WO2019241911A1 - Formulation prototype de moule en résine pour moulage rapide par photodurcissement et son procédé de moulage par remplacement - Google Patents

Formulation prototype de moule en résine pour moulage rapide par photodurcissement et son procédé de moulage par remplacement Download PDF

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Publication number
WO2019241911A1
WO2019241911A1 PCT/CN2018/091850 CN2018091850W WO2019241911A1 WO 2019241911 A1 WO2019241911 A1 WO 2019241911A1 CN 2018091850 W CN2018091850 W CN 2018091850W WO 2019241911 A1 WO2019241911 A1 WO 2019241911A1
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WIPO (PCT)
Prior art keywords
curing
acrylate
layer
photo
resin mold
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Ceased
Application number
PCT/CN2018/091850
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English (en)
Chinese (zh)
Inventor
张丽
黄立
赵�卓
贺晓宁
方绚莱
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BMF Nano Material Technology Co Ltd
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BMF Nano Material Technology Co Ltd
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Priority to PCT/CN2018/091850 priority Critical patent/WO2019241911A1/fr
Publication of WO2019241911A1 publication Critical patent/WO2019241911A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C64/00—Additive manufacturing, i.e. manufacturing of three-dimensional [3D] objects by additive deposition, additive agglomeration or additive layering, e.g. by 3D printing, stereolithography or selective laser sintering
    • B29C64/10—Processes of additive manufacturing
    • B29C64/106—Processes of additive manufacturing using only liquids or viscous materials, e.g. depositing a continuous bead of viscous material
    • B29C64/124—Processes of additive manufacturing using only liquids or viscous materials, e.g. depositing a continuous bead of viscous material using layers of liquid which are selectively solidified
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00—Materials specially adapted for additive manufacturing
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/06—Coating with compositions not containing macromolecular substances
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/16—Nitrogen-containing compounds
    • C08K5/20—Carboxylic acid amides
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
    • C08L33/04—Homopolymers or copolymers of esters

