CN103771837B - Aluminum oxide/zirconium oxide SLM (selective laser melting) ceramic powder material and preparation method thereof - Google Patents
Aluminum oxide/zirconium oxide SLM (selective laser melting) ceramic powder material and preparation method thereof Download PDFInfo
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- CN103771837B CN103771837B CN201310753824.1A CN201310753824A CN103771837B CN 103771837 B CN103771837 B CN 103771837B CN 201310753824 A CN201310753824 A CN 201310753824A CN 103771837 B CN103771837 B CN 103771837B
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Abstract
The invention relates to a novel Al2O3/ZrO2 powder material for SLM (selective laser melting) molding and a preparation method thereof. After molding by laser melting, the powder material forms an oral use Al2O3/ZrO2 composite ceramic material which has uniform internal tissue structure and has no obvious phase segregation. According to the preparation method, an electro-magnetic induction heating furnace and a laser are used for carry out secondary preheating on a powder bed, after achieving the preset preheating temperature, the powder material is molded by laser melting. The gradient of the interior temperature and the exterior temperature of a molten pool in molding of the ceramic material can be effectively reduced, the interior thermal stress can be lowered, cracks on the surface and in the interior of the material are reduced, and the mechanical property of the material is improved. The SLM Al2O3/ZrO2 composite ceramic material molded by the powder material through the preparation method has uniform internal tissues, has no phase segregation, has no obvious cracks on the surface and in the interior, has better mechanical property, and is expected to be used as a material of all-ceramic crown, bridge and inlay to be used in clinic of oral repair.
Description
Technical field
The present invention relates to selective laser melting and coating technique (Selective Laser Melting, SLM) processing ceramic Material Field, be specifically related to a kind of oral cavity aluminum oxide (Al
2o
3)/zirconium white (ZrO
2) preparation method that processes of the powder of diphase ceramic material and its SLM.
Background technology
Aluminum oxide (Al
2o
3) and zirconium white (ZrO
2) composite ceramics reparation physical efficiency reproduction natural teeth color and luster, biology performance is good, can bear and chew load more greatly.The problems such as traditional fabrication mode adopts slip casting, infiltration glass to sinter, and there is technique loaded down with trivial details, and the process-cycle is long.Mainly apply at present dental CAD/CAM system, adopt the mode of numerical control cutting to go material machine-shaping to prefabricated machining ceramics base material after sinter again.According to the high-strength ceramic of dense sintering as base material, its machinability is poor, and stock-removing efficiency is low, tool wear is large.In order to address these problems, the dental CAD being representative with Procera All-ceram/CAM system have employed machining ceramic powder and presses the method tied body or partially sinter body to carry out machine-shaping, carries out fully sintered again, reduce cutting difficulty after cutting to dummy.But, cut a large amount of wastes that the mode of going material to process causes material, add cost of manufacture; Meanwhile, the preparation of pressure knot body needs comparatively complicated equipment and process condition, and double sintering is time-consuming, effort, and volumetric shrinkage during sintering is also fairly obvious, have impact on the making precision of dummy.
Selective laser cladding (Selective Laser Melting, SLM) be the quick increasing material manufacturing technology of a kind of advanced person, take powdered material as raw material, laser irradiation scanning can make powdered material melt and rapid solidification, successively pile up the part that shaping density reaches 100% under the control of the computer, do not limit by structural complexity.The main advantage that it has is: 1. increase material manufacture, the utilization ratio of material is high; 2. once shaped, decreases the step of process operation, reduces cost and difficulty; 3. the processing mode of laser fast thawing rapid hardening imparts the formed material weave construction of uniformity and the mechanical property of excellence more.Because these advantages, SLM technology is applied to rapidly in the every field of materials processing, becomes the focus of research both at home and abroad at present.Chinese scholars can fast and low-cost utilize this fabrication techniques cochrome, pure titanium metal dummy, as the substrate crown etc. of removalbe partial denture bracket, ceramic prosthesis.But utilize the research of SLM technology processing ceramic material less, known research finds there is component segregation and profiled member problems of crack when carrying out ceramic forming material, the mechanical property of forming ceramic part is not enough.
Summary of the invention
The defect existed for above-mentioned prior art or deficiency, the object of the invention is to, and provides a kind of Al shaping for SLM
2o
3/ ZrO
2powdered material and preparation method thereof.
