阅读说明：本技术 一种3d打印高热导氮化硅陶瓷材料与制品 (3D printing high-thermal-conductivity silicon nitride ceramic material and product ) 是由 赵喆 姜焱林 于 2019-11-26 设计创作，主要内容包括：本发明公开了一种3D打印高热导氮化硅陶瓷材料,由包括以下重量份的原料制成：氮化硅陶瓷粉体100～120份、碳化硅纤维17～22份、乙氧化三羟甲基丙烷三丙烯酸酯35～44份、脂肪族聚氨酯二丙烯酸酯24～30份、四(3-巯基丙酸)季戊四醇酯9～12份、光引发剂0.18～0.24份、阻聚剂0.020～0.025份、分散剂4～6份、消泡剂3.5～4.5份。本发明的3D打印高热导氮化硅陶瓷材料的导热系数高,导热性能优异；拉伸强度高,断裂伸长率适中,力学性能等综合性能好。(The invention discloses a 3D printing high-thermal-conductivity silicon nitride ceramic material which is prepared from the following raw materials in parts by weight: 100-120 parts of silicon nitride ceramic powder, 17-22 parts of silicon carbide fiber, 35-44 parts of ethoxylated trimethylolpropane triacrylate, 24-30 parts of aliphatic polyurethane diacrylate, 9-12 parts of pentaerythritol tetrakis (3-mercaptopropionate), 0.18-0.24 part of photoinitiator, 0.020-0.025 part of polymerization inhibitor, 4-6 parts of dispersant and 3.5-4.5 parts of defoaming agent. The 3D printed high-thermal-conductivity silicon nitride ceramic material has high thermal conductivity and excellent thermal conductivity; high tensile strength, moderate elongation at break, good mechanical properties and other comprehensive properties.)

1. The 3D printing high-thermal-conductivity silicon nitride ceramic material is characterized by being prepared from the following raw materials in parts by weight:

100-120 parts of silicon nitride ceramic powder,

17-22 parts of silicon carbide fiber,

35-44 parts of ethoxylated trimethylolpropane triacrylate,

24-30 parts of aliphatic polyurethane diacrylate,

9-12 parts of pentaerythritol tetrakis (3-mercaptopropionate),

0.18 to 0.24 portion of photoinitiator,

0.020 to 0.025 portion of polymerization inhibitor,

4-6 parts of a dispersant,

3.5-4.5 parts of a defoaming agent.

2. The 3D printed high thermal conductivity silicon nitride ceramic material according to claim 1, wherein the 3D printed high thermal conductivity silicon nitride ceramic material is prepared from the following raw materials in parts by weight:

110 portions of silicon nitride ceramic powder,

19.5 parts of silicon carbide fiber,

39.5 portions of ethoxylated trimethylolpropane triacrylate,

27 parts of aliphatic polyurethane diacrylate,

Pentaerythritol tetrakis (3-mercaptopropionate) 10.5 parts,

0.21 part of photoinitiator,

0.023 portion of polymerization inhibitor,

5 portions of dispersant,

And 4 parts of a defoaming agent.

3. The 3D printing high thermal conductivity silicon nitride ceramic material according to claim 1, wherein the particle size of the silicon nitride ceramic powder is 0.4-0.6 μm.

4. The 3D printed high thermal conductivity silicon nitride ceramic material as claimed in claim 1, wherein the photoinitiator is Irgacure784 of Pasteur Chemicals Ltd.

5. The 3D printing high thermal conductivity silicon nitride ceramic material as claimed in claim 1, wherein the polymerization inhibitor is pyrogallol.

6. The 3D printing high thermal conductivity silicon nitride ceramic material as claimed in claim 1, wherein the dispersant is a mixture of ammonium polyacrylate and oleic acid.

7. The 3D printing high thermal conductivity silicon nitride ceramic material according to claim 6, wherein the mass ratio of ammonium polyacrylate and oleic acid in the mixture of ammonium polyacrylate and oleic acid is 1: 0.38 to 0.44.

8. The 3D printed high thermal conductivity silicon nitride ceramic material as claimed in claim 1, wherein the defoaming agent is polydimethylsiloxane.

