CN104628393A - Preparation method of high-performance ceramic - Google Patents
Preparation method of high-performance ceramic Download PDFInfo
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- CN104628393A CN104628393A CN201510082675.XA CN201510082675A CN104628393A CN 104628393 A CN104628393 A CN 104628393A CN 201510082675 A CN201510082675 A CN 201510082675A CN 104628393 A CN104628393 A CN 104628393A
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Abstract
The invention relates to the field of ceramic materials and in particular relates to a preparation method of a high-performance ceramic. The preparation method of the high-performance ceramic comprises the following steps: a) preparing a ceramic part biscuit; b) dumping; c) carrying out isostatic cool pressing treatment; d) presintering; e) preparing a hot isostatic pressing sheath, concretely carrying out synchronous powder feeding and laser cladding treatment, and coating the ceramic part biscuit with the hot istostic pressing sheath; f) hot isostatic pressing sintering; and g) removing the hot isostatic pressing sheath, and precisely processing a ceramic part. The preparation method of the high-performance ceramic has the advantages that multiple technologies are combined, so that a complex ceramic part biscuit can be prepared through selective laser sintering, near-net forming of a complex ceramic part is realized, and compactness of the part biscuit subject to aftertreatment is improved; meanwhile, no vacuumizing or encapsulating needs to be carried out, and production processes are reduced; besides, technique is simple, period is short, efficiency is high, cost is low, and the obtained ceramic part is high in strength and good in performance.
Description
Technical field
The present invention relates to stupalith field, particularly relate to a kind of preparation method of high-performance ceramic.
Background technology
Engineering ceramics is also known as structural ceramics, and the high rigidity possessed with itself, high strength, high-wearing feature and good antiseptic property, be widely used in fields such as oil, chemical industry, machinery, medical science.Traditional ceramics forming method is applicable to the simple part of preparation, and complex-shaped component, usually need the mould by complexity to realize, manufacturing cost is high, and the manufacturing cycle is long.
SLS technology adopts laser selectable layering sintering solid powder, and the cured layer of sinter molding is superposed, and generates the product of desired shape.SLS forming method has manufacturing process simple, degree of flexibility is high, material selection range is wide, material price is cheap, the features such as cost is low, material use efficiency is high, and shaping speed is fast, SLS is made to be suitable for many fields, as prototype checking, mould master mold, essence casting fusible pattern, automobile and other industries.When utilizing SLS technology formed ceramic parts, need to add the lower macromolecular material of fusing point as binding agent, the part blanks obtained also will remove binding agent by binder removal, can sinter after isostatic cool pressing process makes biscuit reach some strength and density.
In order to increase intensity and the density of pottery, people introduce jacket HIP sintering technique, it to have the coated ceramic body of fine and close air-locked metal capsule or to be placed in airtight container through the ceramic part of presintering, using high-pressure inert gas or nitrogen as transmission medium, under High Temperature High Pressure effect, part is sintered, obtain high densification sintered compact.The most outstanding feature of jacket HIP sintering technology have employed high pressure, sintering temperature required for part is reduced greatly, even also can be able to prepare under without the condition of sinter additives high reliability, microstructure evenly, hardly containing the complete dense material of pore.Conventional metals jacket adopts weldprocedure to seal usually, can only be applicable to the part of simple shape, and also will vacuumize jacket before welding, and complex process, difficulty and cost are very high.
In recent years, some researchists have attempted laser powder rapid shaping to combine with hot isostatic pressing technique, such as CN101391302 describes and utilizes selective laser melting (SLM) shaping jacket, and the method is mainly used in the hot isostatic pressing of metal-powder.Ceramic member is prepared according to this method, reserved powder inlet is then needed to load ceramic powder wherein, needing first to vacuumize (being almost difficult to realize) after ram-jolt powder carries out carrying out hot isostatic pressing after welding encapsulates again, complex process, and shrinkage too large (being greater than 50%) during HIP sintering, product size is difficult to control, and for the more complicated part of some structures, regional area is difficult to ram-jolt, cause product to shrink seriously uneven, intelligence manufacture and the near-net-shape of 3D printing can not be realized.
