CN106007723A - Making method of SiC ceramic green body - Google Patents
Making method of SiC ceramic green body Download PDFInfo
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- CN106007723A CN106007723A CN201610343281.XA CN201610343281A CN106007723A CN 106007723 A CN106007723 A CN 106007723A CN 201610343281 A CN201610343281 A CN 201610343281A CN 106007723 A CN106007723 A CN 106007723A
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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
- C04B35/515—Shaped 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
- C04B35/56—Shaped 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
- C04B35/565—Shaped 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
-
- 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
- B28B1/001—Rapid manufacturing of 3D objects by additive depositing, agglomerating or laminating of material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE 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
- B33Y10/00—Processes of additive manufacturing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE 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
- B33Y70/00—Materials specially adapted for additive manufacturing
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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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
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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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3817—Carbides
- C04B2235/3821—Boron carbides
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/422—Carbon
- C04B2235/424—Carbon black
Abstract
The invention relates to making method of a SiC ceramic green body. The method comprises the following steps: mixing SiC powder, a sintering aid, a bonding agent and a solvent by ball milling to obtain a mixed sizing agent; drying the mixed sizing agent or performing spray granulation to obtain uniformly-mixed SiC ceramic powder of which the particle diameter is between 50mum and 100mum; constructing a structural model of the SiC ceramic green body by computer-aided design software, and gradually printing the SiC ceramic powder by a laser powder fusion making technology or a liquid-state photosensitive resin making technology till the SiC ceramic green body is formed, wherein the single-layer thickness is 0.1-0.2mm. A three-dimensional printing technology is adopted, so that SiC ceramics of different structures can be made as required through a computer-aided design; the method has the advantages of no need of any mold during molding, low complexity sensitivity to a product, high product development speed and the like.
Description
Technical field
The present invention relates to a kind of method that 3D printing technique prepares carborundum (SiC) biscuit of ceramics, belong to SiC ceramic neck
Territory.
Background technology
Carborundum (SiC) has the characteristics such as atomic radius is little, bond distance is short, covalency key is strong, thus has excellent power
, calorifics, electric property and chemical stability, have the characteristics such as resistance to irradiation, radioresistance, suction ripple simultaneously, be important core
The reactor material of resistance to neutron irradiation and wave-absorbing and camouflage material, be widely used in precision bearing, sealing member, gas-turbine rotor,
Heat exchanger component, atomic heat pile materials and space optics application material etc., and it is increasingly subject to the attention of people, but
The advantages such as the intrinsic high intensity of SiC ceramic, high rigidity bring a lot of difficulty to its molding, processing simultaneously. especially shape
Complicated ceramic component, it usually needs realize by means of complicated mould. and the making of complicated die has the highest technology difficulty
Degree, needs higher cost of manufacture and longer fabrication cycle, and, mould once completes, and just cannot enter product again
Row amendment. being growing more intense in the market competition, today that the pace of product renewal is accelerated day by day, this production status is the most not
Adapt to the needs of modern enterprise survival and development.
Summary of the invention
For the problems referred to above, it is an object of the invention to provide the molding side of a kind of SiC ceramic material fast, accurately
Method.
To this end, the invention provides a kind of method that 3D printing technique prepares SiC ceramic biscuit, including:
SiC powder body, sintering aid, binding agent, solvent are obtained mixed slurry after ball milling mixes；
Gained mixed slurry is dried or mist projection granulating, is uniformly mixed diameter of particle SiC ceramic powder between 50 μm-100 μm
Body；
Utilize the structural model of computer aided design software structure SiC ceramic biscuit and use laser powder body melting manufacturing technology or liquid
SiC ceramic powder body is successively printed until forming described SiC ceramic biscuit by photosensitive resin manufacturing technology, and wherein thickness in monolayer is
0.1-0.2mm。
The SiC that the present invention uses 3D printing technique according to demand, can be prepared different structure by computer-aided design makes pottery
Porcelain, the method forming process is without mould, the highest to the complexity sensitivity of product, has product development fast etc. a series of excellent
Point.
It is preferred that the sintering aid that described sintering aid is B-C system, wherein B content is not higher than SiC powder body and sintering
The 1wt% of auxiliary agent gross mass, C content is not less than SiC powder body and the 2wt% of sintering aid gross mass.
