CN113149626A - Feed for quartz ceramic injection molding and preparation method thereof - Google Patents
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- CN113149626A CN113149626A CN202110521738.2A CN202110521738A CN113149626A CN 113149626 A CN113149626 A CN 113149626A CN 202110521738 A CN202110521738 A CN 202110521738A CN 113149626 A CN113149626 A CN 113149626A
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- C—CHEMISTRY; METALLURGY
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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
- C04B35/14—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 silica
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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
- B28B1/004—Devices for shaping artificial aggregates from ceramic mixtures or from mixtures containing hydraulic binder
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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
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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
- B28B1/54—Producing shaped prefabricated articles from the material specially adapted for producing articles from molten material, e.g. slag refractory ceramic materials
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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
- B28B3/00—Producing shaped articles from the material by using presses; Presses specially adapted therefor
- B28B3/20—Producing shaped articles from the material by using presses; Presses specially adapted therefor wherein the material is extruded
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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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- 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
- C04B35/634—Polymers
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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
- C04B35/638—Removal thereof
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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
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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
- C04B2235/6562—Heating rate
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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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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
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Abstract
The invention discloses a feed for quartz ceramic injection molding and a preparation method thereof, wherein the feed for quartz ceramic injection molding is prepared by connecting an organic silicon precursor to a surface-shaped core-shell structure of silica particles of fused quartz powder through a covalent bond and then mixing the silica particles under the action of a binder; wherein the fused quartz powder accounts for 70-90 wt%, the organic silicon precursor accounts for 6-15 wt%, and the binder accounts for 4-15 wt%. According to the invention, a covalent bond is formed between the organosilicon precursor containing active groups and the exposed hydroxyl on the surface of silicon dioxide, and the surface of fused quartz is modified, so that the dispersion uniformity of quartz powder is increased, the product density is enhanced, the shrinkage rate is reduced, 50% of quartz yield is introduced, the solid phase content is increased, and the pore defect caused by organic matter volatilization is reduced.
Description
Technical Field
The invention relates to the field of precise ceramic preparation, in particular to a feed for quartz ceramic injection molding and a preparation method thereof.
Background
Fused silica ceramics (quartz ceramics for short) has excellent mechanical and electrical characteristics, such as small thermal expansion coefficient, good bending strength and thermal temperature property, good dielectric property and thermal stability and shape, and the like, is easier to form compared with quartz glass, and is especially suitable for products with complex shapes and large parts, and the cost is far lower than that of quartz glass products, so that fused silica ceramics become an essential material in the novel high-tech fields of aerospace, solar cells, electronic industry, atomic energy industry, national defense and military industry and the like since the advent and wide application range.
The commonly used forming technologies of quartz ceramics at present comprise slip casting, isostatic compaction and the like, and all have the defects of large processing allowance and high cost. The existing injection molding process is difficult to realize and mass production of quartz ceramic structural parts, mainly because the content of organic matters in quartz feed is high, the organic matters are difficult to completely eliminate in the firing process, so that the injection molded ceramic structural parts have the defects of more pores, low density and sintering shrinkage of over 15 percent, and the requirements on mass production of special-shaped products with large demand, small size and complex structure are difficult to meet.
Disclosure of Invention
In order to solve the problems, the invention provides a feed for quartz ceramic injection molding and a preparation method thereof, which can obtain high solid content by introducing an organic silicon precursor, reduce the sintering shrinkage and improve the yield.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a feed for quartz ceramic injection molding is prepared by connecting an organic silicon precursor to the surface of a silicon dioxide particle of fused quartz powder by a covalent bond to form a core-shell structure, and then mixing under the action of a binder;
wherein, the organic silicon precursor contains at least one active agent group of amino, sulfydryl and hydroxyl.
Furthermore, the fused quartz powder accounts for 70-90 wt%, the organic silicon precursor accounts for 6-15 wt%, and the binder accounts for 4-15 wt%.
Further, the binder comprises a framework material, a surfactant; the framework material accounts for 60-94 wt%, and the surfactant accounts for 6-40 wt%.
Further, the organosilicon precursor is amino polysiloxane (amino silicone oil, CAS: 63148-62-0), alpha-hydrogen-omega-hydroxy-polydimethylsiloxane (hydroxy silicone oil, CAS: 70131-67-8), (mercapto) methylsiloxane-dimethylsiloxane copolymer (CAS: 102783-03-9); organosilicon containing active agent groups such as amino, sulfydryl, hydroxyl and the like.
Further, the framework material is at least one of High Density Polyethylene (HDPE), polyvinylpyrrolidone (PVP), atactic polypropylene (APP), polypropylene (PP), polyvinyl chloride (PVC), Polystyrene (PS) and acrylonitrile-butadiene-styrene (ABS).