In order to realize above-mentioned task, the present invention takes following technical solution:
A kind ofly prepare shaping Al for SLM
2o
3/ ZrO
2powdered material, is characterized in that, by Al
2o
3powder and ZrO
2powder forms by mass percentage, Al
2o
3powder accounts for 62.5%, ZrO
2powder accounts for 37.5%, wherein, and ZrO
2the Y of 2% is added with in powder
2o
3stablizer, this obtained Al
2o
3/ ZrO
2powdered material D50 particle diameter is less than 100 μm.
Above-mentioned Al
2o
3/ ZrO
2the method that be processed into SLM ceramic block of powdered material on SLM equipment, is characterized in that, by Al
2o
3/ ZrO
2powdered material is laid on pure Al
2o
3on substrate, single berth powder thickness is 500 μm, and every one deck all adopts same procedure first to carry out preheating, and then carries out cladding forming.
Described preheating, the concrete steps of cladding forming are as follows:
1) paving powder equipment is placed on induction heater, is warming up to about 1200 DEG C;
2) be 150W by laser power settings, spot diameter is 10mm, sweep velocity 4000mm/min, and warm up time is 1min, makes the preheating temperature 1700 DEG C that powder bed reaches desirable;
3) step 2) terminate after, adjustment parameter, laser power is 200W, and spot diameter is 8mm sweep velocity is 10mm/min, carries out single track cladding forming;
4) after step 3) terminates, carry out second time and spread powder, paving powder thickness is 500 μm, is struck off on powder bed surface with scraper plate, then again according to step 1), step 2) order carries out the single track cladding forming of new one deck; Through repeatedly spreading powder, after single track cladding forming, namely form SLM ceramic block material.
Adopt Al of the present invention
2o
3/ ZrO
2powdered material, can be processed into SLM ceramic block on SLM equipment, its interior tissue uniformity, empty phase segregation, surface and inside generate without obvious crackle, and mechanical property is better, be expected to be used as all-ceramic crown, the materials application of bridge and inlay is in oral repairing clinic.Solve the component segregation of prior art and the problem of crackle formation, finally lay the foundation for SLM technology is applied to all-ceramic prosthesis making.
Accompanying drawing explanation
Fig. 1 is that A group powder mixes last ESM photo (50 times);
Fig. 2 is B group powder ESM photo photo (50 times);
Fig. 3 is C group powder ESM photo (100 times);
Fig. 4 is D group powder ESM photo (100 times);
Fig. 5 is different powder grouping test specimen vickers hardness number mean value histogram;
Fig. 6 is A group ESM photo (500 times);
Fig. 7 is B group ESM photo (500 times);
Fig. 8 is C group ESM photo (500 times);
Fig. 9 is B group SEM photo (longitudinal section, 1000 times);
Figure 10 is B group SEM photo (5000 times);
Figure 11 is clear zone point 1 energy spectrum analysis figure;
Figure 12 is different powder mixture ratio grouping test specimen vickers hardness number mean value histogram;
Figure 13 is B group crystalline structure schematic perspective view;
Figure 14 is induction heater schematic diagram;
Figure 15 is experimental system schematic diagram;
Figure 16 is the photo of shaping SLM ceramic block material.
Figure 17 is a kind of structural representation spreading powder equipment.
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Embodiment
The present embodiment provides a kind ofly prepares shaping Al for SLM
2o
3/ ZrO
2powdered material, with Al
2o
3and ZrO
2powder is raw material, according to mass percent preparation, and Al
2o
3powder accounts for 62.5wt%, ZrO
2powder accounts for 37.5wt%, wherein ZrO
2y containing 2wt% in powder
2o
3stablizer, this obtained Al
2o
3/ ZrO
2powdered material D50 particle diameter is less than 100 μm.
By Al
2o
3/ ZrO
2powdered material is processed into SLM ceramic block on SLM equipment, and every one deck all adopts same procedure first to carry out preheating, and then carries out cladding forming.
Below detailed research process:
Experimental system:
The structure of experimental system as shown in figure 15, comprises laser stereoforming equipment, induction heater and paving powder equipment, and paving powder equipment is arranged on induction heater.
Induction heater structural representation as shown in figure 14, comprises water cooled bottom plate 1(length 266mm), body of heater (height 165mm) on gland 5 and water cooled bottom plate 1, have refractory materials 4 in body of heater, body of heater periphery is wound with coil 2, coil 2 two ends tie cable joint 6.The height of induction heater is 225mm, and the internal diameter of burner hearth is 60mm, the in-built graphite 3 of burner hearth.
