CN105669208A - Phenolic resin coated ceramic powder for laser 3D printing and preparation method thereof - Google Patents
Phenolic resin coated ceramic powder for laser 3D printing and preparation method thereof Download PDFInfo
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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Abstract
The invention provides a phenolic resin coated ceramic powder for laser 3D printing. The particle size of the ceramic powder is 10-50 mu m. The ceramic powder comprises 10-30 wt% of phenolic resin, 1-2.5 wt% of urotropine, 0.5-1.5 wt% of stearic acid and the balance of silane coupling agent surface-modified ceramic powder. The preparation method comprises the following steps: a) modifying the surface of the ceramic powder with anhydrous ethanol and a silane coupling agent; b) carrying out reaction on the surface-modified ceramic powder, phenolic resin, urotropine and stearic acid in a closed vessel to obtain an aggregate; and c) pulverizing the aggregate by ball milling, and screening. The ceramic powder is subjected to impurity removal and surface modification, thereby lowering the hydrophilicity, improving the wettability with the adhesive, and enhancing the efficiency of the adhesive and the strength of the initial mold blank. The phenolic resin has the advantages of higher absorptivity for laser and favorable adhesive effect, thereby being beneficial to enhancing the quality of the ceramic part. By using the urotropine as the curing agent and the stearic acid as the lubricant, the strength and plasticity of the SLS blank formed by the phenolic resin coated ceramic powder can be enhanced.
Description
Technical field
The present invention relates to laser 3D and print dusty material preparing technical field, be specifically related to a kind of for laser 3D coating phenolic resin ceramic powders printed and preparation method thereof.
Background technology
Ceramic material especially high-performance ceramic has high rigidity, high temperature resistant, high intensity, good insulating, the many advantages such as corrosion-resistant, is widely used in fields such as Aeronautics and Astronautics, automobile, electronics. But, ceramic material fragility is big, hardness is high, adopts conventional machine processing mode to shape and very easily produces defect, the ceramic part of labyrinth is difficult to more, and during by the shaped ceramic part such as slip casting, isostatic pressed, part shape is still by the restriction of mould, and manufacturing cycle length, cost are high.
Selective laser sintering technology (SelectiveLaserSintering, SLS) it is a kind of 3D printing-forming method shaping thought based on discrete dynamics models, the method breaches traditional material equal-volume and shapes the thinking model with Material removal, can pass through to three-dimensional CAD model along z-axis cut into slices synthetic time series two dimensional surface, then selectively to dusty material layering sintering, the prototype of stack shaping complicated shape or part layer by layer under the effect of laser. This not by the restriction of the complex-shaped degree of formation of parts, do not need the process technology of any moulds of industrial equipment to be considered as the following important channel solving a complicated ceramic member forming difficult problem.
SLS manufactures the method for part generally two kinds: one is Direct Laser fusion method, namely makes dusty material fusing shape by the heat effect of laser, it is adaptable to the metal material of macromolecular material and low melting point; Another is indirect laser sintered method, by melting the binding agent of low melting point, utilize binding agent form VISCOUS FLOW or melt the bonding realizing between powder, then obtain the functor with some strength again through the aftertreatment technology such as defat, sintering, it is adaptable to high-melting-point refractory material. The fusing point of pottery is higher, and very easily cracks under high power laser light direct irradiation, and the indirect laser sintered mode of low power laser generally can only be adopted to shape.
The performance of SLS composite ceramic powder powder material is closely connected with the kind of binding agent, content and incorporation way etc.The kind of binding agent has metal adhesive, inorganic binder and organic binder bond, and metal adhesive is mainly used to shaped ceramic/metallic composite part, and needs high-power laser instrument, and forming speed is slow, cost is high; Inorganic binder Heat stability is good, is difficult to slough in aftertreatment technology, increases production cost and manufacturing cycle; And the laser power of organic binder bond requirement is low, shape easily controllable, be suitable for SLS and manufacture ceramic member.