9. The 3D printed high thermal conductivity silicon nitride ceramic product is characterized in that the 3D printed high thermal conductivity silicon nitride ceramic product is prepared by the 3D printed high thermal conductivity silicon nitride ceramic material according to any one of claims 1 to 8 through an SLA-3D printing process.

Technical Field

The invention relates to the technical field of 3D printing, in particular to a 3D printing high-thermal-conductivity silicon nitride ceramic material and a product.

Background

As one of the important development trends of the future ceramic 3D printing technology, the ceramic SLA (stereo Lithography application) 3D printing technology based on the stereolithography principle has the advantages of high forming quality, large size range of prepared parts, close compactness to an ideal value and the like.

According to the SLA forming technology, photosensitive resin is used as a raw material, laser is controlled through a computer, point-by-point scanning is carried out on the surface of the liquid photosensitive resin according to information of each layered section of a part gas-dimensional CAD model, and resin thin layers in a scanned area generate photopolymerization reaction and are homogenized to form one thin layer of a part. After 1 layer assimilation, the workbench moves downwards by a distance of 1 layer thickness, and then 1 layer of new liquid resin is coated on the surface of the original deceive-formed resin, and scanning and curing are carried out again. And continuously circulating in turn, and overlapping layer by layer until obtaining the blue-dimensional solid model.

The SLA-3D printing process can generally be divided into 3 steps:

1) processing layered data of the 3-dimensional model, namely processing the 3-dimensional model of the part into a text with a format which can be identified by printing equipment such as STL (standard template library) and the like through special software, and performing processing such as support addition, layering and the like;

2) uniformly paving the ceramic raw materials on a workbench of a printer, performing selective photocuring on ultraviolet laser according to part hierarchical data, and then continuously paving the raw materials and printing until the ceramic blank is formed;

3) and degreasing and sintering the ceramic blank to obtain the required ceramic part.

In the SLA-3D printing ceramic process, the components, viscosity and other attributes of the ceramic paste directly influence the accuracy of the implementation of the step 2), and finally influence the performance of the ceramic 3D printing part, and the ceramic paste occupies an important position in the whole 3D printing process.

However, the currently used 3D printing ceramic materials still have the following problems:

1. the product obtained by the 3D printing process is small in heat conductivity coefficient and poor in heat conductivity; low tensile strength, small elongation at break, poor comprehensive properties such as mechanical properties and the like;

2. the forming speed is limited, and the dimensional accuracy is low when a product with a complex shape is formed;

3. the quality of the product obtained by the 3D printing process is poor, and defective products are easy to appear.

Based on the situation, the invention provides a 3D printing high-thermal-conductivity silicon nitride ceramic material and a product, which can effectively solve the problems.

Disclosure of Invention

The invention aims to provide a 3D printing high-thermal-conductivity silicon nitride ceramic material and a product. According to the 3D printing high-thermal-conductivity silicon nitride ceramic material, the raw material composition of the 3D printing high-thermal-conductivity silicon nitride ceramic material is selected through the high-thermal-conductivity ceramic pot, the content of each raw material is optimized, silicon nitride ceramic powder, silicon carbide fiber, ethoxylated trimethylolpropane triacrylate, aliphatic polyurethane diacrylate, pentaerythritol tetrakis (3-mercaptopropionate), a photoinitiator, a polymerization inhibitor, a dispersing agent and a defoaming agent are selected according to a proper ratio, the quality stability of the product is improved, the occurrence of defective products is reduced, and the prepared 3D printing high-thermal-conductivity silicon nitride ceramic material for the high-thermal-conductivity ceramic pot is high in thermal conductivity and excellent in thermal conductivity; high tensile strength, moderate elongation at break, good mechanical properties and other comprehensive properties.

In order to solve the technical problems, the technical scheme provided by the invention is as follows:

the 3D printing high-thermal-conductivity silicon nitride ceramic material is prepared from the following raw materials in parts by weight:

100-120 parts of silicon nitride ceramic powder,

17-22 parts of silicon carbide fiber,

35-44 parts of ethoxylated trimethylolpropane triacrylate,

24-30 parts of aliphatic polyurethane diacrylate,

9-12 parts of pentaerythritol tetrakis (3-mercaptopropionate),

0.18 to 0.24 portion of photoinitiator,

0.020 to 0.025 portion of polymerization inhibitor,

4-6 parts of a dispersant,

3.5-4.5 parts of a defoaming agent.