It is preferred that described sintering aid is Al2O3With rare earth oxide mixture, its middle rare earth is Y2O3、
CeO2、Er2O3In at least one.
Also, it is preferred that the quality of described sintering aid is not less than SiC powder body and the 5wt% of sintering aid gross mass.
It is preferred that described binding agent is phenolic resin, polyvinyl alcohol (PVA), polyvinyl butyral resin (PVB), poly-first
At least one in base acrylic acid methyl ester. (PMMA).
Also, it is preferred that the quality of described binding agent is not less than SiC powder body and the 5wt% of sintering aid gross mass.
It is preferred that described solvent is water or dehydrated alcohol.
It is preferred that the solid content of described mixed slurry is 40-50wt%, preferably 40-45wt%.
It is preferred that the parameter of described laser powder body melting manufacturing technology includes: laser power is 12-15W, and scanning speed is
1500-3000mm/s, sweep span is 0.05-0.1mm, and thickness in monolayer is 0.1-0.2mm.Concrete grammar includes: first,
At equipment workbench upper berth a thin layer dusty material, superlaser according to the parameter of each layer cross section of product, has under the control of the computer
Selectively being scanned powder bed, the dusty material in scanned region is bonded together owing to melting, after one layer processes,
Workbench declines the height of a thickness, then carries out next layer of paving powder and scanning, and new machined layer is bonded as one with preceding layer, weight
Multiple said process is till whole component processing completes.
It is preferred that the parameter of described liquid photosensitive resin manufacturing technology includes: photosensitive resin is epoxy-resin systems, content
For the 2-5wt% of powder quality, laser power is 15-50MW, and scanning speed is 2000-4000mm/s, and sweep span is
0.05-0.1mm, thickness in monolayer is 0.1-0.2mm.Specifically, liquid photosensitive resin manufacturing technology is sent by laser instrument
Ultraviolet light, accumulates a light pencil through optical system, and under the control of the computer, scanning mixes this light beam with powder body selectively
Liquid light maleate resin surface, utilize photosensitive resin meet ultraviolet light solidification mechanism.Curing photosensitive resin layer by layer, often solid
After changing one layer, workbench declines an accurate distance, and makes laser scanner to powder surface resin by new layer of surface geological information
It is scanned, makes new one layer of resin solidify and be bonded on the resin that preceding layer is cured, the most repeatedly.Until produce and generate this zero
Part physical model.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the ceramic powder that embodiment 1 is prepared through mist projection granulating；
Fig. 2 is the SiC ceramic structural model figure of the complicated shape that embodiment 1 obtains through computer Aided Design；
Fig. 3 is the SiC ceramic biscuit pictorial diagram of the complicated shape that embodiment 1 is obtained by 3D printing technique；
Fig. 4 is the SEM figure of the ceramic powder that embodiment 2 is prepared through mist projection granulating；
Fig. 5 is the SiC ceramic structural model figure of the complicated shape that embodiment 2 obtains through computer Aided Design；
Fig. 6 is the SiC ceramic biscuit pictorial diagram of the complicated shape that embodiment 2 is obtained by 3D printing technique.
Detailed description of the invention
The present invention is further illustrated, it should be appreciated that following embodiment is merely to illustrate the present invention below in conjunction with embodiment,
And the unrestricted present invention.
The present invention prepares the uniform mixed powder of sintered SiC.Designed difform by computer aided technique simultaneously
SiC ceramic structure.To be prepared by liquid photosensitive resin manufacturing technology or powder body lf manufacturing technology the most again
SiC powder body 3D is printed as SiC ceramic biscuit material.
The following exemplary ground explanation present invention utilizes the method that 3D printing technique prepares SiC ceramic biscuit.
The present invention, with SiC powder body as raw material, adds sintering aid, binding agent (such as, phenolic resin, polyvinyl alcohol
(PVA), polyvinyl butyral resin (PVB), polymethyl methacrylate (PMMA) etc.), solvent (such as, water or
Dehydrated alcohol) obtain the mixed slurry that solid content is 40-50wt%, preferably 40-45wt% after ball milling mix homogeneously afterwards.Its
In, the quality of described binding agent is not less than SiC powder body and the 5wt% of sintering aid gross mass.
Above-mentioned sintering aid can be the sintering aid of B-C system.Wherein B content is not higher than SiC powder body and sintering aid is total
The 1wt% of quality, C content is not less than SiC powder body and the 2wt% of sintering aid gross mass.