In order to improve the forming efficiency of binding agent, generally adopt method with plastic film, namely under certain process conditions, make ceramic powders as nucleus by tightly be coated on inside organic adhesive, formed polymer-coated ceramic powder composite powder. But, it is applicable at present the SLS film coated ceramic powder shaped and has that organic adhesive kind is few, preparation method is deficient, high in cost of production shortcoming.
Summary of the invention
It is an object of the invention to the defect overcoming prior art to exist, there is provided a kind of for laser 3D coating phenolic resin ceramic powders printed and preparation method thereof, the method utilizes the characteristics such as phenolic resin adhesive bonding force is high and ceramic powders interfacial adhesion is good, shaping shrinkage rate is little, has prepared the coating phenolic resin ceramic powders of excellent combination property.
Technical scheme is as follows:
A kind of for the laser 3D coating phenolic resin ceramic powders printed, it is made up of following raw material: ceramic powders, phenolic resin, hexamethylenamine, stearic acid, dehydrated alcohol and silane coupler.
Described coating phenolic resin ceramic powders particle diameter is 10-50 μm.
In described coating phenolic resin ceramic powders, phenolic resin accounts for 10-30wt%, hexamethylenamine accounts for 1-2.5wt%, stearic acid accounts for 0.5-1.5wt%, surplus is the ceramic powders through silane coupler surface modification, during surface modification, silane coupler consumption is the 1-1.5% of ceramic powders quality, and the mass ratio of dehydrated alcohol and silane coupler is 3-5:1.
Described ceramic powders is the one in carborundum, titanium carbide, zirconium carbide, aluminium oxide, zirconium oxide, and described silane coupler is one or more in vinyl silanes, amino silane, methacryloxypropyl silane.
By a kind of preparation method for the laser 3D coating phenolic resin ceramic powders printed described in such scheme, comprise the following steps:
A) ceramic powders of surface modification is prepared: a certain amount of ceramic powders is dry after weak acid, weak base and water clean respectively, dry ceramic powders is mixed homogeneously by a certain percentage with dehydrated alcohol, silane coupler and stirred and carries out surface treatment, surface treatment complete after by mixture vacuum drying, cross classifying screen and obtain the ceramic powders of surface modification;
B) coating phenolic resin pottery aggregation is prepared: join in the hermetic container filling organic solvent by a certain percentage by the ceramic powders of the step a) surface modification prepared and phenolic resin, pass into argon, the temperature of hermetic container is risen to 65-75 DEG C from room temperature, temperature-rise period adds a certain amount of hexamethylenamine and stearic acid and stirring makes it dissolve, intensification complete after held for some time, then naturally cool to room temperature and obtain coating phenolic resin pottery aggregation;
C) crushing and screening: the coating phenolic resin pottery aggregation prepared by step b) crosses classifying screen after taking out and dry, pulverize.
The described ceramic powders of step a) is the one in carborundum, titanium carbide, zirconium carbide, aluminium oxide, zirconium oxide, described weak acid is the one in dilute hydrochloric acid, dilute sulfuric acid, dust technology, described weak base is the one in dilute sodium hydroxide, dilute sodium carbonate, dilute sulfuric acid calcium, and described silane coupler is one or more in vinyl silanes, amino silane, methacryloxypropyl silane.
In step a), silane coupler consumption is the 1-1.5% of ceramic powders quality, and the mass ratio of dehydrated alcohol and silane coupler is 3-5:1.
The described organic solvent of step b) is the one in ethanol, carbon tetrachloride, oxolane, and hermetic container heating rate is 0.5-1 DEG C/min, and temperature retention time is 1-2h.
In step b), the weight proportion of each component is in end product coating phenolic resin ceramic powders, and phenolic resin is 10-30wt%, and hexamethylenamine is 1-2.5wt%, and stearic acid is 0.5-1.5wt%, and surplus is the ceramic powders of surface modification.
The powder that step a) and step c) all selects particle diameter to be 10-50 μm after crossing classifying screen.
Provided by the invention for the laser 3D coating phenolic resin ceramic powders preparation method printed, have the advantage that
1. pair ceramic powders has carried out the removal of impurity and surface modification treatment, reduces the hydrophilic of pottery, improves the wellability of itself and binding agent, improve binding agent efficiency and the intensity of initial parison.