In test, applicant has made a kind of paving powder equipment, its structural representation as shown in figure 17, comprise base 7, the substrate 8 of band groove is placed with above base 7, be fixed with guide post 9 at stainless steel base 7 four angles, above the substrate 8 of band groove, be at least placed with the stainless steel plate 10 of a hollow by guide post 9.
The hollow position of stainless steel plate 10 is corresponding with the groove location of the substrate 8 of band groove.The thickness of stainless steel plate 10 is identical or different.
Paving powder equipment principle of work is: every a slice stainless steel plate 10 is placed in the top of band groove substrate 8, namely being equivalent to will band groove substrate 8(powder bed) corresponding have dropped one deck (floor height is determined by stainless steel plate thickness), the paving powder sintering of the hollow space of stainless steel plate can be realized the upwards shaping of powdered material.Because stainless steel plate is fixed on above the groove of substrate by guide post all the time before shaping end, therefore in the course of processing, there will not be caving in of powder bed, good supporting role is served to formed material.
In the present embodiment, laser stereoforming equipment adopts LSF III Type B laser stereoforming equipment, is provided by Northwestern Polytechnical University's state key solidification experiments room; During experiment, the laser apparatus in LSF III Type B laser stereoforming equipment is positioned at above paving powder equipment, under atmosphere protection condition, carry out cladding forming.
Induction heater adopts GYDY-XASR induction heater, and rated output 30KW, is purchased from the auspicious electric furnace company limited in Xi'an three.
Experiment material:
Pure Al
2o
3substrate (70mm × 50mm × 20mm), is purchased from Materials Co., Ltd of Wuhan Xintai City;
Al
2o
3/ ZrO
2powder (Al
2o
3account for 62.5wt%, ZrO
2account for 37.5wt%), wherein ZrO
2the interior Y containing 2wt%
2o
3stablizer, powder D50 is < 100 μm, and by Beijing, Rui Fazhiyuan Science and Technology Ltd. provides by the requirement of applicant.
Principle of design:
Al
2o
3and ZrO
2eutectic ratio be 58.5wt%:41.5wt%, but applicant studies discovery, at the Al mixed according to this ratio
2o
3/ ZrO
2mixed powder material inside organization structure after laser formation creates obvious thing phase segregation, has the zirconia grains of volume particle size to separate out, have impact on the homogeneity of thing Entropy density deviation.Reason may be in laser cladding process, Al
2o
3boiling point lower (3000 DEG C) and ZrO
2boiling point relatively high (4300 DEG C), part Al
2o
3break both eutectic ratios after steam raising, just defined the zirconia grains of volume particle size when both grow to aluminum oxide deficiency in eutectic ratio and form border with adjacent eutectic.Therefore the mixed powder that selective oxidation al proportion is greater than eutectic ratio can make up the loss of aluminum oxide in SLM moulding process, the Al that applicant finds in mixed powder through overtesting
2o
3: ZrO
2under the ratio condition of=62.5wt%:37.5wt%, compensate for Al in laser cladding process
2o
3loss, make the interior tissue thing Entropy density deviation uniformity of forming ceramic material.
Al
2o
3/ ZrO
2the fusing point of eutectic material is 1860 DEG C, research finds that the fast thawing rapid hardening process of laser melting coating can make the internal stress of stupalith excessive and cause the formation of crackle, and studies have found that and powder to be heated under fusing point about 200 DEG C before laser melting coating, significantly can be lowered into the thermal stresses of shaped material inside, thus the stupalith that molded surface and inner flawless generate, therefore have employed in the present embodiment and first carry out one-level preheating with induction heater, and then adopt laser to carry out the secondary preheating (temperature is lower than fusing point) of powder bed, the technological line of cladding forming is carried out again after reaching desirable preheating temperature.
To Al before experiment
2o
3substrate surface uses acetone clean dirt, by Al after first polishing with No. 200 sand paper
2o
3/ ZrO
2powder is laid on pure Al
2o
3on substrate, single berth powder thickness is 500 μm, and every one deck all adopts same procedure first to carry out preheating, and then carries out cladding forming.
