阅读说明：本技术 Dlp 3d打印技术制备zta陶瓷器件的方法 (The method that DLP 3D printing technique prepares ZTA ceramic component ) 是由 赵喆 孙颖 王操 于 2019-09-26 设计创作，主要内容包括：本发明公开了一种DLP 3D打印技术制备ZTA陶瓷器件的方法,其特征在于,将氧化锆粉体与氧化铝粉体混合,干燥后球磨,得到氧化锆/氧化铝混合粉体；在树脂中添加复合分散剂、复合引发剂,制得混合液；将氧化锆/氧化铝混合粉体加入到步骤S3得到的混合液中,使用行星球磨直至粉体完全分散,制得ZTA浆料；将ZTA浆料倒入DLP打印机料槽中,进行打印,得到ZTA坯体；将ZTA坯体进行烧结,制得ZTA陶瓷器件。本发明有效解决了ZTA陶瓷成型中的开裂和密度不均匀的问题,以及现有的ZTA陶瓷制备技术中材料结构不均匀,特别是微观结构不均匀的技术缺陷,同时实现了材料结构与功能协调设计。(The invention discloses a kind of methods that DLP 3D printing technique prepares ZTA ceramic component, which is characterized in that mixes Zirconium powder with alumina powder, ball milling after drying obtains zirconium oxide/aluminium oxide mixed powder；Composite dispersing agent, composite initiator are added in resin, and mixed liquor is made；Zirconium oxide/aluminium oxide mixed powder is added in the mixed liquor that step S3 is obtained, using planetary ball mill until powder is completely dispersed, ZTA slurry is made；ZTA slurry is poured into DLP printer hopper, is printed, ZTA green body is obtained；ZTA green body is sintered, ZTA ceramic component is made.The present invention solves the problems, such as that material structure is uneven in cracking and Density inhomogeneity and existing ZTA ceramics processing in the molding of ZTA ceramics, especially the non-uniform technological deficiency of microstructure, while realizing material structure and orthofunction design.)

1. a kind of method that DLP 3D printing technique prepares ZTA ceramic component, which comprises the following steps:

Step S1, Zirconium powder is mixed with alumina powder, ball milling after drying obtains zirconium oxide/aluminium oxide mixed powder；

Step S2, composite dispersing agent is added in resin, is mixed 5~10 minutes；

Step S3, continue to add composite initiator in resin, be mixed 10~15 minutes, mixed liquor is made；

Step S4, zirconium oxide/aluminium oxide mixed powder is added in the mixed liquor that step S3 is obtained, using planetary ball mill until Powder is completely dispersed, and ZTA slurry is made；

Step S5, ZTA slurry is poured into DLP printer hopper, is printed, obtain ZTA green body；

Step S6, ZTA green body is sintered, ZTA ceramic component is made.

2. the method that DLP 3D printing technique as described in claim 1 prepares ZTA ceramic component, which is characterized in that the step The mass ratio of Zirconium powder and alumina powder is 5:95~15:85 in rapid S1.

3. the method that DLP 3D printing technique as described in claim 1 prepares ZTA ceramic component, which is characterized in that the step After mixing Zirconium powder with alumina powder in rapid S1,2h is dried in 100 DEG C of baking ovens, then rolling ball milling is for 24 hours.

4. the method that DLP 3D printing technique as described in claim 1 prepares ZTA ceramic component, which is characterized in that the step Resin in rapid S2 is hydroxyethyl methacrylate, 1,6 hexanediyl esters, three kinds of trimethylolpropane trimethacrylate Combination.

5. the method that DLP 3D printing technique as described in claim 1 prepares ZTA ceramic component, which is characterized in that the step The combination that composite dispersing agent in rapid S2 is two kinds of BYK-180, BYK-106.

6. the method that DLP 3D printing technique as described in claim 1 prepares ZTA ceramic component, which is characterized in that the step Resin and zirconium oxide/aluminium oxide mixed powder volume ratio in rapid S2 are 45:55, the mass ratio with composite dispersing agent be (2: 8)~(8:2).

7. the method that DLP 3D printing technique as described in claim 1 prepares ZTA ceramic component, which is characterized in that the step Composite initiator is made of the diphenyl phosphine oxide and 1- hydroxycyclohexyl phenyl ketone that mass ratio is 1:1 in rapid S4；It is compound to draw The dosage for sending out agent is the 1% of resin quality.

8. the method that DLP 3D printing technique as described in claim 1 prepares ZTA ceramic component, which is characterized in that the step The rate of ball milling is 200~300rpm in rapid S4；The solid volume content of ZTA slurry obtained is greater than 55%.

9. the method that DLP 3D printing technique as described in claim 1 prepares ZTA ceramic component, which is characterized in that the step The scraper speed of DLP printer is 600~1500step/s in rapid S5, and optical source wavelength is 355~460nm.

10. the method that DLP 3D printing technique as described in claim 1 prepares ZTA ceramic component, which is characterized in that the step It is sintered to pressureless sintering in rapid S6, sintering temperature is 1600 DEG C, soaking time 2h.

Technical field

The present invention relates to a kind of methods that DLP 3D printing technique prepares ZTA ceramic component, belong to increases material manufacturing technology neck Domain.

Background technique

DLP 3D printing technique, i.e. digital light processing molding (Digital Light Processing, DLP), principle That slicing treatment is carried out to model using Slice Software, generate be able to reflect part section figure cut layer data, by this document Dynamic view generator is driven, the area source of feature wavelength irradiates dynamic view generator, after light path system, in photosensitive resin Surface forms specified part section view, can disposably realize the solidification of entire part layer.After this layer of part section generates, Workbench moves down a thickness, carries out the solidification of next part layer, so recycles, until printing terminates.

