CN108863392A - A kind of increasing material manufacturing method of silicon carbide ceramics - Google Patents

A kind of increasing material manufacturing method of silicon carbide ceramics Download PDF

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Publication number
CN108863392A
CN108863392A CN201810747328.8A CN201810747328A CN108863392A CN 108863392 A CN108863392 A CN 108863392A CN 201810747328 A CN201810747328 A CN 201810747328A CN 108863392 A CN108863392 A CN 108863392A
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ceramic
layer
temperature
trays
thermosetting resin
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林彬
王皓吉
魏金花
李晓雷
赵菲菲
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Tianjin University
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Tianjin University
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/565Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
    • C04B35/573Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained by reaction sintering or recrystallisation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B28WORKING CEMENT, CLAY, OR STONE
    • B28BSHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B1/00Producing shaped prefabricated articles from the material
    • B28B1/001Rapid manufacturing of 3D objects by additive depositing, agglomerating or laminating of material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B28WORKING CEMENT, CLAY, OR STONE
    • B28BSHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B17/00Details of, or accessories for, apparatus for shaping the material; Auxiliary measures taken in connection with such shaping
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y10/00Processes of additive manufacturing
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63Preparing 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
    • C04B35/632Organic additives
    • C04B35/634Polymers
    • C04B35/63448Polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B35/63452Polyepoxides
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/602Making the green bodies or pre-forms by moulding
    • C04B2235/6026Computer aided shaping, e.g. rapid prototyping

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Ceramic Products (AREA)

Abstract

The present invention relates to a kind of increasing material manufacturing method of silicon carbide ceramics, including:The ceramic part model printed will be needed to be layered, determine every layer of region for needing to bond;One layer of ceramic powders of laying on trays;Thermosetting resin bonding agent is sprayed on the region that this layer needs to bond using nozzle, the thermosetting resin bonding agent includes epoxy monomer and curing agent;Using the thermosetting resin bonding agent on this layer of ceramic powders of heating devices heat, heat cure cross-linking polymerization is brought it about, this layer of ceramic powders are bonded;Successively printing, until forming complete ceramic body;Ceramic body is cleaned up;Ceramic body after cleaning up is put into sintering furnace and is calcined, method is as follows:140 DEG C are heated to, keeps the temperature 3 hours;700 DEG C are heated under air environment again, keeps the temperature 5 hours;It is finally heated to 2020 DEG C in an inert atmosphere, keeps the temperature 10 hours, sinters solid ceramic finished part into.

