconia ceramics is injected into mold, injection pressure 3MPa, mold temperature is 90 DEG C, pressure maintaining
10 minutes, makes ceramic aqueous creme that gel solidification reaction occur, obtain 3Y zirconia ceramics base injection member；
Step 4, it demoulds:
Pressure release demoulding can be carried out after the reaction was completed to gel solidification.；
Step 5, dry:
By obtained ceramic blank injection member 120 DEG C drying 2 hours in an oven；
Step 6, it is sintered:
Then compact zirconia ceramics, density 6.05g/cm are obtained in 1520 DEG C of sintering3。
Claims (3)
1. a kind of Aqueous injection moulding process of structural ceramics, which comprises the steps of:
Step 1, ceramic aqueous creme is equipped with:
Ceramic aqueous creme outfit is carried out according to following weight percent:
Pure water 10 ~ 15%,
Ceramic powder 85 ~ 90%,
Following raw material is additional based on ceramic powder weight percent:
Dispersing agent 0.1 ~ 0.5%,
Thixotropic agent 0.05 ~ 0.5%,
Forming agent 1 ~ 2%,
The ceramic powder be 95 aluminium oxide or 3Y zirconium oxide,
The dispersing agent is ammonium polymethacrylate；
The thixotropic agent is aqueous polyamide wax；
The forming agent contains monomeric acrylamide, crosslinking agent methylene-bisacrylamide, initiator ammonium persulfate, catalyst four
Methyl ethylenediamine and polymerization inhibitor tert-butyl catechol；
Step 2, vacuum temp control mud refining:
Above-mentioned material investment vacuum pugmill is kneaded, melting temperature sets 5~20 DEG C, and mixing time is 1~3 hour,
Vacuum degree is set as -0.01MPa (vacuum meter registration), obtains ingredient uniformly and the not ceramic aqueous creme of bubbles；
Step 3, it is injection moulded
The ceramic aqueous creme is injected into mold elevated cure by injection (mo(u)lding) machine to form, injection pressure is 3~
12MPa, mold temperature control between 60 DEG C ~ 90 DEG C, pressure maintaining 5~10 minutes, make ceramic aqueous creme that gel solidification occur anti-
It answers, obtains ceramic blank injection member；
Step 4, it demoulds:
Pressure release demoulding can be carried out after the reaction was completed to gel solidification；
Step 5, dry:
Obtained ceramic blank injection member is dried and dehydrated in an oven, 120 DEG C drying 2 hours；
Step 6, it is sintered:
Dried ceramic blank injection member is sintered in sintering furnace, sintering temperature is 1520 DEG C~1650 DEG C.
2. a kind of Aqueous injection moulding process of structural ceramics according to claim 1, which is characterized in that including walking as follows
It is rapid:
Step 1, the water base creme of 95 aluminium oxide ceramics is equipped with:
The water base creme of 95 aluminium oxide ceramics is carried out according to following weight percent to be equipped with:
Pure water 10%,
95 aluminium oxide formula powders 90%,
Following raw material is additional based on 95 alumina powder weight percent:
Ammonium polymethacrylate 0.2%,
Aqueous polyamide wax 0.1%,
Acrylamide: 1.5%,
Methylene-bisacrylamide: 0.15%,
10% ammonium persulfate aqueous solution: 0.001%,
Tetramethylethylenediamine: 0.001%,
Tert-butyl catechol 0.001%,
Step 2, vacuum temp control mud refining:
Above-mentioned material investment vacuum pugmill is kneaded, melting temperature is set as 5 DEG C, and mixing time is 1 hour, vacuum degree
It is set as -0.01MPa, obtains ingredient uniformly and the not water base creme of 95 aluminium oxide ceramics of bubbles；
Step 3, it is injection moulded:
The water base creme of aluminium oxide ceramics is injected into mold, injection pressure 12MPa, mold temperature is 60 DEG C, and pressure maintaining 5 divides