Summary of the invention
Object of the present invention solves above-mentioned prior art produced problem exactly, provides a kind of preparation method of high-performance ceramic.
For this reason, the invention discloses a kind of preparation method of high-performance ceramic, it comprises the following steps:
A) ceramic part part base preparation;
B) binder removal process;
C) isostatic cool pressing process;
D) presintering process;
E) hot isostatic pressing jacket makes: synchronous powder feeding system Laser Cladding Treatment, the coated hot isostatic pressing jacket of ceramic part base substrate;
F) HIP sintering;
G) hot isostatic pressing jacket is removed, precision sizing ceramic part.
In certain embodiments, described binder removal is treated to and first rises to softening point temperature T1-10 DEG C with the speed of 3 ~ 6 DEG C/min, then rises to 150 DEG C with the heat-up rate of 2 ~ 4 DEG C/min and eliminate water vapour, insulation 1h, finally rise to T2+50 DEG C with the speed of 2 DEG C/min, insulation 2h; Binding agent fusing point or softening temperature T1, complete decomposition temperature T2.Wherein preferred, described binder removal is treated to and rises to softening point temperature 70 DEG C with the speed of 4 DEG C/min, then rises to 150 DEG C with the heat-up rate of 2 DEG C/min and eliminate water vapour, and insulation 1h, finally rises to 700 DEG C with the speed of 2 DEG C/min, insulation 2h; Or rise to softening point temperature 90 DEG C with the speed of 4 DEG C/min, then rise to 150 DEG C with the heat-up rate of 2 DEG C/min and eliminate water vapour, insulation 1h, finally rises to 700 DEG C with the speed of 2 DEG C/min, insulation 2h.
In certain embodiments, described isostatic cool pressing is treated to isostatic cool pressing blowdown rate 2 ~ 6MPa/s, and pressure rises to 200 ~ 350MPa, pressurize 30s step-down again.
In certain embodiments, described presintering treatment temp is lower than temperature during HIP sintering, and gas atmosphere is determined by agglomerated material.
In certain embodiments, described step e is ceramic part base substrate, synchronous powder feeding system laser cladding equipment molding space put into by substrate, ceramic part base substrate bottom center, substrate center overlap with molding space coordinate origin, and ceramic part base substrate direction and jacket three-dimensional model one_to_one corresponding, start lamination under vacuum conditions and make hot isostatic pressing jacket; Metal-powder particle diameter used 20 ~ 100 μm, its material adjusts according to ceramic part material, hot isostatic pressing jacket at high temperature has lower yield strength and good plastic deformation ability, and in hot isostatic pressing, the pressure of gaseous media passes through metal capsule stepless action on ceramic member.And sheath material at high temperature has good deformability, the isolation of jacket internal and external environment can be ensured.
Described hot isostatic pressing jacket and ceramic part base substrate shrink-fit, to make to be wrapped in lamination print procedure cladding on ceramic body, jacket thickness 0.1 ~ 5mm.
Synchronous powder feeding system method controllability is good, easily realizes automatization, does not interfere in the process making jacket with ceramic body part.
In certain embodiments, described HIP sintering is that sintering temperature is determined by agglomerated material, selects argon gas or nitrogen as HIP atmosphere, pressure 100 ~ 300MPa.
In certain embodiments, the method for described removal hot isostatic pressing jacket has: machinery is removed, laser cutting, is mainly used in simple part jacket; Acid etching, is mainly used in complex-shaped metal capsule.
Patent of the present invention combines rapid shaping technique, synchronous powder feeding system laser melting and coating technique, isostatic cool pressing technology and hot isostatic pressing technique, complicated ceramic part base substrate can be manufactured by selective laser sintering, with synchronous powder feeding system laser cladding equipment, metal in close cladding is formed jacket in pre-sintered ceramic piece surface, after high temperature sintering, achieve the near-net-shape of complicated ceramic part.The method technique is simple, and the cycle is short, and efficiency is high, and cost is low, and the ceramic part intensity of making is high, and performance is good.