Description

A kind of increasing material manufacturing method of silicon carbide ceramics
Technical field
The present invention relates to a kind of forming methods of ceramic material, more particularly to one kind is based on additional manufacturing technology, i.e., three-dimensional The ceramic material increasing material manufacturing method of article manufacturing technology.
Background technique
Ceramic material has many advantages, such as low-density, high rigidity, high heat resistance, high abrasion, has in extensive industrial circle Fabulous application prospect, such as heat-insulated, heat proof material, ceramic bearing etc..Traditional ceramic forming material method is by ceramic log Material, usually powder or slurry be put into mold carry out high temperature sintering formed blank, reuse machine cut, grinding method into Row finishing, to obtain final product.But due to ceramic material high-melting-point, hard crisp unmanageable characteristic, tradition molding Method is needed using expensive mold and machine tool, grinding tool, and production technology is complicated, and the process-cycle is long.
The part model to be manufactured is used computer program using the thought of successively additional manufacture by increases material manufacturing technology Layered shaping, the X-Y scheme for being needed to print from level to level are carried out, then passes through 3D printer and successively prints, stacks these two dimensions Figure ultimately forms 3 d part entity.This material manufacturing technology can be to avoid using mold and subsequent machining Process, to realize the quick manufacture of part.
There are several disclosed ceramic material increasing material manufacturing methods at present, has had the main of certain correlation with the application Have:
United States Patent (USP) 5,204,055 is spread on the table from level to level using previously prepared ceramic powders, and is successively used Bonding agent is ejected into selection area by injector head, makes the powder bonding in the region, so successively accumulation, ultimately form part at Product.This technology does not include the solid-phase sintering of ceramics, only the fixation between bonding agent realization material powder, therefore final part Intensity is very low.
8,568,649 B1 of United States Patent (USP) US uses polyvinyl alcohol as bonding agent on the basis of the former, and in ceramics After powder bonding molding, then carried out high temperature sintering.On the one hand the bonding agent ingredient in high temperature removal material is utilized;Another party Face makes ceramic powders that high temperature solid state reaction occur, and forms the entity of consolidation, to improve part strength compared to the former.But by It is very big (the preferred molecular weight of the patent is 9,000 to 10,000) in polyvinyl alcohol molecule amount, it is difficult to penetrate into small ceramic powder Among last gap.Therefore ceramic powders partial size must be sufficiently large, so that bonding agent is penetrated into the gap for providing sufficient.In this way, Contain many holes inside final finished material, be equivalent to the initial crack of material internal and concentrate stress point, reduces material Expect the reliability of intensity and part.
Chinese patent CN 105601287 A, CN 03935036 A etc. disclose and some carried out using light-curing adhesives Ceramic powders bonding, to realize the technical method of three-dimensional manufacture.These methods use sodium metasilicate, magnesium fluosilicate etc. as solidification Agent, hexafluorophosphate, 6- isopropylbenzene cyclopentadienyl iron etc. are used as initiator.This kind of bonding agent can be by UV radiation curing, formation The chemical bonds such as silicon oxygen, fluosilicic, to realize the bonding of ceramic powders.The disadvantage is that introducing the impurity different from ceramic particle ingredient Element, such as sodium, fluorine, phosphorus, iron to hinder the solid-phase crystallization reaction of ceramic particle, and then weaken Material Strength, Huo Zhezao At the decline of other aspect service performances.
Summary of the invention
The present invention proposes a kind of to realize increasing material manufacturing method high-densit, that high-strength carborundum is ceramic.The present invention is using such as Lower technical solution:
A kind of increasing material manufacturing method of silicon carbide ceramics, includes the steps that following:
1) the ceramic part model printed will be needed to be layered, determines every layer of region for needing to bond, and generate control Program.
2) one layer of silicon carbide ceramics powder of laying on trays;
3) thermosetting resin bonding agent is sprayed on the region that this layer needs to bond using nozzle, the thermosetting resin is viscous Connecing agent includes epoxy monomer and curing agent;
4) using the thermosetting resin bonding agent on this layer of ceramic powders of heating devices heat, heat cure crosslinking is brought it about Polymerization reaction bonds this layer of ceramic powders;
5) successively printing, until forming complete ceramic body;
6) ceramic body is cleaned up, removes the unglued ceramic powders adhered to thereon;
7) ceramic body after cleaning is placed in sintering furnace, is heated to 140 DEG C, keep the temperature 3 hours;Again under air environment 700 DEG C are heated to, keeps the temperature 5 hours;It is finally heated to 2020 DEG C in an inert atmosphere, keeps the temperature 10 hours, sinters solid into Ceramic part finished product.
Preferably, using three epoxy-phenyl para-aminophenol TGAP, four epoxy-phenyl diaminodiphenylmethane TGDDM it is mixed Object is closed as epoxy monomer;Use diethyl toluene diamine DETDA as curing agent, TGAP, TGDDM and DETDA's rubs Your ratio is 2:1:5.
Used manufacturing equipment includes:Rack, the feed tray for carrying ceramic powders as raw material, work support Disk, stone scraper plate, curing agent delivery pipe, epoxy monomer delivery pipe, mixing chamber, nozzle and heating device, feed tray and Trays can move up and down, and the raw ceramic materials powder that stone scraper plate is used to will be above rack rushes at trays, make it On trays formed one layer of uniform material layer to be printed, curing agent delivery pipe and epoxy monomer delivery pipe with mix Room connection, nozzle are used to the thermosetting resin bonding agent obtained after mixing chamber mixes being injected in work support according to control program The region that every layer of specified needs bond on disk;Heating device is used for the material layer to be printed of heating work pallet and its carrying, Its temperature is set to be higher than the solidification temperature of thermosetting resin.
Preferably, water cooling plant is disposed with around nozzle and mixing chamber.
Compared with prior art, beneficial effects of the present invention are:
(1) epoxy monomer and hardener molecules amount very little used, therefore with non-in the gap of ceramic powders Normal good wellability, can effectively bond the very small ceramic powders of partial size, to improve the compactness of material, reduce material Porosity inside material realizes high-densit, high-strength ceramic increasing material manufacturing;