Further, the surfactant is at least one of Stearic Acid (SA), Oleic Acid (OA), and carboxystearic acid (HSA).
The invention also provides a preparation method of the feed for quartz ceramic injection molding, which comprises the steps of firstly condensing fused quartz powder and an organic silicon precursor, then heating and melting a framework material and a surfactant to obtain a binder, then adding a condensation product into the binder for mixing, sending the mixture into an extruder, and carrying out extrusion granulation to obtain the feed for quartz ceramic injection molding.
Further, the framework material is at least one of High Density Polyethylene (HDPE), polyvinylpyrrolidone (PVP), atactic polypropylene (APP), polypropylene (PP), polyvinyl chloride (PVC), Polystyrene (PS) and acrylonitrile-butadiene-styrene (ABS).
Further, the surfactant is at least one of Stearic Acid (SA), Oleic Acid (OA), carboxystearic acid (HSA), and a silane coupling agent.
Further, an internal mixer is used for mixing, the mixing time is 2-10 hours, and the mixing temperature is 120-200 ℃.
The invention also aims to provide a preparation method of the quartz ceramic material, which comprises the steps of carrying out injection molding, degreasing and sintering treatment on the feed for injection molding of the quartz ceramic material to obtain the quartz ceramic material.
Further, the injection pressure of the injection molding is 40-90 MPa, and the injection temperature is 150-220 ℃.
Further, the degreasing adopts high-pressure ethanol steam as a degreasing agent.
The invention has the beneficial effects that:
according to the invention, a covalent bond is formed between the organosilicon precursor containing active groups and the exposed hydroxyl on the surface of silicon dioxide, and the surface of fused quartz is modified, so that the dispersion uniformity of quartz powder is increased, the product density is enhanced, the shrinkage rate is reduced, 50% of quartz yield is introduced, and the solid phase content is increased; in addition, the organic silicon has the performances of inorganic materials and organic materials, and has the characteristics of low surface tension, small viscosity-temperature coefficient, high compressibility and the like, so that the organic silicon adhesive can partially or even completely replace components such as paraffin, a surfactant and the like in the traditional adhesive by introducing the organic silicon precursor, thereby reducing the addition amount of organic substances and reducing the pore defect caused by volatilization of organic matters.
The quartz ceramic prepared by the feed for quartz ceramic injection molding is prepared by a high-pressure injection molding process, and the ceramic blank is degreased under the condition of high-temperature and high-pressure ethanol steam, so that the potential safety hazard of environmental protection caused by degreasing by using environmental protection oil in the traditional quartz ceramic feed system is solved.
The quartz ceramic system developed by the invention reduces the shrinkage rate, improves the precision, reduces or even eliminates the machining amount in the later period on the premise of meeting the performance requirement, realizes the near-net-size preparation, and lays a good foundation for realizing the low-cost and mass production of the special-shaped quartz ceramic antenna window and the antenna housing.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method of a quartz ceramic material comprises the following steps:
(1) condensation: 80wt% of quartz powder and 20 wt% of amino polysiloxane (amino silicone oil) react in a mixer for 8 hours at 90 ℃;
(2) preparing a binder: adding 40wt% of High Density Polyethylene (HDPE), 40wt% of random polypropylene (APP) and 20 wt% of stearic acid into a mixer, melting at 180 ℃, stirring, fully mixing uniformly, and cooling for later use to obtain a binder;
(2) mixing: putting 10 wt% of binder and 90wt% of condensation product obtained in the step (1) into a mixing roll, and uniformly mixing at 180 ℃;
(3) and (3) granulation: granulating the mixed materials in a granulator to obtain quartz ceramic feed with the diameter of less than 5 mm;
(4) injection molding: cooling and crushing the prepared feed, feeding the feed into a hopper of a high-pressure injection molding machine through an automatic feeding machine, injecting the ceramic feed into a precision mold under the conditions that the injection pressure is 60MPa and the injection temperature is 160 ℃, and opening the mold to obtain a ceramic blank;
(5) degreasing: degreasing the ceramic blank at the temperature of 110 ℃ under the condition of 6 atmospheric alcohol steam;
(6) and (3) sintering: drying the degreased ceramic blank at the temperature of 100 ℃, putting the ceramic blank into a pushed slab kiln through a mechanical arm, carrying out heat preservation on the ceramic blank at the temperature of 500 ℃ for 2 hours, carrying out binder removal treatment, wherein the heating rate is 18 ℃/h, then heating to 1480 ℃ for sintering, the heating rate is 120 ℃/h, and the heat preservation time is 4h, thus obtaining the low-deformation high-precision quartz ceramic material.