Accompanying drawing explanation
Fig. 1 gear part sketch and the coated sectional view of jacket thereof;
Fig. 2 gear jacket makes schematic diagram and side direction powder-supplying spray head sketch;
Fig. 3 Si
3n
4pottery Fracture scan sem image compares;
Fig. 4 manual acetabulum prosthese sketch;
Fig. 5 jacket makes schematic diagram and coaxial powder-feeding shower nozzle sketch;
Fig. 6 Al
2o
3pottery Fracture scan sem image compares.
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further.These embodiments are only not used in for illustration of the present invention and limit the scope of the invention.The experimental technique of unreceipted actual conditions in the following example, the usually conveniently conditioned disjunction condition of advising according to manufacturer.Unless otherwise indicated, otherwise all per-cent and number all by weight.
Unless otherwise defined, all specialties used in literary composition and scientific words and one skilled in the art the same meaning be familiar with.In addition, any method similar or impartial to described content and material all can be applicable in the inventive method.The use that better implementation method described in literary composition and material only present a demonstration.
Embodiment 1:Si
3n
4(participate in Fig. 1, A is gear base substrate to gear part, and B is the gear base substrate being covered with hot isostatic pressing jacket, and wherein 1 is gear base substrate; 2 is jacket)
(1) use the three-dimensional digital model of 3-D Moulding Design software (as UG, Solidworkds) design gear and jacket thereof, and import Selective Laser Sintering after being transferred to STL form with slicing delamination software.
(2) Si of sintering aid will be mixed with according to certain ratio
3n
4powder, two atmosphere A type epoxy powder mix rear Selective Laser Sintering lamination by ball milling and print Si
3n
4gear biscuit.Si used
3n
4granulating powders particle diameter 20 ~ 150 μm, bisphenol A type epoxy resin powder diameter 10 ~ 80 μm.In Selective Laser Sintering, laser apparatus used is the CO of 50w
2laser apparatus, pre-heating temperature 40 ~ 60 DEG C, thickness in monolayer 0.1 ~ 0.2mm, sweep span 0.1 ~ 0.2mm, sweep velocity 800 ~ 4000mm/s.
(3) to Si
3n
4gear part base substrate carries out binder removal process, the agent of removing low temperature bonding.First rise to softening point temperature 70 DEG C with the speed of 4 DEG C/min, then rise to 150 DEG C with the heat-up rate of 2 DEG C/min and eliminate water vapour, insulation 1h, finally rises to 700 DEG C with the speed of 2 DEG C/min, insulation 2h.
(4) to Si
3n
4gear base substrate carries out isostatic cool pressing process, isostatic cool pressing buck speed 2 ~ 6MPa/s, and pressure rises to 200 ~ 350MPa, pressurize 30s pressure release again.
(5) by the Si after isostatic cool pressing
3n
4gear part carries out presintering, and sintering atmosphere is nitrogen, calcined temperature 1400 ~ 1650 DEG C.
(6) by the Si through pre-burning
3n
4molding space put into by gear, substrate, Si
3n
4gear base substrate bottom center, substrate center overlap with molding space coordinate origin, and base substrate part direction and jacket three-dimensional model one_to_one corresponding, start lamination under vacuum conditions and make hot isostatic pressing jacket.Metal-powder particle diameter used 20 ~ 100 μm, fusing point is greater than 1550 DEG C.(participation Fig. 2)
(7) Si of jacket will be covered with
3n
4gear is put into hot isostatic pressing stove and is carried out high temperature sintering.Sintering temperature 1550 ~ 1700 DEG C, select argon gas or nitrogen as HIP atmosphere, pressure is 100 ~ 300MPa, and top temperature soaking time is 1 ~ 6h.
(8) hot isostatic pressing metal capsule is removed by acid etching, then precision sizing Si
3n
4gear part.