2. adhesive phenolic resin is higher to the absorbance of laser, and bond effect is good, and the carbon skeleton formed after pyrolysis is conducive to the post processing of carbide ceramics, improves ceramic part quality.
3. the ethanol selected, carbon tetrachloride, the organic solvent such as oxolane, solute effect is good, and boiling point is low, volatile, eliminates the operation of decompression distillation, saves cost.
4. using hexamethylenamine as firming agent, stearic acid, as lubricant, can improve intensity and the plasticity of coating phenolic resin ceramic powders molding SLS base substrate.
Accompanying drawing explanation
Fig. 1 is coating phenolic resin ceramic powders preparation flow figure of the present invention;
Fig. 2 is coating phenolic resin ceramic powders of the present invention preparation and SLS forming principle schematic diagram.
Detailed description of the invention
For making those of ordinary skill in the art fully understand technical scheme and beneficial effect, absolutely prove further below in conjunction with drawings and the specific embodiments.
Embodiment 1
A kind of coating phenolic resin silicon carbide ceramics powder, including the phenolic resin of 20-30wt%, 1.5-2.5wt% hexamethylenamine, 1-1.5wt% stearic acid, surplus is the carborundum of surface modification. The preparation flow of this coating phenolic resin silicon carbide ceramics powder and principle as shown in Figure 1-2, specifically include following steps:
(1) prepare the silicon carbide ceramics powder of surface modification: take 1000g silicon carbide ceramics powder, respectively after dilute hydrochloric acid, dilute sodium hydroxide and water clean, put into vacuum drying oven and be dried. Then the mixed liquor of 30g dehydrated alcohol and 10g vinyl silanes is mixed homogeneously with aforementioned silicon carbide ceramics powder, use agitating device to be sufficiently stirred for mixture simultaneously and carry out surface modification treatment. After having reacted, mixture vacuum drying, sub-sieve are obtained the silicon carbide ceramics powder of surface modification that particle diameter is 10 microns.
(2) coating phenolic resin silicon carbide ceramics aggregation is prepared: join in the hermetic container filling ethanol by the silicon carbide ceramics powder of surface modification, phenolic resin, pass into argon shield. Make the temperature in hermetic container rise to 65-75 DEG C from room temperature with the speed of 0.5-1 DEG C/min, the process of intensification adds hexamethylenamine and stearic acid, and stirs with agitating device so that it is be completely dissolved. The addition of each material is as previously mentioned. Intensification is incubated 1-2h after completing under argon atmosphere, naturally cools to room temperature subsequently, obtains coating phenolic resin silicon carbide ceramics aggregation. The solvent of volatilization is recycled again.
(3) pulverize and sieve: the coating phenolic resin silicon carbide ceramics aggregation prepared is taken out from hermetic container, put in vacuum drying oven and be dried, then by its ball mill pulverizing, screening, the coating phenolic resin silicon carbide ceramics powder that particle diameter is 10 microns is obtained.
Embodiment 2
A kind of coating phenolic resin titanium carbide ceramic powder, including the phenolic resin of 15-25wt%, 1-2wt% hexamethylenamine, 0.5-1wt% stearic acid, surplus is the titanium carbide of surface modification. The preparation method of this coating phenolic resin titanium carbide ceramic powder is as follows:
(1) prepare the titanium carbide ceramic powder of surface modification: take 1000g titanium carbide ceramic powder, respectively after dilute sulfuric acid, dilute sodium carbonate and water clean, put into vacuum drying oven and be dried. Then the mixed liquor of 60g dehydrated alcohol and 15g amino silane is mixed homogeneously with aforementioned titanium carbide ceramic powder, use agitating device to be sufficiently stirred for mixture simultaneously and carry out surface modification treatment. After having reacted, mixture vacuum drying, sub-sieve are obtained the titanium carbide ceramic powder of the surface modification that particle diameter is 30 microns.