According to the 3D printing high-thermal-conductivity silicon nitride ceramic material, the raw material composition of the 3D printing high-thermal-conductivity silicon nitride ceramic material is selected through the high-thermal-conductivity ceramic pot, the content of each raw material is optimized, silicon nitride ceramic powder, silicon carbide fiber, ethoxylated trimethylolpropane triacrylate, aliphatic polyurethane diacrylate, pentaerythritol tetrakis (3-mercaptopropionate), a photoinitiator, a polymerization inhibitor, a dispersing agent and a defoaming agent are selected according to a proper ratio, the quality stability of the product is improved, the occurrence of defective products is reduced, and the prepared 3D printing high-thermal-conductivity silicon nitride ceramic material for the high-thermal-conductivity ceramic pot is high in thermal conductivity and excellent in thermal conductivity; high tensile strength, moderate elongation at break, good mechanical properties and other comprehensive properties.

In the raw materials of the high-thermal-conductivity silicon nitride ceramic material for 3D printing of the high-thermal-conductivity ceramic pot, silicon nitride ceramic powder and silicon carbide fiber in proper proportion are selected and matched with each other to play a good synergistic effect, so that the high-thermal-conductivity silicon nitride ceramic material for 3D printing of the high-thermal-conductivity ceramic pot has the characteristics of high thermal conductivity, high strength, low density, high temperature resistance and the like;

according to the raw materials of the high-thermal-conductivity silicon nitride ceramic material for 3D printing of the high-thermal-conductivity ceramic pot, the ethoxylated trimethylolpropane triacrylate, the aliphatic polyurethane diacrylate and the tetra (3-mercaptopropionic acid) pentaerythritol ester are selected according to a proper proportion, wherein the ethoxylated trimethylolpropane triacrylate and the aliphatic polyurethane diacrylate are used as photocuring monomers or prepolymers, and the tetra (3-mercaptopropionic acid) pentaerythritol ester is used as a modifier, and are matched with each other to achieve a good synergistic effect, so that the mechanical properties such as tensile strength, elongation at break and the like of the high-thermal-conductivity silicon nitride ceramic material for 3D printing of the high-thermal-conductivity ceramic pot are greatly improved, the tensile strength is high, the elongation at break is moderate, and the mechanical properties are good.

In the raw materials of the high thermal conductivity silicon nitride ceramic material 3D printed by the high thermal conductivity ceramic pot, a dispersant (preferably, the dispersant is a mixture of ammonium polyacrylate and oleic acid, preferably, the mass ratio of the ammonium polyacrylate to the oleic acid in the mixture of the ammonium polyacrylate and the oleic acid is 1: 0.38-0.44.) is selected in a proper proportion, so that silicon nitride ceramic powder and silicon carbide fibers can be uniformly dispersed in a mixture of ethoxylated trimethylolpropane triacrylate, aliphatic polyurethane diacrylate and pentaerythritol tetrakis (3-mercaptopropionate) in the raw material system of the high thermal conductivity ceramic pot, the high thermal conductivity silicon nitride ceramic material 3D printed by the high thermal conductivity ceramic pot has uniform components, high dimensional accuracy and smooth surface, the high thermal conductivity silicon nitride ceramic material 3D printed by the high thermal conductivity ceramic pot has high thermal conductivity, the heat-conducting property is excellent; high tensile strength, moderate elongation at break and good mechanical property.

Preferably, the 3D printing high thermal conductivity silicon nitride ceramic material is prepared from the following raw materials in parts by weight:

110 portions of silicon nitride ceramic powder,

19.5 parts of silicon carbide fiber,

39.5 portions of ethoxylated trimethylolpropane triacrylate,

27 parts of aliphatic polyurethane diacrylate,

Pentaerythritol tetrakis (3-mercaptopropionate) 10.5 parts,

0.21 part of photoinitiator,

0.023 portion of polymerization inhibitor,

5 portions of dispersant,

And 4 parts of a defoaming agent.

Preferably, the particle size of the silicon nitride ceramic powder is 0.4-0.6 μm.

Preferably, the photoinitiator is Irgacure784 from basf chemicals, inc.

Preferably, the polymerization inhibitor is pyrogallol.

Preferably, the dispersant is a mixture of ammonium polyacrylate and oleic acid.