(9) performance test: the Si that above-mentioned processing step manufactures
3n
4part, microtexture is even, and relative density is more than 99%, and measuring method is with reference to GB/T 3850; Hardness (HV10) is at 1500kgf/mm
2above, measuring method is with reference to GB/T 16534; Fracture toughness property is at 6.0MPam
1/2above, measuring method is with reference to ASTMF2094; Three-point bending resistance intensity is at more than 1000MPa, and measuring method is with reference to GB/T 6569, and the Weibull modulus calculated by bending strength can reach more than 12.
(10) carry out fracture observation by scanning electron microscope, photo as shown in Figure 3, the Si that A figure is prepared for method described in patent of the present invention
3n
4pottery fracture, because sintering time is shorter, comparatively traditional method is low for sintering temperature, therefore tiny, the even size distribution of its crystal grain, and Si prepared by traditional method
3n
4pottery (B figure) coarse grains, distribution of sizes are uneven.
Embodiment 2: preparation Al
2o
3manual acetabulum (see Fig. 4)
(1) three-dimensional digital model of manual acetabulum and compression molding metal die is designed with 3-D Moulding Design software (as UG, Solidworks).
(2) Al of the materials such as releasing agent, sintering agent, binding agent will be mixed with
2o
3powder carries out compression molding, manufacturing artificial acetabular component biscuit.
(3) to Al
2o
3manual acetabulum base substrate carries out binder removal process, except no-bonder.First rise to softening point temperature 90 DEG C with the speed of 4 DEG C/min, then rise to 150 DEG C with the heat-up rate of 2 DEG C/min and eliminate water vapour, insulation 1h, finally rises to 700 DEG C with the speed of 2 DEG C/min, insulation 2h.
(4) to Al
2o
3manual acetabulum base substrate carries out isostatic cool pressing process, isostatic cool pressing buck speed 2 ~ 6MPa/s, and pressure rises to 200 ~ 350MPa, pressurize 20s step-down again.
(5) by the Al after isostatic cool pressing
2o
3manual acetabulum base substrate carries out presintering, calcined temperature 1000 ~ 1200 DEG C.
(6) by the Al of presintering
2o
3synchronous powder feeding system laser cladding equipment molding space put into by manual acetabulum base substrate, substrate, Al
2o
3manual acetabulum base substrate bottom center, substrate center overlap with molding space coordinate origin, and base substrate part direction and jacket three-dimensional model one_to_one corresponding, start lamination under vacuum conditions and make jacket.Metal-powder particle diameter used 20 ~ 100 μm, fusing point is greater than 1200 DEG C.(see Fig. 5)
(7) Al of metal capsule will be covered with
2o
3manual acetabulum base substrate is put into hot isostatic pressing stove and is carried out high temperature sintering.Sintering temperature 1200 ~ 1400 DEG C, selects argon gas or nitrogen as HIP atmosphere, gaseous tension 100 ~ 200MPa.
(8) jacket, then precision sizing Al is removed by laser cutting or mechanical workout
2o
3manual acetabulum part.
(9) performance test: the Al that above-mentioned processing step manufactures
2o
3part, microtexture is even, and relative density is more than 99%, and measuring method is with reference to GB/T 3850; Hardness (HV10) is at 1800kgf/mm
2above, measuring method is with reference to GB/T 16534; Fracture toughness property is at 5.0MPam
1/2above, measuring method is with reference to ASTM F2094; Three-point bending resistance intensity is at more than 600MPa, and measuring method is with reference to GB/T 6569, and the Weibull modulus calculated by bending strength can reach more than 12.
(10) carry out fracture observation by scanning electron microscope, photo as shown in Figure 6, the Al that A figure is prepared for method described in patent of the present invention
2o
3pottery fracture, because sintering time is shorter, temperature is lower, its crystal grain is tiny, size is divided evenly, and Al prepared by traditional method
2o
3pottery (B figure) coarse grains, distribution of sizes are uneven.