(2) coating phenolic resin titanium carbide ceramic aggregation is prepared: join in the hermetic container filling carbon tetrachloride by the titanium carbide ceramic powder of surface modification, phenolic resin, pass into argon shield. Make the temperature in hermetic container rise to 65-75 DEG C from room temperature with the speed of 0.5-1 DEG C/min, the process of intensification adds hexamethylenamine and stearic acid, and stirs with agitating device so that it is be completely dissolved. The addition of each material is as previously mentioned. Intensification is incubated 1-2h after completing under argon atmosphere, naturally cools to room temperature subsequently, obtains coating phenolic resin titanium carbide ceramic aggregation. The solvent of volatilization is recycled again.
(3) pulverize and sieve: the coating phenolic resin titanium carbide ceramic aggregation prepared is taken out from hermetic container, put in vacuum drying oven and be dried, then by its ball mill pulverizing, screening, the coating phenolic resin titanium carbide ceramic powder that particle diameter is 30 microns is obtained.
Embodiment 3
A kind of coating phenolic resin zirconia ceramics powder, including the phenolic resin of 10-20wt%, 1-2wt% hexamethylenamine, 0.5-1wt% stearic acid, surplus is the zirconium oxide of surface modification. The preparation method of this coating phenolic resin zirconia ceramics powder is as follows:
(1) prepare the zirconia ceramics powder of surface modification: take 1000g zirconia ceramics powder, respectively after dust technology, dilute sulfuric acid calcium and water clean, put into vacuum drying oven and be dried. Then the mixed liquor of 50g dehydrated alcohol and 10g methacryloxypropyl silane is mixed homogeneously with aforementioned oxidation zircon ceramic powder, use agitating device to be sufficiently stirred for mixture simultaneously and carry out surface modification treatment. After having reacted, mixture vacuum drying, sub-sieve are obtained the zirconia ceramics powder of the surface modification that particle diameter is 50 microns.
(2) coating phenolic resin zirconia ceramics aggregation is prepared: join in the hermetic container filling oxolane by the zirconia ceramics powder of surface modification, phenolic resin, pass into argon shield. Make the temperature in hermetic container rise to 65-75 DEG C from room temperature with the speed of 0.5-1 DEG C/min, the process of intensification adds hexamethylenamine and stearic acid, and stirs with agitating device so that it is be completely dissolved. The addition of each material is as previously mentioned. Intensification is incubated 1-2h after completing under argon shield, naturally cools to room temperature subsequently, obtains coating phenolic resin zirconia ceramics aggregation. The solvent of volatilization is recycled again.
(3) pulverize and sieve: the coating phenolic resin zirconia ceramics aggregation prepared is taken out from hermetic container, put in vacuum drying oven and be dried, then by its ball mill pulverizing, screening, the coating phenolic resin zirconia ceramics powder that particle diameter is 50 microns is obtained.
Coating phenolic resin ceramic powders prepared by the present invention obtains moulded blank by SLS forming machine, can obtain the ceramic part of better performances after the complete defat of gained blank through high temperature sintering. Phenolic resin has characteristics such as bonding force height, shaping shrinkage rate be little as bonding agent, and its SLS parison has stronger follow-up from strengthening ability. Therefore, select with ceramic powders bonding interface better and the higher phenolic resin of SLS drip molding intensity and portions additive as bonding agent, be conducive to improving shape base intensity, reduce the content of polymer bonding agent, improve part accuracy.
Claims (10)
1. the coating phenolic resin ceramic powders for laser 3D printing, it is characterised in that be made up of following raw material: ceramic powders, phenolic resin, hexamethylenamine, stearic acid, dehydrated alcohol and silane coupler.
2. coating phenolic resin ceramic powders as claimed in claim 1, it is characterised in that: described coating phenolic resin ceramic powders particle diameter is 10-50 μm.
3. coating phenolic resin ceramic powders as claimed in claim 1, it is characterized in that: in described coating phenolic resin ceramic powders, phenolic resin accounts for 10-30wt%, hexamethylenamine accounts for 1-2.5wt%, stearic acid accounts for 0.5-1.5wt%, surplus is the ceramic powders through silane coupler surface modification, during surface modification, silane coupler consumption is the 1-1.5% of ceramic powders quality, and the mass ratio of dehydrated alcohol and silane coupler is 3-5:1.
