阅读说明：本技术 一种3d打印陶瓷制备方法及其产品 (Preparation method of 3D printing ceramic and product thereof ) 是由 段帅帅 罗丽荣 田晓聪 靳洪允 侯书恩 于 2020-06-09 设计创作，主要内容包括：本发明公开了一种3D打印陶瓷制备方法及其产品。本发明的一种3D打印陶瓷制备方法,包括如下步骤：S1：将陶瓷粉末加入到粘结剂和有机溶剂的混合溶液中搅拌均匀得浆料；S2：采用微流挤出成形设备将浆料挤出成型,得到陶瓷坯体,将打印出的陶瓷坯体立即浸入到无机溶液中快速成型,所述有机溶剂与所述无机溶液互溶；S3：待陶瓷坯体固化变硬后取出干燥；S4：去除粘结剂；S5：高温煅烧得到陶瓷。本发明提供的陶瓷浆料具有良好的流动性和稳定性,具有适当的固相含量,打印出的浆料具有优良的形状保持能力,煅烧制得的陶瓷坯体多孔且不易开裂；通过有机溶剂和陶瓷粉末的比例调控孔隙率大小,实现多级孔结构,可制备复杂几何形状的陶瓷零件。(The invention discloses a preparation method of 3D printing ceramic and a product thereof. The invention discloses a preparation method of 3D printing ceramic, which comprises the following steps: s1: adding ceramic powder into a mixed solution of a binder and an organic solvent, and uniformly stirring to obtain slurry; s2: extruding and molding the slurry by adopting microflow extrusion molding equipment to obtain a ceramic blank, immediately immersing the printed ceramic blank into an inorganic solution for rapid molding, wherein the organic solvent and the inorganic solution are mutually soluble; s3: taking out and drying the ceramic blank after the ceramic blank is cured and hardened; s4: removing the binder; s5: and (4) calcining at high temperature to obtain the ceramic. The ceramic slurry provided by the invention has good fluidity and stability, has proper solid content, has excellent shape retention capacity, and is porous and not easy to crack; the porosity is regulated and controlled by the proportion of the organic solvent and the ceramic powder, a hierarchical pore structure is realized, and ceramic parts with complex geometric shapes can be prepared.)

1. A preparation method of 3D printing ceramic is characterized by comprising the following steps: the method comprises the following steps:

s1: adding ceramic powder into a mixed solution of a binder and an organic solvent, and uniformly stirring to obtain slurry;

s2: extruding and molding the slurry by adopting microflow extrusion molding equipment to obtain a ceramic blank, immediately immersing the printed ceramic blank into an inorganic solution for rapid molding, wherein the organic solvent and the inorganic solution are mutually soluble;

s3: taking out and drying the ceramic blank after the ceramic blank is cured and hardened;

s4: preserving the heat of the dried ceramic blank at 500-600 ℃ for 3h to remove the binder;

s5: and (4) calcining the ceramic body obtained in the step S4 at a high temperature to obtain the ceramic product.

2. The method for preparing 3D printed ceramics according to claim 1, wherein: in the step S5, the calcination temperature is 1100-1500 ℃, the temperature rise rate is 5-20 ℃/min, and the time is 2.5-6 h.

3. A method of preparing a 3D printed ceramic as claimed in claim 1 or 2, wherein: the mass ratio of the binder to the organic solvent to the ceramic powder is 2.8-4.2: 1: 1.

4. A method of preparing a 3D printed ceramic as claimed in claim 1 or 2, wherein: the binder comprises polyether sulfone and/or polyvinyl alcohol.

5. The method for preparing 3D printing ceramic according to claim 4, wherein the method comprises the following steps: the organic solvent comprises one or more of N-methyl-2-pyrrolidone, dimethylformamide and dimethyl sulfoxide.

6. The method for preparing 3D printing ceramic according to claim 5, wherein the method comprises the following steps: the inorganic solution includes deionized or distilled water.

7. The method for preparing 3D printing ceramic according to claim 4, wherein the method comprises the following steps: the ceramic powder comprises ZrO₂、Al₂O₃、TiO₂And SiC.

8. The method for preparing 3D printed ceramics according to claim 7, wherein: the particle size of the ceramic powder is in the nanometer or submicron level.

