CN-117658657-B - Photo-curing 3D printing fiber reinforced ceramic matrix composite slurry and preparation method thereof

CN117658657BCN 117658657 BCN117658657 BCN 117658657BCN-117658657-B

Abstract

The invention provides a photo-curing 3D printing fiber reinforced ceramic matrix composite slurry and a preparation method thereof. The invention provides a photocuring 3D printing fiber reinforced ceramic matrix composite slurry and a preparation method thereof, and the problems of low curing thickness, long molding time and the like of non-oxide ceramic powder with high light absorption value in the photocuring molding printing process can be solved by introducing ceramic precursor powder with lower absorbance into the slurry. The invention can improve the solidification thickness of the sizing agent and shorten the forming time, thereby effectively improving the printing forming efficiency.

Inventors

LI SHAN
JIN BAOJIE
ZHENG XINQI
WANG GONG
LIU BINGSHAN

Assignees

中国科学院空间应用工程与技术中心

Dates

Publication Date: 20260512
Application Date: 20231205

Claims (1)

1. The preparation method of the photo-curing 3D printing fiber reinforced ceramic matrix composite slurry is characterized in that the photo-curing 3D printing fiber reinforced ceramic matrix composite slurry comprises polycarbosilane powder, chopped carbon fibers, acrylate monomers, prepolymer, plasticizer, photoinitiator and high-molecular dispersing agent, and the preparation process of the photo-curing 3D printing fiber reinforced ceramic matrix composite slurry comprises the following steps: Preparing polycarbosilane powder, namely thermally curing liquid polycarbosilane for 4 hours at 150 ℃, then ball-milling the liquid polycarbosilane at the speed of 300r/min for 4 hours, and obtaining the polycarbosilane powder with the particle size of 1-10 mu m after ball-milling; The preparation of the photosensitive resin mixture comprises the steps of sequentially adding ethoxy trimethylolpropane triacrylate TMPEO 3 TA, polyurethane acrylate PUA, polyethylene glycol PGE-200 and phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide BAPO into a material tank according to a certain mass ratio, placing the materials on a magnetic stirrer, uniformly mixing the materials for 1h at a speed of 800 r/min to prepare a uniformly mixed photosensitive resin mixture, wherein the mass ratio of PUA to TMPEO TA is 0.143:1, the mass ratio of PEG-200 to PUA+ TMPEO 3 TA is 0.25:1, and the BAPO accounts for 3% of the total mass of TMPEO 3 TA, PUA and PEG-200; The preparation of the fiber reinforced ceramic matrix composite slurry comprises the steps of mixing a photosensitive resin mixture, polycarbosilane powder and a high molecular dispersing agent, stirring for 1min at a speed of 1500r/min in a homogenizer, adding chopped carbon fibers, stirring for 2min at a speed of 1500r/min again, and finally obtaining the uniformly mixed fiber reinforced ceramic matrix composite slurry, wherein the volume content of the photosensitive resin mixture is 63.99%, the volume content of the polycarbosilane powder is 11%, the volume content of the chopped carbon fibers is 25%, the volume content of the dispersing agent is 4200 high molecular dispersing agent is 0.01%, the printing parameters are exposure power of 30.50 mw/cm 2 , exposure time is 10 s, and the printing layer thickness is 50 mu m.

Description

Photo-curing 3D printing fiber reinforced ceramic matrix composite slurry and preparation method thereof Technical Field The invention belongs to the technical field of 3D printing, and particularly relates to a photo-curing 3D printing fiber reinforced ceramic matrix composite slurry and a preparation method thereof. Background When the fiber reinforced ceramic matrix composite is printed by photocuring 3D, the ceramic powder and the reinforcement fiber are mainly mixed for preparing the slurry, and the method has the following problems that the non-oxide ceramic powder with high light absorption value such as silicon carbide, silicon nitride and the like has higher absorption and scattering to ultraviolet light, so that the slurry is difficult to solidify in the photocuring forming printing process, and has the problems of low solidifying thickness, long forming time and the like. Disclosure of Invention Aiming at the defects existing in the prior art, the invention provides a photocuring 3D printing fiber reinforced ceramic matrix composite slurry and a preparation method thereof, which can effectively solve the problems. The technical scheme adopted by the invention is as follows: The invention provides a photo-curing 3D printing fiber reinforced ceramic matrix composite slurry which comprises ceramic precursor powder, reinforcement fibers, a photosensitive resin mixture and a high-molecular dispersing agent. The volume ratio of each component is preferably 11-31 parts of the ceramic precursor powder, 5-25 parts of the reinforcing body fiber, 44-74 parts of the photosensitive resin mixture and 0.01-0.03 part of the polymer dispersing agent. Preferably, the ceramic powder comprises 0-30 parts by volume of ceramic powder, wherein the ceramic powder is silicon carbide powder, and the particle size of the ceramic powder is 4-40 mu m. Preferably, the ceramic precursor powder is any one of polycarbosilane, polysiloxane and polysilazane, and the particle size of the ceramic precursor powder is 1-100 mu m. Preferably, the reinforcement fiber is any one or a mixture of a plurality of chopped carbon fibers and silicon carbide fibers, and the length of the reinforcement fiber is 50-500 mu m. Preferably, the photosensitive resin mixture is a mixture of acrylate monomers, prepolymers, plasticizers and photoinitiators. Preferably, the acrylic ester monomer is a mixture of a plurality of acrylic ester monomers, the prepolymer is one or a mixture of a polyurethane acrylic ester prepolymer and a polyester acrylic ester prepolymer, the plasticizer is polyethylene glycol, and the photoinitiator is phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide. Preferably, the polymer dispersant is one or a mixture of more than one of SP710 polymer dispersant, BYK111 polymer dispersant, KOS110 polymer dispersant, 4200 polymer dispersant and 20000 polymer dispersant. The invention also provides a preparation method of the photo-curing 3D printing fiber reinforced ceramic matrix composite slurry, which comprises the following steps: Step S1, preparing ceramic precursor powder: step S1.1, placing a formula amount of liquid ceramic precursor into an oven for heat curing treatment, wherein the heat curing temperature is 120-250 ℃, and the heat curing time is 2-4 hours; step S1.2, placing the ceramic precursor after the heat curing in the step S1.1 into a ball milling tank for ball milling treatment, wherein the ball milling rotation speed is 100-400 rpm, and the ball milling time is 2-6 hours, so as to obtain ceramic precursor coarse powder; s1.3, screening the ceramic precursor coarse powder by using a screen to obtain ceramic precursor powder with the required particle size; step S2, preparing fiber reinforced ceramic matrix composite slurry: And sequentially adding the ceramic precursor powder, the reinforcement fiber, the photosensitive resin mixture and the high molecular dispersing agent according to the formula amount into a material tank, and stirring by using a homogenizing mixer to obtain the fiber reinforced ceramic matrix composite slurry which is uniformly mixed. The photo-curing 3D printing fiber reinforced ceramic matrix composite slurry and the preparation method thereof provided by the invention have the following advantages: The invention provides a photocuring 3D printing fiber reinforced ceramic matrix composite slurry and a preparation method thereof, and the problems of low curing thickness, long molding time and the like of non-oxide ceramic powder with high light absorption value in the photocuring molding printing process can be solved by introducing ceramic precursor powder with lower absorbance into the slurry. The invention can improve the solidification thickness of the sizing agent and shorten the forming time, thereby effectively improving the printing forming efficiency. Drawings FIG. 1 is a schematic flow chart of a preparation method of a photo-curing 3D printing fiber reinforced ceramic matrix composit