Preferably, the mass ratio of the ammonium polyacrylate to the oleic acid in the mixture of the ammonium polyacrylate and the oleic acid is 1: 0.38 to 0.44.

Preferably, the defoamer is polydimethylsiloxane.

The invention also provides a 3D printed high thermal conductivity silicon nitride ceramic product, which is prepared by adopting the 3D printed high thermal conductivity silicon nitride ceramic material through an SLA-3D printing process.

Compared with the prior art, the invention has the following advantages and beneficial effects:

according to the 3D printing high-thermal-conductivity silicon nitride ceramic material, the raw material composition of the 3D printing high-thermal-conductivity silicon nitride ceramic material is selected through the high-thermal-conductivity ceramic pot, the content of each raw material is optimized, silicon nitride ceramic powder, silicon carbide fiber, ethoxylated trimethylolpropane triacrylate, aliphatic polyurethane diacrylate, pentaerythritol tetrakis (3-mercaptopropionate), a photoinitiator, a polymerization inhibitor, a dispersing agent and a defoaming agent are selected according to a proper ratio, the quality stability of the product is improved, the occurrence of defective products is reduced, and the prepared 3D printing high-thermal-conductivity silicon nitride ceramic material for the high-thermal-conductivity ceramic pot is high in thermal conductivity and excellent in thermal conductivity; high tensile strength, moderate elongation at break, good mechanical properties and other comprehensive properties.

In the raw materials of the high-thermal-conductivity silicon nitride ceramic material for 3D printing of the high-thermal-conductivity ceramic pot, silicon nitride ceramic powder and silicon carbide fiber in proper proportion are selected and matched with each other to play a good synergistic effect, so that the high-thermal-conductivity silicon nitride ceramic material for 3D printing of the high-thermal-conductivity ceramic pot has the characteristics of high thermal conductivity, high strength, low density, high temperature resistance and the like;

according to the raw materials of the high-thermal-conductivity silicon nitride ceramic material for 3D printing of the high-thermal-conductivity ceramic pot, the ethoxylated trimethylolpropane triacrylate, the aliphatic polyurethane diacrylate and the tetra (3-mercaptopropionic acid) pentaerythritol ester are selected according to a proper proportion, wherein the ethoxylated trimethylolpropane triacrylate and the aliphatic polyurethane diacrylate are used as photocuring monomers or prepolymers, and the tetra (3-mercaptopropionic acid) pentaerythritol ester is used as a modifier, and are matched with each other to achieve a good synergistic effect, so that the mechanical properties such as tensile strength, elongation at break and the like of the high-thermal-conductivity silicon nitride ceramic material for 3D printing of the high-thermal-conductivity ceramic pot are greatly improved, the tensile strength is high, the elongation at break is moderate, and the mechanical properties are good.

In the raw materials of the high thermal conductivity silicon nitride ceramic material 3D printed by the high thermal conductivity ceramic pot, a dispersant (preferably, the dispersant is a mixture of ammonium polyacrylate and oleic acid, preferably, the mass ratio of the ammonium polyacrylate to the oleic acid in the mixture of the ammonium polyacrylate and the oleic acid is 1: 0.38-0.44.) is selected in a proper proportion, so that silicon nitride ceramic powder and silicon carbide fibers can be uniformly dispersed in a mixture of ethoxylated trimethylolpropane triacrylate, aliphatic polyurethane diacrylate and pentaerythritol tetrakis (3-mercaptopropionate) in the raw material system of the high thermal conductivity ceramic pot, the high thermal conductivity silicon nitride ceramic material 3D printed by the high thermal conductivity ceramic pot has uniform components, high dimensional accuracy and smooth surface, the high thermal conductivity silicon nitride ceramic material 3D printed by the high thermal conductivity ceramic pot has high thermal conductivity, the heat-conducting property is excellent; high tensile strength, moderate elongation at break and good mechanical property.

Detailed Description

In order that those skilled in the art will better understand the technical solutions of the present invention, the following description of the preferred embodiments of the present invention is provided in connection with specific examples, which should not be construed as limiting the present patent.

The test methods or test methods described in the following examples are conventional methods unless otherwise specified; the reagents and materials, unless otherwise indicated, are conventionally obtained commercially or prepared by conventional methods.