9. The method for preparing 3D printed ceramics according to claim 1, wherein: in the step S3, the drying temperature is 75-85 ℃, and the drying time is 12-14 h.

10. A ceramic prepared by a method of preparing a 3D printed ceramic as claimed in any one of claims 1 to 9.

Technical Field

The invention relates to the technical field of ceramic 3D printing, in particular to a preparation method of 3D printing ceramic and a product thereof.

Background

As a traditional inorganic non-metallic material, the ceramic has excellent properties of high strength, corrosion resistance, wear resistance, high temperature resistance and the like, and is widely concerned and applied in various industries such as biological medicine, electronics, aerospace and the like.

Additive Manufacturing (AM), commonly known as 3D printing, is a new and advanced material forming technology which is popular at present, and numerous domestic and foreign research institutions and enterprises participate in research, development and innovation of the technology. The ceramic 3D printing technology is used as a combination of the ceramic material and the 3D printing technology, so that the ceramic product with a complex shape can be manufactured, and the ceramic product has the advantages of high forming speed, low cost, high forming precision and the like. In view of the current situation of ceramic 3D printing, the development of the current ceramic 3D printing technology is not mature enough, and many problems to be solved, such as how to prepare ceramic slurry with good viscosity, low fluidity and uniform mixing, exist. In the sintering process, the blank is easy to generate the defects of cracks, deformation, different shrinkage rates in all directions and the like, and the sintering difficulty is increased.

Disclosure of Invention

The invention aims to provide a preparation method of a 3D printing ceramic and a product thereof, aiming at the defects in the prior art.

The invention discloses a preparation method of 3D printing ceramic, which comprises the following steps:

s1: adding ceramic powder into a mixed solution of a binder and an organic solvent, and uniformly stirring to obtain slurry;

s2: extruding and molding the slurry by adopting microflow extrusion molding equipment to obtain a ceramic blank, immediately immersing the printed ceramic blank into an inorganic solution for rapid molding, wherein the organic solvent and the inorganic solution are mutually soluble;

s3: taking out and drying the ceramic blank after the ceramic blank is cured and hardened;

s4: preserving the heat of the dried ceramic blank at 500-600 ℃ for 3h to remove the binder;

s5: and (4) calcining the ceramic body obtained in the step S4 at a high temperature to obtain the ceramic product.

Further, in the step S5, the calcination temperature is 1100-1500 ℃, the temperature rise rate is 5-20 ℃/min, and the time is 2.5-6 h.

Further, the mass ratio of the binder to the organic solvent to the ceramic powder is 2.8-4.2: 1: 1.

Further, the binder comprises polyether sulfone and/or polyvinyl alcohol.

Further, the organic solvent comprises one or more of N-methyl-2-pyrrolidone, dimethylformamide or dimethyl sulfoxide.

Further, the inorganic solution includes deionized water or distilled water.

Further, the ceramic powder includes ZrO₂、Al₂O₃、TiO₂And SiC.

Further, the particle size of the ceramic powder is in the nanometer or submicron level.

Further, the drying temperature in the step S3 is 75-85 ℃, and the drying time is 12-14 h.

A ceramic prepared by the method.

The ceramic slurry provided by the invention has good fluidity and stability, has proper solid content, has excellent shape retention capacity, and is porous and not easy to crack; the method has the advantages of one-step molding, controllable shape, simple process, low cost and high molding precision, the porosity is regulated and controlled by the proportion of the organic solvent and the ceramic powder, the hierarchical pore structure is realized, the higher the mass ratio of the organic solvent to the ceramic powder is, the higher the porosity is, the hierarchical pore structure is realized, the organic solvent and the inorganic solution in the ceramic blank are mutually dissolved and separated, and meanwhile, the polymer binder in the ceramic blank forms macromolecular gel, so that the rapid curing molding of the ceramic blank is realized, the calcining condition is controlled, the ceramic strength value is increased, the porosity of the prepared ceramic is more than 10 percent, the strength is more than 1500MPa, and the ceramic part with complex geometric shape can be prepared.

Drawings

Fig. 1 is a flow chart of a 3D printing ceramic preparation method of the present invention.

Detailed Description

The following are specific embodiments of the present invention and are further described with reference to the drawings, but the present invention is not limited to these embodiments.