(2) chemical element contained by epoxy monomer of the present invention and curing agent is mainly carbon, hydrogen, oxygen, nitrogen, in height Under warm oxygen-enriched environment, it is easy to be oxidized to carbon dioxide, water and nitrogen oxides, therefore will not be residual in high-temperature calcination sintering process It stays in inside ceramic product, to realize the increasing material manufacturing of high purity ceramic;
(3) nozzle of the present invention can achieve high-precision bonding agent spraying, while not need mold and machining Ceramic material disposal molding may be implemented in cutter, thus realize ceramic material efficiently, high-precision modeling;
(4) technical solution of the present invention only mixes epoxy monomer, curing agent, and under high temperature environment Heating, resin adhesive just have solidification viscosity, and therefore, nozzle of the invention and bonding agent transfer pipeline will not block, thus No longer need nozzle and transfer pipeline clean and maintenance;
(5) solid particle is also not present in epoxy monomer and curing agent viscosity very little, even if jet velocity is quickly, Very big impact force will not be caused to nozzle, therefore the service life and reliability of nozzle can be improved, and improve the printing of material Efficiency;
Detailed description of the invention
Fig. 1 is the flow diagram of the method for the present invention.
Fig. 2 is the schematic illustration of apparatus of the present invention.
Specific embodiment
The present invention as shown in Figure 1 adopts the following technical scheme that:
1, using computer software, the ceramic part model printed will be needed to be layered, and will determine what every layer of needs bonded Region, and generate printer control program;
2, one layer of very thin ceramic powders of laying on trays;
3, epoxy monomer and hardener mixture are sprayed on the region that this layer needs to bond according to program using nozzle;
4, using the thermosetting resin bonding agent on this layer of ceramic powders of heating devices heat, heat cure crosslinking is brought it about Polymerization reaction bonds this layer of ceramic powders;
5, successively printing, until forming complete ceramic body;
6, ceramic body is cleaned up, removes the unglued ceramic powders adhered to thereon;
7, the ceramic body after cleaning up is put into the calcining of sintering furnace high temperature, on the one hand removes what ceramic body included On the other hand resin adhesive ingredient makes the ceramic powders in ceramic body that solid phase reaction occur, forms fine and close ceramic part Finished product.
The material of above-mentioned ceramic powders can be iron oxide, zinc oxide, manganese oxide, aluminium oxide, silica, zirconium oxide, oxygen Change magnesium, yttrium oxide, silicon nitride, silicon carbide or other can be sintered by high temperature solid state reaction to be formed ceramics metal oxide, Nitride, carbide or salt and their combination, perhaps by the modified above-mentioned powder in surface or in order to improve material The mixed-powder of other powder, fiber, crystal whisker-shaped additive is added in performance.The particle diameter of above-mentioned ceramic powders can be in 10nm- 1000nm, it is therefore preferable to which 30nm-500nm is more preferably 50nm-200nm.
Above-mentioned epoxy monomer, which refers to, can realize the cured monomer molecule material of heat cross-linking by epoxy functionality Material, can select Bisphenol F glycidol ether (BFDGE), three epoxy-phenyl para-aminophenol (TGAP), four epoxy-phenyl diamino The Orqanics Monomers such as diphenyl-methane (TGDDM) or above-mentioned several combination.Above-mentioned curing agent refers to can be with epoxy monomer The epoxy functionality of molecule reacts to realize the chemical reagent of crosslinking curing, can select diethyl toluene diamine (DETDA).The mixture of above-mentioned epoxy monomer and curing agent can produce cross-linking reaction, shape under high-temperature heating effect At the resin solid of macromolecular, to realize the bonding to ceramic powders.
Since each amidine functional group in curing agent can be sent out with 2 epoxy-phenyl functional groups in epoxy monomer The ratio of raw cross-linking reaction, above-mentioned epoxy monomer and curing agent needs to calculate accordingly, so that the amido on each curing agent Functional group can correspond to 1.5-3, it is therefore preferable to the epoxy-phenyl functional group on 1.8-2.5 thermosetting resin, to guarantee The abundant progress of cross-linking reaction.
Above-mentioned heating device, the resistance heater that can be mounted on trays are also possible to a kind of moveable It is installed on the light source or radiation or hot blow air heating device of 3D printer other positions, either to realize on trays The thermosetting resin bonding agent sprayed is heating and curing.Above-mentioned heating device needs that thermosetting resin bonding agent is heated and protected It holds between 150 DEG C -240 DEG C, preferably between 180 DEG C -200 DEG C, so that thermosetting resin cross-linking reaction ingredient occurs.For Reduction energy consumption can also arrange thermal insulation material in trays regions.In order to protect the steady of other workpieces of printing device Fixed operation, can also be arranged heat-barrier material and radiator between trays region and other component.
Above-mentioned cleaning process, it is therefore an objective to the unglued ceramic powders for adhering to ceramic body surface, in order to reach this Purpose, the mode that can use the mechanical brushing such as hairbrush are removed, and also can use water flow, the mode of gas washout is removed, can also To remove in the way of ultrasonic vibration, it is also possible to the combination of above-mentioned several mode.
Ceramic body is first heated to 120 DEG C -150 DEG C by above-mentioned high-temperature burning process, and keeps the temperature 2-5 hours, to remove it In the moisture that contains;Later, optional calcination temperature is 300 DEG C -700 DEG C, preferably 500 DEG C -600 when removing bonding agent DEG C, 2-8 hours are kept the temperature, preferably 4-6 hours, environment was air (oxygen-containing) atmosphere;It is allowed to that solid phase occurs in sintering ceramic powder When reaction, calcination temperature, time and gaseous environment need to refer to the related request of be sintered ceramic composition.
In order to realize the increasing material manufacturing of above-mentioned ceramic body, following application epoxy monomer and curing agent can be used to make Printer is bonded for the ceramic powders of bonding agent.
As shown in Fig. 2, bonding printer as the ceramic powders of bonding agent using epoxy monomer and curing agent, mainly Including:Rack 1, feed tray 2, trays 3, heating device 4, stone scraper plate 5, curing agent delivery pipe 6, epoxy monomer Delivery pipe 7, mixing chamber 8, water cooling plant 9, nozzle 10 and other booster actions motor, transmission device, guide rail, heat-insulated knot The components such as structure, radiator structure, water pump, water tank.