By pure Al
2o
3substrate is placed in the surface of paving powder equipment, is warming up to about 1200 DEG C; Be 150W by laser power settings, spot diameter is 10mm, sweep velocity 4000mm/min, and warm up time is 1min, makes powder bed reach preheating temperature 1700 DEG C; Adjustment parameter, laser power is 200W, and spot diameter is 8mm sweep velocity is 10mm/min, carries out single track cladding forming; Re-start paving powder, paving powder thickness is 500 μm, is struck off on powder bed surface with scraper plate, and then above-mentioned steps order carries out the shaping of new one deck again.Repeatedly spread powder, after shaping, namely form SLM ceramic block material (photo of shaping SLM ceramic block material is see Figure 16).
Applicant, in research process, first have studied the microtexture of ceramic material powder for laser formation material and the impact of mechanical property of different grain size and pattern, and then optimizes the ceramic powder of applicable SLM processing.
Test method is: 4 groups of different grain sizes and pattern Al2O3/ZrO2 powder are divided into groups situation as table 1:
Table 1:Al
2o
3/ ZrO
2mixed powder grouping situation
| Powder divides into groups | D50 granularity | Pattern | Grinding mode |
| A | ＜1μm | Spherical | Atomization |
| B | ＜1μm | Irregular | Comminution by gas stream |
| C | ＜100μm | Ball-type | Atomization |
| D | ＜100μm | Sheet | Ball mill pulverizing |
Powder morphology and globule size is observed under scanning electron microscope:
By 4 groups of powder uniform spreading powder, carry out the scanning of individual layer laser melting coating, laser power 500W, sweep velocity 30 μm/s, spot diameter 5mm, thickness in monolayer 4mm, atmosphere is argon gas.Shaping SLM ceramic test piece is cut, embedding, polishing (80 order to 1200 order) and polishing, test specimen microtexture is observed under scanning electron microscope, energy spectrum analysis material is formed, and 6 points chosen by each test specimen, and test microhardness (HV) is to evaluate its mechanical property.
Experimental result: see the vickers hardness number of 4 groups of raw ceramic materials powder stereoscan photographs of Fig. 1 to Fig. 4 and 4 groups of powder compacting stupaliths of table 2 and Fig. 5.
Table 2: different powder grouping test specimen vickers hardness number (GPa)
Discussion of results: analyze from mechanical property, find that A, B group shows the hardness value low compared with C, D two groups, can say the low mechanical property of material, its reason may be because A, B two groups is nanoscale powder (< 1 μm), can produce agglomeration after paving powder makes powder distribution density differ, and the place that during laser melting coating, powder loosens relatively easily produces defect and pore.A, C two groups of powder are atomization ball-type powder but the microtexture of material and hardness aspect are all obviously distinguished with B, D group nothing of same particle sizes rank different-shape after shaping, can think under the condition of powder size indifference, the stuctures and properties of powder morphology to formed material has no significant effect.So we have selected the ceramic powder material that the larger powder of granularity is prepared as SLM.
Secondly, applicants studied Al
2o
3and ZrO
2the proportioning of mixed powder and the phase structure of formed material inside and the relation between distributing, acquisition can prepare Al
2o
3/ ZrO
2the proportioning raw materials of eutectic composite ceramics, and then the problem solving the inner thing phase segregation of formed material.Experimental technique: the Al choosing 3 kinds of different ratio
2o
3and ZrO
2mixed powder (wherein ZrO
2in containing 5wt%Y
2o
3), grouping situation is as shown in table 3, ZrO in the A group in mixed powder
2account for 37.5wt%, ZrO in B group
2account for 42.5wt%, ZrO in C group
2account for 47.5wt%.
Table 3:Al
2o
3/ ZrO
2powder mixture ratio grouping (wt%)
| ZrO 2 | Al 2O 3 | |
| A | 37.5 | 62.5 |
| B | 42.5 | 57.5 |
| C | 47.5 | 52.5 |
Laser cladding forming is carried out, by scanning electron microscopic observation forming ceramic material microstructure after Homogeneous phase mixing; Utilize the microhardness of microhardness instrument test material.3 groups of different ratio powdered molding material, 500 times of stereoscan photographs (transverse section) are see Fig. 6, Fig. 7 and Fig. 7.
B composing type material 1000 times of stereoscan photographs (longitudinal section) see Figure 10 see Fig. 9, B composing type material 5000 times of photos, are selected clear zone point 1 to carry out energy spectrum analysis, are obtained analytical results and see Figure 11 in Figure 10; 3 composing type material microhardness values are see table 4 and Fig. 1.