4. the coating phenolic resin ceramic powders as described in any one of claim 1-3, it is characterized in that: described ceramic powders is the one in carborundum, titanium carbide, zirconium carbide, aluminium oxide, zirconium oxide, described silane coupler is one or more in vinyl silanes, amino silane, methacryloxypropyl silane.
5. the preparation method for the laser 3D coating phenolic resin ceramic powders printed, it is characterized in that comprising the following steps: a) prepare the ceramic powders of surface modification: a certain amount of ceramic powders is dry after weak acid, weak base and water clean respectively, dry ceramic powders is mixed homogeneously by a certain percentage with dehydrated alcohol, silane coupler and stirred and carries out surface treatment, surface treatment complete after by mixture vacuum drying, cross classifying screen and obtain the ceramic powders of surface modification; B) coating phenolic resin pottery aggregation is prepared: join in the hermetic container filling organic solvent by a certain percentage by the ceramic powders of the step a) surface modification prepared and phenolic resin, pass into argon, the temperature of hermetic container is risen to 65-75 DEG C from room temperature, temperature-rise period adds a certain amount of hexamethylenamine and stearic acid and stirring makes it dissolve, intensification complete after held for some time, then naturally cool to room temperature and obtain coating phenolic resin pottery aggregation; C) crushing and screening: the coating phenolic resin pottery aggregation prepared by step b) crosses classifying screen after taking out and dry, pulverize.
6. the preparation method of coating phenolic resin ceramic powders as claimed in claim 5, it is characterized in that: in step a), ceramic powders is the one in carborundum, titanium carbide, zirconium carbide, aluminium oxide, zirconium oxide, described weak acid is the one in dilute hydrochloric acid, dilute sulfuric acid, dust technology, described weak base is the one in dilute sodium hydroxide, dilute sodium carbonate, dilute sulfuric acid calcium, and described silane coupler is one or more in vinyl silanes, amino silane, methacryloxypropyl silane.
7. the preparation method of coating phenolic resin ceramic powders as claimed in claim 5, it is characterised in that: in step a), silane coupler consumption is the 1-1.5% of ceramic powders quality, and the mass ratio of dehydrated alcohol and silane coupler is 3-5:1.
8. the preparation method of coating phenolic resin ceramic powders as claimed in claim 5, it is characterized in that: the described organic solvent of step b) is the one in ethanol, carbon tetrachloride, oxolane, hermetic container heating rate is 0.5-1 DEG C/min, and temperature retention time is 1-2h.
9. the preparation method of coating phenolic resin ceramic powders as claimed in claim 5, it is characterized in that: in step b), the weight proportion of each component is in end product coating phenolic resin ceramic powders, phenolic resin is 10-30wt%, hexamethylenamine is 1-2.5wt%, stearic acid is 0.5-1.5wt%, and surplus is the ceramic powders of surface modification.
10. the preparation method of coating phenolic resin ceramic powders as claimed in claim 5, it is characterised in that: the powder that step a) and step c) all selects particle diameter to be 10-50 μm after crossing classifying screen.
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Cited By (23)
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| CN106380206A (en) * | 2016-09-07 | 2017-02-08 | 济南大学 | Preparation method of zirconium nitride powder material for 3DP (three-dimensional printing) forming |
| CN107170953A (en) * | 2017-05-12 | 2017-09-15 | 西安工程大学 | A kind of warm therapy powdery electrode printed material and its preparation method for printing electrode |
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| CN110385395B (en) * | 2019-08-02 | 2021-01-08 | 中北大学 | Modified precoated sand for selective laser sintering and preparation method thereof |
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| CN113121242A (en) * | 2021-03-05 | 2021-07-16 | 中国科学院上海硅酸盐研究所 | Short carbon fiber toughened silicon carbide composite material and preparation method thereof |
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| CN115353324A (en) * | 2022-08-30 | 2022-11-18 | 航天特种材料及工艺技术研究所 | High-thermal-conductivity ablation-resistant composite material and preparation method thereof |
| CN116410013A (en) * | 2023-04-17 | 2023-07-11 | 潍坊华美智能科技有限公司 | Silicon carbide ceramic and preparation method thereof |
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