The ceramic powders 11 as raw material are carried on feed tray 2.
When every layer of printing, feed tray 2 moves up a small distance, and the raw ceramic materials powder 11 for carrying it is higher than machine The upper surface of frame 1;It works at the same time pallet 3 and moves down same distance;Later, stone scraper plate 5, will be high by left movement to right side It is rushed at trays 3 in the raw ceramic materials powder 11 of rack, it is made to form one layer of uniform material to be printed on trays 3 The bed of material.
Curing agent and epoxy monomer are delivered to mixed by curing agent delivery pipe 6 and epoxy monomer delivery pipe 7 respectively It closes in room 8, by controlling the feed flow of two delivery pipes, can control the ratio of curing agent and epoxy monomer.Curing agent After being sufficiently mixed in mixing chamber 8 with epoxy monomer, every layer of specified needs are ejected into according to program by nozzle 10 and are glued The region of knot.
4 heating work pallet 3 of heating device and its material layer to be printed of carrying, make its temperature be higher than thermosetting resin Solidification temperature.
It, can be in nozzle 10 and mixing chamber 8 weeks in order to avoid the high temperature at trays 3 is transmitted to nozzle 10 and mixing chamber 8 Cloth sets water cooling plant 9, and high temperature is avoided to make mixing chamber 8 or curing agent and epoxy monomer premature cure in nozzle 10.
The mixture of the epoxy monomer and curing agent that are sprayed by nozzle 10, under the high temperature action of heating device 4 Solidification bonds the ceramic powders in specified region, successively prints, ultimately forms ceramic body 12.
Below with reference to examples illustrate the present invention.
Embodiment 1:The increasing material manufacturing method of aluminium oxide ceramics
1) modelling and layering:Design needs the part model printed, is layered using computer software, calculates every Layer needs the region bonded, and generates the printer control program comprising bonding agent jet path.
2) preparation of alumina ceramic powder raw material:Select the alumina ceramic powder that particle diameter is 60nm as former Material is put into the feed tray of ceramic powders bonding printer.
3) the calculating proportion of bonding agent:Use Bisphenol F glycidol ether (BFDGE) as epoxy monomer, each of which It include two epoxy functionalities on molecule;Use diethyl toluene diamine (DETDA) as curing agent, is wrapped on each of which molecule Containing two amidine functional groups.Select the epoxy group in corresponding 2.2 epoxy monomers of amidine functional group on each curing agent Functional group, thus may determine that the molar ratio of BFDGE and DETDA is 2.2:1.
4) conveying speed of curing agent delivery pipe and epoxy monomer delivery pipe is adjusted, to realize two required in 3) The molar ratio of kind bonding agent ingredient.
5) printer is used, according to the layer-by-layer laying alumina ceramic powder of program, mixes sufficient ring using nozzle injection The mixture of oxygen resin monomer and curing agent, and said mixture is heated by Resistant heating device additional on trays It keeps to 200 DEG C, makes it by heat cure, ceramic powders are bonded.Ultimately form the ceramic body of printing part.
6) ceramic body is taken out from trays, is placed in water, brush away the unglued of surface attachment using hairbrush Powder.It places into supersonic wave cleaning machine later, by ultrasonic wave excitation hydrone, realizes further cleaning.
7) ceramic body after cleaning is placed in sintering furnace, is heated to 140 DEG C, keep the temperature 3 hours, it is contained therein to remove Moisture;600 DEG C are heated under air environment again, 6 hours are kept the temperature, to remove bonding agent ingredient therein;Finally in air ring It is heated to 1200 DEG C under border, keeps the temperature 8 hours, alumina powder is made to sinter solid ceramic finished part into.
Embodiment 2:The increasing material manufacturing method of silicon carbide ceramics
1) modelling and layering:With embodiment 1;
2) preparation of silicon carbide ceramics powder raw material:By partial size be 100nm β-SiC powder and micro C, B powder according to 100:3:1 ratio is uniformly mixed, as raw material;
3) the calculating proportion of bonding agent:Use three epoxy-phenyl para-aminophenol (TGAP), four epoxy-phenyl diamino two The mixture of phenylmethane (TGDDM) includes accordingly three, four epoxy functionals on each molecule as epoxy monomer Group;Use diethyl toluene diamine (DETDA) as curing agent, includes two amidine functional groups on each of which molecule.It is selected every The epoxy functionality in corresponding 2 epoxy monomers of amidine functional group on a curing agent, thus may determine that TGAP, The molar ratio of TGDDM and DETDA is 2:1:5.
4) conveying speed of curing agent delivery pipe and epoxy monomer delivery pipe is adjusted, to realize two required in 3) The molar ratio of kind bonding agent ingredient.
5) printer is used, according to the layer-by-layer laying silicon carbide ceramics powder of program, mixes sufficient ring using nozzle injection The mixture of oxygen resin monomer and curing agent, and protected by heat radiation heating devices heat said mixture additional on printer It holds to 180 DEG C, makes it by heat cure, ceramic powders are bonded.Ultimately form the ceramic body of printing part.
6) ceramic body is taken out from trays, rinses green body using high pressure water flow, it is unglued to go to surface to adhere to Powder.It places into supersonic wave cleaning machine later, by ultrasonic wave excitation hydrone, realizes further cleaning.
7) ceramic body after cleaning is placed in sintering furnace, is heated to 140 DEG C, keep the temperature 3 hours, it is contained therein to remove Moisture;700 DEG C are heated under air environment again, 5 hours are kept the temperature, to remove bonding agent ingredient therein;Finally in indifferent gas It is heated to 2020 DEG C under body environment, keeps the temperature 10 hours, silicon carbide powder is made to sinter solid ceramic finished part into.
Embodiment 3:The increasing material manufacturing method of ferrite ceramics
1) modelling and layering, the calculating proportion of bonding agent, print procedure can be found in embodiment 1 or embodiment 2.
2) preparation of ferrite ceramics powder raw material:Use the manganese-zinc ferrite powder that the trade mark is PC40 as raw material.
3) according to preceding method, ceramic body is printed after completing and cleaning up, ceramic body is placed in sintering furnace, is added Heat keeps the temperature 3 hours, to 140 DEG C to remove moisture contained therein;600 DEG C are heated under air environment again, keeps the temperature 6 hours, with Remove bonding agent ingredient therein;It is finally heated to 1200 DEG C in an inert atmosphere, keeps the temperature 5 hours, makes manganese-zinc ferrite It is powder sintered at solid ceramic finished part.