Clock makes ceramic aqueous creme that gel solidification reaction occur；Obtain 95 aluminium oxide ceramics base injection members；
Step 4, it demoulds:
Pressure release demoulding can be carried out after the reaction was completed to gel solidification；
Step 5, dry:
By obtained ceramic blank injection member 120 DEG C drying 2 hours in an oven；
Step 6, it is sintered:
Then compact aluminum oxide ceramic, density 3.85g/cm are obtained in 1650 DEG C of sintering3。
3. a kind of Aqueous injection moulding process of structural ceramics according to claim 1, which is characterized in that including walking as follows
It is rapid:
Step 1, the water base creme preparation of 3Y zirconia ceramics:
The water base creme of 3Y zirconia ceramics is carried out according to following weight percent to be equipped with:
Pure water 10%,
3Y zirconia powder 90%,
Following raw material is additional based on 3Y zirconia powder quality:
Ammonium polymethacrylate 0.4%,
Aqueous polyamide wax 0.2%,
Acrylamide: 2.0%,
Methylene-bisacrylamide: 0.2%,
10% ammonium persulfate aqueous solution: 0.001%,
Tetramethylethylenediamine: 0.001%,
Tert-butyl catechol 0.001%,
Step 2, vacuum temp control mud refining:
Above-mentioned material investment vacuum pugmill is kneaded, melting temperature is set as 20 DEG C, and mixing time is 3 hours, vacuum
Degree is set as -0.01MPa, obtains ingredient uniformly and the not water base creme of 3Y zirconia ceramics of bubbles；
Step 3, it is injection moulded:
Then the water base creme of 3Y zirconia ceramics is injected into mold, injection pressure 3MPa, mold temperature is 90 DEG C, pressure maintaining
10 minutes, makes ceramic aqueous creme that gel solidification reaction occur, obtain 3Y zirconia ceramics base injection member；
Step 4, it demoulds:
Pressure release demoulding can be carried out after the reaction was completed to gel solidification；
Step 5, dry:
By obtained ceramic blank injection member 120 DEG C drying 2 hours in an oven；
Step 6, it is sintered:
Then compact zirconia ceramics, density 6.05g/cm are obtained in 1520 DEG C of sintering3。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114057429A (en) * | 2021-11-30 | 2022-02-18 | 上海高铝氧新材料有限公司 | Ultrathin high-temperature-resistant alumina/PVA continuous fiber sheet and preparation method thereof |
| CN114149257A (en) * | 2020-12-21 | 2022-03-08 | 辽宁英冠高技术陶瓷股份有限公司 | Preparation method of gel injection molding 5G filter ceramic |
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| CN1304907A (en) * | 2000-12-29 | 2001-07-25 | 清华大学 | Colloid injection method and equipment for shaping ceramics |
| CN1528710A (en) * | 2003-10-10 | 2004-09-15 | 清华大学 | Pressure-Induced Rapid In-Situ Solidification of Concentrated Ceramic Suspensions |
| CN103086941A (en) * | 2012-12-19 | 2013-05-08 | 吉林大学 | N-acryloyl succinimide and synthetic method thereof |
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2019
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1304907A (en) * | 2000-12-29 | 2001-07-25 | 清华大学 | Colloid injection method and equipment for shaping ceramics |
| CN1528710A (en) * | 2003-10-10 | 2004-09-15 | 清华大学 | Pressure-Induced Rapid In-Situ Solidification of Concentrated Ceramic Suspensions |
| CN103086941A (en) * | 2012-12-19 | 2013-05-08 | 吉林大学 | N-acryloyl succinimide and synthetic method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114149257A (en) * | 2020-12-21 | 2022-03-08 | 辽宁英冠高技术陶瓷股份有限公司 | Preparation method of gel injection molding 5G filter ceramic |
| CN114057429A (en) * | 2021-11-30 | 2022-02-18 | 上海高铝氧新材料有限公司 | Ultrathin high-temperature-resistant alumina/PVA continuous fiber sheet and preparation method thereof |
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Application publication date: 20191022 |