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3D printed prepared silicon carbide ceramic and ceramic lining pipeline using same

A silicon carbide ceramic, 3D printing technology, applied in the field of 3D printing ceramics, can solve the problems of different compositions and properties, difficult to ensure the yield, high linear shrinkage, achieve good high temperature stability and high temperature wear resistance, reduce equipment Replacement cycle, the effect of low linear shrinkage

Inactive Publication Date: 2019-01-22
宁波设会物联网科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The solid 3D printing ceramic raw material is a mixture of ceramic powder and a certain binder. The principle is that the binder coats or bonds the ceramic powder during the pyrolysis process to form a ceramic with a certain strength. The binder and the binder are two different species, and their composition and properties are different, so it is difficult to form a ceramic with a uniform composition.
Liquid 3D printing ceramic raw materials can be divided into two types: ceramic slurry and solution blend. When the 3D printing ceramic raw material is slurry, in order to ensure the stability and uniformity of the slurry, it is necessary to add stabilizers, etc. The addition of stabilizers will cause ceramic pores. , which is detrimental to the performance of ceramics
When the 3D printing ceramic raw material is a liquid blend, its density is not higher than 0.5g / cm 3 , the density of silicon carbide ceramics is 2.4~3.2g / cm 3 , if you want to prepare dense silicon carbide ceramics from liquid raw materials, the linear shrinkage rate is high, and it is difficult to guarantee the yield
So far, the application of heat-curable cross-linked polycarbosilane has yet to be developed, and the application of 3D printing silicon carbide ceramic technology has not been reported.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] A preparation process of silicon carbide ceramics prepared by 3D printing is as follows:

[0040] Step 1: Preparation of heat-curable cross-linked polycarbosilane: dissolve polycarbosilane (commercially available, molecular weight 2800, softening point 300° C.) in xylene and tetravinylsilane (commercially available) in a mass ratio of 1: 1. Place in an autoclave, add platinum catalyst, vacuumize to replace high-purity nitrogen, and increase the pressure to 12.5MPa; then heat up to 110°C for 30 hours under the protection of high-purity nitrogen; cool, and distill under reduced pressure to obtain the solid product PVCS .

[0041] After characterization, the molecular weight of heat-curable cross-linked polycarbosilane is 3150. PVCS can be completely cross-linked and cured when it is treated at 400°C in a nitrogen atmosphere, and the gel content reaches 100%. During the pyrolysis process at ~1200°C, no foaming and flow will occur when turning to silicon carbide ceramics, ...

Embodiment 2

[0046] A preparation process of silicon carbide ceramics prepared by 3D printing is as follows:

[0047] Step 1: Preparation of heat-curable cross-linked polycarbosilane, refer to (Gu Xishuang, Song Yongcai. Synthesis and properties of heat-curable cross-linked polycarbosilane [J]. Silicone Materials, 2015, 29(6): 462-468 .): Dissolve polycarbosilane (commercially available, molecular weight 1500, softening point 200°C) in xylene and tetrapropenylsilane (commercially available) at a mass ratio of 1:1, place in an autoclave, add platinum catalyst, Vacuumize to replace high-purity nitrogen, increase the pressure to 12.5 MPa; then heat up to 110°C under the protection of high-purity nitrogen to react for 30 hours; cool, and distill under reduced pressure to obtain the solid product PVCS. After characterization, the molecular weight of heat-curable cross-linked polycarbosilane is 1726. It can be completely cross-linked and cured when it is treated at 400°C in a nitrogen atmosphere...

Embodiment 3

[0052] A preparation process of silicon carbide ceramics prepared by 3D printing is as follows:

[0053] Step 1: The preparation of thermally curable cross-linked polycarbosilane is the same as in Example 1.

[0054] Step 2: Prepare a solution of the heat-curable cross-linked polycarbosilane and cyclohexane prepared in step 1 according to the mass ratio of 6:4, add the prepared solution into the 3D printer, heat the solution to 70°C, and keep it warm for 10 minutes. Spray the hot solution from the nozzle onto the carrier at 70°C. The nozzle is 0.8mm away from the carrier. With the volatilization of the solvent, a layer of solid heat-curable cross-linked polycarbosilane is formed on the carrier. Then, the newly formed solid polycarbosilane Spray hot solvent on top to form a new layer of solid heat-curable cross-linked polycarbosilane, repeat spraying hot solvent, accumulate solid heat-curable cross-linked polycarbosilane layer by layer, and form a silicon carbide ceramic prefab...

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Abstract

The invention discloses a 3D printed prepared silicon carbide ceramic and a ceramic lining using the same. The 3D printed prepared silicon carbide ceramic is prepared by the steps: dissolving a heat curable crosslinked polycarbosilane into a solution, adding into a 3D printer, heating the solution to the temperature of 70 DEG C to 135 DEG C, carrying out heat preservation for a period of time, andthen spraying to a carrier with the temperature of 70 DEG C to 135 DEG C from a nozzle; along with evaporation of a solvent, forming a layer of solid heat curable crosslinked polycarbosilane, then taking the solid heat curable crosslinked polycarbosilane as a new carrier, carrying out next spraying, spraying repeatedly, and accumulating the solid heat curable crosslinked polycarbosilane layer bylayer to form a preform; then putting the preform into a heat treatment device, and successively carrying out solvent removal and crosslinking curing treatment of the heat curable crosslinked polycarbosilane successively; and then putting into a pyrolysis furnace, in an argon atmosphere, carrying out pyrolysis at the temperature of 1110 DEG C, and finally obtaining the 3D printed silicon carbide ceramic. The prepared silicon carbide ceramic has the characteristics of single raw materials, high product purity, high strength, corrosion resistance, high temperature resistance, good heat conductivity and impact resistance and the like; as the ceramic lining, the silicon carbide ceramic has high practical application value and has a promotion effect on the application of the 3D printed siliconcarbide ceramic and heat curable crosslinked polycarbosilane.

Description

technical field [0001] The invention belongs to the technical field of 3D printing ceramics, and in particular relates to a silicon carbide ceramic prepared by 3D printing. Background technique [0002] The methods currently used to prepare rapid prototyping of silicon carbide ceramics are: layered solid manufacturing (abbreviated as LOM); fused deposition modeling (abbreviated as FDM); shape deposition modeling (abbreviated as SDM); stereolithography (abbreviated as SLA); selective laser sintering ( SLS for short); inkjet printing method (IJM for short). Huang Xiaoting prepared a ceramic slurry with a certain solid content using camphene, silicon carbide, binder, and dispersant, and prepared a ceramic body by using 3D technology (see "Preparation and Performance Research of 3D Printed Silicon Carbide Ceramics", China Silicic Acid Special Ceramics Branch of Salt Society, Abstracts of the 19th National High-Tech Ceramics Academic Annual Conference, 2016: 1), in patent CN1084...

Claims

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Application Information

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IPC IPC(8): C04B35/565B33Y10/00B33Y70/00B33Y80/00
CPCB33Y10/00B33Y70/00B33Y80/00C04B35/571C04B35/573C04B2235/6562C04B2235/77C04B2235/9615
Inventor 顾福祥
Owner 宁波设会物联网科技有限公司