Claims (5)

1. a kind of increasing material manufacturing method of silicon carbide ceramics, includes the steps that following:
1) the ceramic part model printed will be needed to be layered, determines every layer of region for needing to bond, and generate control program.
2) one layer of silicon carbide ceramics powder of laying on trays;
3) thermosetting resin bonding agent is sprayed on the region that this layer needs to bond, the thermosetting resin bonding agent using nozzle Including epoxy monomer and curing agent;
4) using the thermosetting resin bonding agent on this layer of ceramic powders of heating devices heat, heat cure cross-linked polymeric is brought it about Reaction bonds this layer of ceramic powders;
5) successively printing, until forming complete ceramic body;
6) ceramic body is cleaned up, removes the unglued ceramic powders adhered to thereon;
7) ceramic body after cleaning is placed in sintering furnace, is heated to 140 DEG C, keep the temperature 3 hours;It is heated under air environment again To 700 DEG C, 5 hours are kept the temperature;It is finally heated to 2020 DEG C in an inert atmosphere, keeps the temperature 10 hours, sinters solid ceramic into Finished part.
2. the manufacturing method according to claim 1, which is characterized in that the particle diameter of ceramic powders is in 10nm-1000nm.
3. the manufacturing method according to claim 1, which is characterized in that use three epoxy-phenyl para-aminophenol TGAP, four The mixture of epoxy-phenyl diaminodiphenylmethane TGDDM is as epoxy monomer;Made using diethyl toluene diamine DETDA For curing agent, the molar ratio of TGAP, TGDDM and DETDA are 2:1:5.
4. the manufacturing method according to claim 1, which is characterized in that used manufacturing equipment includes:Rack carries The feed tray of ceramic powders as raw material, trays, stone scraper plate, curing agent delivery pipe, epoxy monomer conveying Pipe, mixing chamber, nozzle and heating device, feed tray and trays can move up and down, and stone scraper plate is for will be above machine The raw ceramic materials powder of frame rushes at trays, so that it is formed one layer of uniform material layer to be printed on trays, firmly Agent delivery pipe and epoxy monomer delivery pipe are connected to mixing chamber, and nozzle is used for the thermosetting that will be obtained after mixing chamber mixes Property resin adhesive according to control program be injected in the region that every layer of specified needs bond on trays;Heating device is used for Heating work pallet and its material layer to be printed of carrying make its temperature be higher than the solidification temperature of thermosetting resin.
5. according to the method described in claim 4, it is characterized in that, being disposed with water cooling plant around nozzle and mixing chamber.
CN201810747328.8A 2018-07-09 2018-07-09 A kind of increasing material manufacturing method of silicon carbide ceramics Pending CN108863392A (en)