Scope of the present invention is not by the restriction of described specific embodiments, and described embodiment, only as the single example of illustrating all respects of the present invention, also comprises method and the component of functional equivalent in the scope of the invention.In fact, except content as herein described, those skilled in the art can easily grasp multiple improvement of the present invention with reference to description above and accompanying drawing.Described improvement also falls within the scope of appended claims.Every section of reference mentioned above is listed in herein as a reference all in full.
Claims (10)
1. a preparation method for high-performance ceramic, it comprises the following steps:
A) ceramic part part base preparation;
B) binder removal process;
C) isostatic cool pressing process;
D) presintering process;
E) hot isostatic pressing jacket makes: synchronous powder feeding system Laser Cladding Treatment, the coated hot isostatic pressing jacket of ceramic part part base;
F) HIP sintering;
G) hot isostatic pressing jacket is removed, precision sizing ceramic part.
2. preparation method according to claim 1, it is characterized in that described binder removal is treated to and first rise to softening point temperature T1-10 DEG C with the speed of 3 ~ 6 DEG C/min, rise to 150 DEG C with the heat-up rate of 2 ~ 4 DEG C/min again and eliminate water vapour, insulation 1h, finally rise to T2+50 DEG C with the speed of 2 DEG C/min, insulation 2h; Binding agent fusing point or softening temperature T1, complete decomposition temperature T2; Binding agent fusing point or softening temperature are T1, and the complete decomposition temperature of binding agent is T2.
3. preparation method according to claim 2, it is characterized in that described binder removal is treated to and rise to softening point temperature 70 DEG C with the speed of 4 DEG C/min, then rise to 150 DEG C with the heat-up rate of 2 DEG C/min and eliminate water vapour, insulation 1h, finally rise to 700 DEG C with the speed of 2 DEG C/min, insulation 2h.
4. preparation method according to claim 2, it is characterized in that the speed that described binder removal is treated to 4 DEG C/min rises to softening point temperature 90 DEG C, then rise to 150 DEG C with the heat-up rate of 2 DEG C/min and eliminate water vapour, insulation 1h, finally rise to 700 DEG C with the speed of 2 DEG C/min, insulation 2h.
5. preparation method according to claim 1, it is characterized in that described isostatic cool pressing is treated to isostatic cool pressing blowdown rate 2 ~ 6MPa/s, pressure rises to 200 ~ 350MPa, pressurize 30s step-down again.
6. preparation method according to claim 1, it is characterized in that described presintering treatment temp is lower than temperature during HIP sintering, gas atmosphere is determined by agglomerated material.
7. preparation method according to claim 1, it is characterized in that described step e is ceramic part part base, synchronous powder feeding system laser cladding equipment molding space put into by substrate, ceramic part Jian Pi bottom center, substrate center overlap with molding space coordinate origin, and ceramic part base substrate direction and jacket three-dimensional model one_to_one corresponding, start lamination under vacuum conditions and make hot isostatic pressing jacket.
8. preparation method according to claim 7, is characterized in that described hot isostatic pressing jacket and ceramic part part base shrink-fit, thickness 0.1 ~ 5mm.
9. preparation method according to claim 7, it is characterized in that described hot isostatic pressing jacket adopts metal-powder, its particle diameter 20 ~ 100 μm, its material adjusts according to ceramic part material.