In traditional preparation process, the material of ZTA is equipped with, forming method, to preparing uniform doping, have certain knot There is very big challenge in the ZTA ceramic material of structure, while can aggravate the inhomogeneities on ZTA material microstructure.

Summary of the invention

The technical problems to be solved by the present invention are: cracking and Density inhomogeneity in existing ZTA ceramics forming process The problem of and existing ZTA ceramics processing in material structure it is uneven, especially the non-uniform technology of microstructure lack It falls into.

To solve the above-mentioned problems, the present invention provides a kind of method that DLP 3D printing technique prepares ZTA ceramic component, Characterized by comprising the following steps:

Step S1, Zirconium powder is mixed, ball milling after drying with alumina powder, obtains zirconium oxide/aluminium oxide mixing Powder；

Step S2, composite dispersing agent is added in resin, is mixed 5~10 minutes；

Step S3, continue to add composite initiator in resin, be mixed 10~15 minutes, mixed liquor is made；

Step S4, zirconium oxide/aluminium oxide mixed powder is added in the mixed liquor that step S3 is obtained, uses planetary ball mill Until powder is completely dispersed, ZTA slurry is made；

Step S5, ZTA slurry is poured into DLP printer hopper, is printed, obtain ZTA green body；

Step S6, ZTA green body is sintered, ZTA ceramic component is made.

Preferably, the mass ratio of Zirconium powder and alumina powder is 5:95~15:85 in the step S1.

Preferably, dry in 100 DEG C of baking ovens after mixing Zirconium powder with alumina powder in the step S1 2h, then rolling ball milling is for 24 hours.

Preferably, the resin in the step S2 is hydroxyethyl methacrylate (HEMA), 1,6 hexanediyl esters (HDDA), the combination of three kinds of trimethylolpropane trimethacrylate (TMPTA).

Preferably, the combination that the composite dispersing agent in the step S2 is two kinds of BYK-180, BYK-106.Dispersing agent can have Effect prevents ceramic powder from settling, and reunites, realizes the high stability of slurry.The ZTA ceramic slurry of good dispersion, in print procedure Self-leveling ability is stronger, it is easier to form, and be able to maintain the stability and service life of longer time.Composite dispersing agent can obtain Solid concentration can be promoted to dispersed preferable slurry and further, monodisperse agent can only obtain the slurry of flowing, or obtain The slurry solid concentration arrived is lower.The dispersing uniformity of zirconium oxide, alumina powder in resin can be improved in composite dispersing agent, Be conducive to the uniformity of printing shaping, the density of sintering and performance.

Preferably, the resin in the step S2 and zirconium oxide/aluminium oxide mixed powder volume ratio are 45:55, and multiple The mass ratio for closing dispersing agent is (2:8)~(8:2).

Preferably, composite initiator is 1:1 by mass ratio in the step S4 diphenyl phosphine oxide and 1- hydroxy cyclohexylphenyl Base phenyl ketone composition；The dosage of composite initiator is the 1% of resin quality.

Preferably, the rate of ball milling is 200~300rpm in the step S4, and control stirring rate is 200~300rpm, It avoids causing slurry temperature to increase because stirring rate is too fast, influences the performance of ZTA slurry, to influence printing effect and finished product Rate；The solid volume content of ZTA slurry obtained is greater than 55%, and viscosity is low, in order to DLP printing shaping and preparation high density Finished product, solid concentration is higher, and the consistency of the ZTA ceramics of preparation is higher.

Preferably, the scraper speed of DLP printer is 600~1500step/s, optical source wavelength 355 in the step S5 ~460nm.

Preferably, it is sintered to pressureless sintering in the step S6, sintering temperature is 1600 DEG C, soaking time 2h.

The present invention mixes ceramic powders with dispersing agent and photoinitiator in a solvent, forms the ceramic suspension of stable homogeneous Slurry；Again by DLP 3D printer according to selected slice model by slurry from the layer-by-layer photocuring of hopper on printing substrate, beat Print terminates, and can be formed with some strength and flexible green compact；Finished product is obtained finally by degreasing sintered；It is characterized in that: Aluminium oxide and zirconia ceramics powder premixing ball milling are increased into powder dispersing uniformity；By hybrid ceramic powder and dispersing agent and Photoinitiator solvent mixing in improve ceramic powder solid concentration, reduce solvent content, still can get be uniformly dispersed, viscosity Ceramic slurry low, the holding time is long；It can print ZTA ceramic structure with complex shape and the print time be short, after being not present Phase working process.

The present invention is based on the characteristics of DLP printed material, by selecting suitable aluminium oxide, Zirconium powder mixed proportion, The type and ratio of resin, dispersing agent and initiator have prepared the ZTA ceramic slurry of low viscosity, high solid loading, Neng Goutong Cross the ZTA ceramic component of DLP 3D printing complexity, and can obtain high-precision, high-compactness, strong mechanical performance finished device, have Effect solves the problems, such as material in cracking and Density inhomogeneity and existing ZTA ceramics processing in the molding of ZTA ceramics Structure is uneven, especially the non-uniform technological deficiency of microstructure, while realizing material structure and orthofunction design, control The technical problem of " property " and complicated shape increasing material manufacturing control " shape " perfect combination.

Specific embodiment

In order to make the present invention more obvious and understandable, it is hereby described in detail below with preferred embodiment.