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Cited By (3)

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CN114474707A (en) * 2022-02-10 2022-05-13 北京京城增材科技有限公司 Method for manufacturing silicon carbide substrate for aluminizing
CN115233301A (en) * 2022-09-21 2022-10-25 青禾晶元(天津)半导体材料有限公司 Porous silicon carbide ceramic crystal support and preparation method and application thereof
CN115286394A (en) * 2022-07-28 2022-11-04 中国科学院上海硅酸盐研究所 Preparation method of silicon carbide ceramic material for binder jet printing

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CN105778423A (en) * 2016-04-09 2016-07-20 余若冰 Novel thermosetting 3D printing material
CN107325770A (en) * 2017-05-26 2017-11-07 苏州汉力新材料有限公司 A kind of 3D printing powder binding agent and its application

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CN115286394A (en) * 2022-07-28 2022-11-04 中国科学院上海硅酸盐研究所 Preparation method of silicon carbide ceramic material for binder jet printing
CN115233301A (en) * 2022-09-21 2022-10-25 青禾晶元(天津)半导体材料有限公司 Porous silicon carbide ceramic crystal support and preparation method and application thereof
CN115233301B (en) * 2022-09-21 2022-12-02 青禾晶元(天津)半导体材料有限公司 Porous silicon carbide ceramic crystal support and preparation method and application thereof

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