Above-mentioned sintering aid can be also Al2O3With rare earth oxide mixture.Wherein, described rare earth oxide is Y2O3、
CeO2、Er2O3In at least one.Now sintering aid (Al2O3With rare earth oxide mixture) quality be not less than SiC
Powder body and the 5wt% of sintering aid gross mass.
The mixed slurry that solid content is 40-50wt% is directly dried or carried out mist projection granulating, the SiC pottery being uniformly mixed
Porcelain powder body, diameter of particle is between 50 μm-100 μm, as illustrated in figure 1 or 4.This spherical particle diameter 50 μm-
Powder fluidity between 100 μm is excellent, it is simple to laying.
Utilize the structural model of computer aided design software structure SiC ceramic biscuit, as illustrated in fig. 2 or fig. 5.
With the SiC ceramic powder body of mix homogeneously as raw material, according to computer aided design software structure SiC ceramic biscuit
Structural model uses laser powder body melting manufacturing technology successively to be printed by ceramic powder until forming described SiC ceramic biscuit.
Above-mentioned laser powder body melting manufacturing technology is to utilize the heat effect of high energy laser beam to make dusty material soften or fusing, viscous
Form a series of thin layer of type, and progressively superposition obtains 3D solid parts.Concrete parameter includes: laser power is 12-
15W, scanning speed is 1500-3000mm/s, and sweep span is 0.05-0.1mm.Wherein when printing biscuit, the list of printing
Layer thickness (or monolayer thickness) can be called 0.1-0.2mm.
Or with the SiC ceramic powder body of mix homogeneously as raw material, according to computer aided design software structure SiC ceramic element
The structural model of base uses liquid photosensitive resin manufacturing technology successively to be printed by ceramic powder until forming described SiC ceramic biscuit.
Above-mentioned liquid photosensitive resin manufacturing technology is the ultraviolet light sent by laser instrument, accumulates a thin light through optical system
Bundle, this light beam under the control of the computer, scans the liquid light maleate resin surface mixed with powder body selectively, utilizes photosensitive resin
Meet the mechanism of ultraviolet light solidification.Curing photosensitive resin layer by layer, often after solidification one layer, workbench declines an accurate distance,
And make laser scanner be scanned to powder surface resin by new layer of surface geological information, make new one layer of resin solidify and glue
On the resin that preceding layer is cured, the most repeatedly.Until producing and generating this material object parts model.Its technique is based on liquid light
The photopolymerization principle work of quick resin.This liquid material is in certain wavelength (such as, λ=325nm) and power (example
Such as, P=30MW) ultraviolet light irradiate under photopolymerization reaction, material can be occurred rapidly to change from liquid to solid.Concrete ginseng
Number includes: photosensitive resin is epoxy-resin systems, and content is the 2-5wt% of powder quality, and laser power can be 15-50MW,
Scanning speed can be 2000-4000mm/s, and sweep span can be 0.05-0.1mm.Wherein when printing biscuit, the monolayer of printing
Thickness (or monolayer thickness) can be called 0.1-0.2mm.
Enumerate embodiment further below to describe the present invention in detail.It will similarly be understood that following example are served only for this
Bright it is further described, it is impossible to being interpreted as limiting the scope of the invention, those skilled in the art is according to the present invention's
Some nonessential improvement and adjustment that foregoing is made belong to protection scope of the present invention.The technique ginseng that following example is concrete
Number etc. is the most only an example in OK range, in the range of i.e. those skilled in the art can be done suitably by explanation herein
Select, and do not really want to be defined in the concrete numerical value of hereafter example.
Embodiment 1
By SiC powder body 965g, sintering aid B4C (0.5wt%) 5g, C black (3wt%) 30g, powder body 1000g altogether, additionally add
Enter phenolic resin 100g, PMMA 100g mixing, be made into the slurry (solvent is dehydrated alcohol) that solid content is 45wt%, with
SiC ball 2000g is ball-milling medium, mixes 24h, and it is about 60 μm that mist projection granulating obtains the size of mix homogeneously powder body
SiC powder body, as shown in Figure 1.Obtain difform SiC ceramic structure according to computer-aided design, such as Fig. 2 simultaneously
Shown in.Manufacturing 3D printing technique, laser power 15W by laser powder body melting, scanning speed is 1500mm/s, scanning
Spacing is 0.1mm.The thickness that wherein monolayer prints is 0.1mm.Powder body is printed the SiC ceramic biscuit obtaining complicated shape,
As shown in Figure 3.Fig. 3 is the SiC heat exchanger plate biscuit printed.