Example 2
A preparation method of a quartz ceramic material comprises the following steps:
(1) condensation: reacting 85wt% of quartz powder and 15wt% of amino polysiloxane (amino silicone oil) in a mixer at 90 ℃ for 8 hours;
(2) preparing a binder: adding 45 wt% of acrylonitrile-butadiene-styrene (ABS), 40wt% of polyvinylpyrrolidone (PVP) and 15wt% of stearic acid into a mixer, melting at 200 ℃, stirring, fully mixing uniformly, and cooling for later use to obtain a binder;
(2) mixing: putting 10 wt% of binder and 90wt% of condensation product obtained in the step (1) into a mixing roll, and uniformly mixing at 180 ℃;
(3) and (3) granulation: granulating the mixed materials into ceramic feed with the diameter of 3-3.5 mm and the length of 4-6 mm by using a granulator;
(4) injection molding: cooling and crushing the prepared feed, feeding the feed into a hopper of a high-pressure injection molding machine through an automatic feeding machine, injecting the ceramic feed into a precision mold under the conditions that the injection pressure is 90MPa and the injection temperature is 190 ℃, and opening the mold to obtain a ceramic blank;
(5) degreasing: degreasing the ceramic blank at 130 ℃ under the condition of 10 atmospheric alcohol steam;
(6) and (3) sintering: drying the degreased ceramic blank at the temperature of 100 ℃, putting the ceramic blank into a pushed slab kiln through a mechanical arm, carrying out heat preservation on the ceramic blank at the temperature of 500 ℃ for 4 hours for glue removal treatment, wherein the heating rate is 10 ℃/h, then heating to 1550 ℃ for sintering, the heating rate is 100 ℃/h, and the heat preservation time is 5 hours, so that the low-deformation high-precision quartz ceramic material can be prepared.
Comparative example
A ceramic material prepared in the same manner as in example 1 was used using methyl silicone oil instead of amino silicone oil.
The dimensional shrinkage of the various examples and comparative examples is shown in table 1.
From table 1, it can be seen that the quartz ceramic prepared by adding the amino-substituted organosilicon precursor has lower shrinkage, smaller fluctuation and higher product qualification rate than the quartz ceramic prepared by adding the all-methyl-substituted organosilicon precursor, and can be used for mass production of special-shaped products with large demand and complex structure.
The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or ambit of the invention as defined in the appended claims.
Claims (10)
1. The feed for injection molding of quartz ceramics is characterized in that the feed is formed by mixing an organic silicon precursor connected to the surface of silica particles of fused quartz powder through a covalent bond under the action of a binder;
wherein, the organic silicon precursor contains at least one active agent group of amino, sulfydryl and hydroxyl.
2. A feedstock according to claim 1, wherein the fused silica powder is 70-90 wt%, the organosilicon precursor is 6-15 wt%, and the binder is 4-15 wt%.
3. The feedstock of claim 1, wherein said binder comprises a skeletal material, a surfactant; the framework material accounts for 60-94 wt%, and the surfactant accounts for 6-40 wt%.
4. The feedstock according to claim 1, wherein the organosilicon precursor contains amino groups.
5. A feedstock according to claim 3, wherein said framework material is at least one of High Density Polyethylene (HDPE), polyvinylpyrrolidone (PVP), atactic polypropylene (APP), polypropylene (PP), polyvinyl chloride (PVC), Polystyrene (PS), Acrylonitrile Butadiene Styrene (ABS).
6. The feedstock according to claim 1, wherein the surfactant is at least one of Stearic Acid (SA), Oleic Acid (OA), and carboxystearic acid (HSA).
7. A method for preparing a feedstock for injection molding of quartz ceramic according to any one of claims 1 to 6,
firstly, condensing fused quartz powder and an organic silicon precursor, then heating and fusing a framework material and a surfactant to obtain a binder, then adding a condensation product into the binder for mixing, sending the mixture into an extruder, and performing extrusion granulation to obtain the feed for injection molding of quartz ceramics.
8. The preparation method of the quartz ceramic material is characterized in that the quartz ceramic material is obtained by carrying out injection molding, degreasing and sintering treatment on the feed for injection molding of the quartz ceramic.
9. The method for preparing a quartz ceramic material according to claim 8, wherein the injection pressure of the injection molding is 40-90 MPa, and the injection temperature is 150-220 ℃.
10. The method for preparing a quartz ceramic material according to claim 8, wherein the degreasing uses high-pressure ethanol vapor as a degreasing agent.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114436632A (en) * | 2022-01-19 | 2022-05-06 | 山东工业陶瓷研究设计院有限公司 | High-temperature thermal shock resistant ceramic material and preparation method thereof |
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- 2021-05-13 CN CN202110521738.2A patent/CN113149626B/en active Active
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