Table 4: different powder mixture ratio grouping test specimen vickers hardness number (GPa)
Discussion of results: the fibrous ZrO in stereoscan photograph in visible A group material
2crystal grain is at Al
2o
3be evenly distributed in matrix, and in B, C two groups, there is obvious polynuclear plane, from B group 1000 times of photos (Fig. 9), can find that this structure has separated out the ZrO2 crystal of volume particle size on border in 5000 times of (Figure 10) stereoscan photographs and EDAX results, the longitudinal section photo in conjunction with B group can find that this is a kind of column co-crystal structures (Figure 13) along scanning direction growth.
Research finds, can separate out the crystal of zirconium oxide of volume particle size, cause thing phase segregation under this conditions of mixture ratios.In A group, the ratio of aluminum oxide is greater than eutectic ratio, its thing Entropy density deviation then more uniformity, and without obvious thing phase segregation, surface and inside generate without obvious crackle, and mechanical property is better.And the ratio of aluminum oxide is more less than B group in C group, therefore also form the structure identical with B group.The difference demonstrated on three groups of materials microstructures is compared in hardness test, can think that the powder mixture ratio forming ceramic material of A group has more homogeneous thing Entropy density deviation and better mechanical property.Be expected to be used as all-ceramic crown, the materials application of bridge and inlay is in oral repairing clinic.
Claims (1)
1. an Al
2o
3/ ZrO
2powdered material is processed into the method for SLM ceramic block on SLM equipment, it is characterized in that:
Described Al
2o
3/ ZrO
2powdered material is by Al
2o
3powder and ZrO
2powder forms by mass percentage, Al
2o
3powder accounts for 62.5%, ZrO
2powder accounts for 37.5%, wherein, and ZrO
2containing the Y of 2% in powder
2o
3stablizer, this obtained Al
2o
3/ ZrO
2powdered material D50 particle diameter is less than 100 μm;
Working method is: by Al
2o
3/ ZrO
2powdered material is laid on pure Al
2o
3on substrate, single berth powder thickness is 500 μm, and every one deck all adopts same procedure first to carry out preheating, and then carries out cladding forming, and concrete working method is:
Described preheating, the concrete steps of cladding forming are as follows:
(1) paving powder equipment is placed on induction heater, is warming up to 1200 DEG C;
(2) be 150W by laser power settings, spot diameter is 10mm, sweep velocity 4000mm/min, and warm up time is 1min, makes the preheating temperature of powder bed be 1700 DEG C;
(3) after step (2) terminates, adjustment laser power is 200W, and spot diameter is 8mm sweep velocity is 10mm/min, carries out single track cladding forming;
(4) after step (3) terminates, carry out second time and spread powder, paving powder thickness is 500 μm, is struck off on powder bed surface with scraper plate, then again according to step (1), step (2) order carries out the single track cladding forming of new one deck; Through repeatedly spreading powder, after single track cladding forming, namely form SLM ceramic block material.
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|---|---|---|---|
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|---|---|---|---|
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| CN103771837B true CN103771837B (en) | 2015-05-13 |
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| DE102015205787A1 (en) * | 2015-03-31 | 2016-10-06 | Siemens Aktiengesellschaft | Method for producing a component from MAX phases |
| CN106187179B (en) * | 2016-07-14 | 2019-01-29 | 广东省材料与加工研究所 | One kind is wear-resistant to use ZrO2-Al2O3Complex phase ceramic particle and its preparation method and application |
| CN109761587B (en) * | 2019-03-07 | 2021-05-07 | 西北工业大学 | Preparation of Al2O3-GdAlO3-ZrO2Method for preparing ternary eutectic ceramics |
| CN110496965B (en) * | 2019-08-26 | 2022-01-11 | 江苏大学 | Method and device for preparing flexible additive gradient functional material |
| CN110981548A (en) * | 2019-12-27 | 2020-04-10 | 西北工业大学 | Laser repairing method for crack of C/C composite ultrahigh-temperature ceramic coating |
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| CN103193486A (en) * | 2013-03-18 | 2013-07-10 | 大连理工大学 | Method for laser engineered net shaping of Al2O3-ZrO2 eutectic ceramic structure |
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Non-Patent Citations (1)
| Title |
|---|
| Net Shaped High Performance Oxide Ceramic Parts by Selective Laser Melting;Hagedorn, Yves-Christian at al.;《Physics Procedia》;20101231;第5卷;说明书第3页第[0016]段 * |
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