Embodiment 2
By SiC powder body 900g, Al2O3And Y2O3(10wt%) 100g 1000g powder body altogether, it is possible to additionally incorporate PVA5g, PMMA
100g mixes, and is made into the slurry (solvent is water) that solid content is 45wt%, with SiC ball 2000g as ball-milling medium, and mixing
24h, it is the SiC powder body (as shown in Figure 4) about 50 μm that mist projection granulating obtains mix homogeneously diameter of particle size.Simultaneously
Difform SiC ceramic structure is obtained, as shown in Figure 5 according to computer-aided design.Beaten by laser powder body melting 3D
Print technology, laser power 14W, scanning speed is 3000mm/s, and sweep span is 0.1mm.The thickness that wherein monolayer prints
For 0.2mm.Powder body is printed the SiC ceramic biscuit obtaining complicated shape, as shown in Figure 6.Fig. 6 is the SiC reflection printed
Mirror biscuit.
Claims (10)
1. the preparation method of a SiC ceramic biscuit, it is characterised in that including:
SiC powder body, sintering aid, binding agent, solvent are obtained mixed slurry after ball milling mixes；
Gained mixed slurry is dried or mist projection granulating, is uniformly mixed diameter of particle SiC ceramic powder body between 50 μm-100 μm；
Utilizing the structural model of computer aided design software structure SiC ceramic biscuit and use laser powder body melting manufacturing technology or liquid photosensitive resin manufacturing technology successively to be printed by SiC ceramic powder body until forming described SiC ceramic biscuit, wherein thickness in monolayer is 0.1-0.2mm.
Method the most according to claim 1, it is characterised in that described sintering aid is the sintering aid of B-C system, wherein B content is not higher than SiC powder body and the 1wt% of sintering aid gross mass, and C content is not less than SiC powder body and the 2wt% of sintering aid gross mass.
Method the most according to claim 1, it is characterised in that described sintering aid is Al2O3With rare earth oxide mixture, described rare earth oxide is Y2O3、CeO2、Er2O3In at least one.
Method the most according to claim 3, it is characterised in that the quality of described sintering aid is not less than SiC powder body and the 5wt% of sintering aid gross mass.
5. according to the method according to any one of claim 1-4, it is characterised in that described binding agent is at least one in phenolic resin, PVAC polyvinylalcohol, polyvinyl butyral resin PVB, polymetylmethacrylate.
Method the most according to claim 5, it is characterised in that the quality of described binding agent is not less than SiC powder body and the 5wt% of sintering aid gross mass.
7. according to the method according to any one of claim 1-6, it is characterised in that described solvent is water or dehydrated alcohol.
8. according to the method according to any one of claim 1-7, it is characterised in that the solid content of described mixed slurry is 40-50wt%, preferably 40-45wt%.
9. according to the method according to any one of claim 1-8, it is characterised in that the parameter of described laser powder body melting manufacturing technology includes: laser power is 12-15W, and scanning speed is 1500-3000mm/s, and sweep span is 0.05-0.1mm.
10., according to the method according to any one of claim 1-8, it is characterised in that the parameter of described liquid photosensitive resin manufacturing technology includes: liquid photosensitive resin is epoxy-resin systems, content is the 2-5wt% of powder quality；Laser power is 15-50MW, and scanning speed is 2000-4000mm/s, and sweep span is 0.05-0.1mm.
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| CN106830901A (en) * | 2017-02-20 | 2017-06-13 | 醴陵市陶瓷3D打印研究所 | A kind of ceramic particle and preparation method for laser sintered ceramic 3D printing |
| CN107130752A (en) * | 2017-05-08 | 2017-09-05 | 佛山市蓝瑞欧特信息服务有限公司 | A kind of solar-energy building composite plate structure |
| CN107296985A (en) * | 2017-05-15 | 2017-10-27 | 广东工业大学 | A kind of methods and applications based on Stereolithography 3 D-printing bioceramic scaffold |
| CN108752000A (en) * | 2018-07-07 | 2018-11-06 | 河源市极致知管信息科技有限公司 | A kind of ceramic slurry and preparation method thereof |
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Cited By (24)
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