10. preparation method according to claim 1, described HIP sintering is that sintering temperature is determined by agglomerated material, selects argon gas or nitrogen as HIP atmosphere, pressure 100 ~ 300MPa.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105130429A (en) * | 2015-07-30 | 2015-12-09 | 重庆卓田齿克科技有限公司 | Zirconia ceramic block production technology |
| CN108456002A (en) * | 2018-02-08 | 2018-08-28 | 广东工业大学 | A method of being suitable for the 3D printing ceramic component based on Stereolithography of selfreparing/self-reinforcing |
| CN110125390A (en) * | 2018-02-08 | 2019-08-16 | 罗天珍 | The padding and compacting sintering process of 3 D-printing metal powder bond blank |
| CN110494236A (en) * | 2017-03-20 | 2019-11-22 | 斯特拉塔西斯公司 | Use the method and system of the material increasing material manufacturing of powder |
| CN110961624A (en) * | 2018-04-26 | 2020-04-07 | 罗天珍 | Filling degreasing and compaction sintering method for three-dimensional printed powder bonding blank |
| CN112521130A (en) * | 2019-08-28 | 2021-03-19 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of ceramic part based on 3D printing technology |
| US11059100B2 (en) | 2016-04-11 | 2021-07-13 | Stratasys Ltd. | Method and apparatus for additive manufacturing with powder material |
| CN113563087A (en) * | 2021-07-05 | 2021-10-29 | 淄博国创中心先进车用材料技术创新中心 | Silicon nitride ceramic component and method for producing same |
| CN113563088A (en) * | 2021-07-30 | 2021-10-29 | 淄博国创中心先进车用材料技术创新中心 | Porous silicon nitride ceramic component and method for producing same |
| CN113929475A (en) * | 2021-11-03 | 2022-01-14 | 中科听海(苏州)电子科技有限责任公司 | Method for preparing piezoelectric ceramic based on hot isostatic pressing process |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105130429A (en) * | 2015-07-30 | 2015-12-09 | 重庆卓田齿克科技有限公司 | Zirconia ceramic block production technology |
| US11059100B2 (en) | 2016-04-11 | 2021-07-13 | Stratasys Ltd. | Method and apparatus for additive manufacturing with powder material |
| US11691196B2 (en) | 2016-04-11 | 2023-07-04 | Stratasys Ltd. | Method and apparatus for additive manufacturing with powder material |
| CN110494236B (en) * | 2017-03-20 | 2022-07-26 | 斯特拉塔西斯公司 | Method and system for additive manufacturing of materials using powders |
| CN110494236A (en) * | 2017-03-20 | 2019-11-22 | 斯特拉塔西斯公司 | Use the method and system of the material increasing material manufacturing of powder |
| US11400516B2 (en) | 2017-03-20 | 2022-08-02 | Stratasys Ltd. | Method and system for additive manufacturing with powder material |
| CN108456002A (en) * | 2018-02-08 | 2018-08-28 | 广东工业大学 | A method of being suitable for the 3D printing ceramic component based on Stereolithography of selfreparing/self-reinforcing |
| CN110125390A (en) * | 2018-02-08 | 2019-08-16 | 罗天珍 | The padding and compacting sintering process of 3 D-printing metal powder bond blank |
| CN108456002B (en) * | 2018-02-08 | 2021-03-16 | 广东工业大学 | Method for 3D printing of ceramic component based on photocuring forming and suitable for self-repairing/self-enhancing |
| CN110961624A (en) * | 2018-04-26 | 2020-04-07 | 罗天珍 | Filling degreasing and compaction sintering method for three-dimensional printed powder bonding blank |
| CN112521130A (en) * | 2019-08-28 | 2021-03-19 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of ceramic part based on 3D printing technology |
| CN113563087A (en) * | 2021-07-05 | 2021-10-29 | 淄博国创中心先进车用材料技术创新中心 | Silicon nitride ceramic component and method for producing same |
| CN113563088A (en) * | 2021-07-30 | 2021-10-29 | 淄博国创中心先进车用材料技术创新中心 | Porous silicon nitride ceramic component and method for producing same |
| CN113929475A (en) * | 2021-11-03 | 2022-01-14 | 中科听海(苏州)电子科技有限责任公司 | Method for preparing piezoelectric ceramic based on hot isostatic pressing process |
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Address after: 200437 No. 99, Handan Road, Shanghai, Hongkou District Patentee after: Shanghai Material Research Institute Co.,Ltd. Address before: 200437 No. 99, Handan Road, Shanghai, Hongkou District Patentee before: SHANGHAI Research Institute OF MATERIALS |
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