Definitions

  • the invention belongs to the field of photo-curing, and particularly relates to a prototype of a resin mold used for photo-curing rapid molding and an investment casting process thereof.
  • Investment casting or "lost wax” casting is a precision casting process in which wax patterns are transformed into solid metal parts after multiple steps of processing.
  • Investment casting makes it possible to economically produce near-net-shape metal parts with complex geometries and features, including alloys that are difficult to machine or are not machined.
  • near-net-shape forming of castings can reduce processing time and costs and bring parts to specifications.
  • traditional investment casting is popular, the low-volume production of investment casting is very expensive in prototype, maintenance, custom or special component production due to the high cost of molds for wax patterns and the long manufacturing and shaping cycles. of.
  • Rapid prototyping (RP) technology is rapidly becoming the standard tool for product design and manufacturing. With its disruptive capabilities, it can quickly manufacture 3D parts for design verification or as a functional prototype and production tool, and is an indispensable tool for shortening product design and development time cycles.
  • RP Rapid prototyping
  • SLA stereolithography
  • DLP digital light processing
  • SLS selective laser sintering
  • FDM fused deposition / fuse deposition
  • LOM layered solid manufacturing
  • EBFF electron beam fuse deposition
  • Rapid prototyping is the most direct casting model for precision casting.
  • the dimensional accuracy of castings mainly depends on the accuracy of the prototype.
  • SLA and DLP are made by photo-curing using photosensitive resin as the material. Due to the characteristics of good surface quality, high dimensional accuracy, and the ability to achieve relatively fine dimensional molding, SLA and DLP have been widely used. .
  • Light curing rapid prototyping investment casting technology is to replace the wax pattern in investment casting with a prototype of liquid photosensitive resin, that is, the resin prototype is first printed layer by layer on the light curing rapid prototyping machine, and then the refractory material is poured multiple times, such as Fused silica, alumina and magnesia ceramic pastes are used to form investment casting shells. After drying until the shells are solidified, the resin is fired to remove the resin. The resulting refractory ceramic shell is used as the casting shell. Cool to obtain metal parts.
  • the photosensitive resin system composed of reactive diluent, unsaturated acrylate and epoxy oligomer, and ultraviolet photoinitiator is used for laser rapid molding.
  • the photosensitive resin system composed of reactive diluent, unsaturated acrylate and epoxy oligomer, and ultraviolet photoinitiator is used for laser rapid molding.
  • CN 105802257A traditional rosin and paraffin are used as the matrix, and a small amount of additives are added to obtain a solid resin at room temperature.
  • the mixture system is heated and liquefied and spray-cooled and solidified by a 3D printing nozzle.
  • the resin used for photo-curing rapid molding is a thermosetting resin after the photo-curing reaction. It cannot melt and flow after being heated. It can only be softened first, and then gasified and disappeared as the temperature continues to rise. In the initial stage of the mold baking and removal of the resin mold prototype, the mold may expand and crack due to the thermal expansion of the prototype; in addition, if the initial thermal decomposition temperature of the resin is high, or the thermal decomposition process is concentrated in a local temperature range, it is easy to produce too much The gas cracked the shell.
  • the resin mold prototype After the baking is completed, if the resin mold prototype has a large amount of ash residue or tar-like residue that is not easy to remove, it will cause defects such as inclusions in the casting.
  • the system formula is a conventional photo-curing photosensitive resin.
  • the double bonds are cross-linked into a three-dimensional network structure under the initiation of a photoinitiator, and are cured layer by layer until the desired Model. Then, a ceramic slurry is poured on the mold, and then baked.
  • the photo-curing reaction is a thermosetting resin material
  • the present invention provides a resin mold for photo-curing rapid molding, which includes, by weight percentage, a photosensitive resin: 60-95 wt%, and an inert low-molecular weight substance: 5-40 wt%.
  • the photosensitive resin includes, by weight percentage, 10-70 wt% of an active oligomer, 20-70 wt% of a reactive diluent, 0.2-6 wt% of a photoinitiator, and the balance is a functional auxiliary.
  • the active oligomer is at least one of acrylate, acrylamide and silane acrylate.
  • the acrylate is selected from at least one of pure acrylate, epoxy acrylate, urethane acrylate, and polyester acrylate.
  • the reactive diluent uses at least one of a bifunctional or polyfunctional alkyl acrylate, an alkoxy acrylate, and an ethylene glycol acrylate.
  • the photoinitiator uses a free-radical type and a cationic type photoinitiator which can absorb under 250-440 nm ultraviolet light.
  • the free radical type photoinitiator uses phenylbis (2,4,6-trimethylbenzoyl) phosphine oxide, ethyl 2,4,6-trimethylbenzoylphosphonic acid, and diphenyl (2, 4,6-trimethylbenzoyl) phosphine oxide, bis 2,6-difluoro-3-pyrrolephenylferrocene, 2-isopropylthioanthrone, 4-phenylbenzophenone, At least one of 2-phenylbenzyl-2-dimethylamine-1- (4-morpholine benzylphenyl) butanone;
  • the cationic photoinitiator uses an aryldiazonium salt, a diaryl iodonium salt, At least one of a triarylsulfonium salt and an aromatic ferrocen
  • the functional additive uses at least one of a defoaming agent, a leveling agent, and an adhesion promoter, and the additive amount of each additive is 0.5-4% of the total weight of the resin mold.
  • the defoamer uses at least one of aliphatic amide, polyethylene glycol, modified polydimethylsiloxane, and polymer solution without silicone;
  • the leveling agent uses polyacrylate compound, polyether / At least one of a polyester / aralkyl-modified dimethylsiloxane solution and a fluorocarbon-modified polyacrylate copolymer solution;
  • the adhesion promoter uses amine silane, phosphate polymer, and epoxy silane At least one of oligomers.
  • Inert low-molecular-weight substances use suitable moderate-boiling substances, and their boiling points are preferably in the range of 120-250 ° C; and their molecular weights are in the range of 50-5000, preferably 200-1000; inert low-molecular-weight substances use inert oligomers and inert small molecules At least one of the diluents.
  • the inert oligomer may be at least one of polycaprolactone polyol, polypropylene glycol, ethylene polymer, and polyvinylpyrrolidone.
  • the inert small molecule diluent may be at least one of ethylene glycol, glycerol, propylene carbonate, butoxymethacrylamide, and diethylene glycol dimethyl ether.
  • the inert low-molecular-weight substances do not participate in the photo-curing polymerization reaction, do not react with the functional groups in the components in the photosensitive system, have better solubility in the photosensitive resin system, and have a lower solubility during the firing process.
  • a method for preparing a photo-curing system the active oligomer, a reactive diluent, a photoinitiator, a functional auxiliary, and an inert low-molecular-weight substance are stirred at a medium speed for 5-15h at a certain ratio to obtain a uniform photo-curing system.
  • the viscosity range of the system is 100-3000 cp, and the preferred viscosity is 100-1500 cp.
  • Investment casting or "lost wax” casting is a precision casting process in which a resin mold is transformed into solid metal parts after multiple steps of processing.
  • the invention combines the rapid prototyping technology and the investment casting technology, and uses a rapid prototype to prepare a direct casting model. Compared with traditional wax mold casting, this method has the advantages of low cost, high efficiency, non-deformation, and can produce more precise castings. It only needs to change the CAD geometric model to obtain the casting mold very conveniently, which can greatly save the production.
  • the time of the mold can achieve efficient and high-precision rapid casting in the art casting, jewelry and other industries, and has a wide application prospect in the industrial fields such as aviation and civil parts.
  • the present invention adopts the above technical solution, and has the advantages that: Adding an inert low-molecular-weight substance to the photo-curing system, the inert substance does not participate in the photo-curing polymerization reaction, does not react with the functional groups in the components of the photosensitive system, has good solubility in the photosensitive resin system, and During the firing process, gasification or decomposition at a lower temperature leaves a void in the three-dimensional model, and in the process of further increasing the temperature, the model expands to the void to prevent cracking of the shell. After the calcination was completed, the resin mold prototype was completely consumed, and no tar-like residue or obvious ash was found in the mold shell.
  • Preparation method of light curing system the oligomer, reactive diluent, photoinitiator, functional assistant and inert low molecular weight substance are stirred at a medium speed for 5-15h at a certain ratio to obtain a uniform light curing system.
  • the viscosity range of this system is 100-3000 cp, and the preferred viscosity is 100-1500 cp.
  • a light curing molding process method includes the following steps:
  • Step A Design a three-dimensional solid model by modeling software, slice the model according to the designed solidified layer thickness using the slicing software, and import the sliced file into the light curing rapid prototyping machine (SLA or DLP) control software;
  • SLA or DLP light curing rapid prototyping machine
  • Step B The above-mentioned photo-curing system is placed under SLA or DLP to perform point-by-point / layer-by-layer exposure curing, and when a layer is processed, a section of the part is generated;
  • Step C The forming platform rises or falls by a distance of a solidified layer thickness, and the thickness of each layer ranges from 20 to 100 ⁇ m;
  • Step D Repeat the above steps, and build up the layer by layer to obtain a three-dimensional solid model.
  • the layer thickness is 20, 50, 75, or 100 ⁇ m.
  • the wavelength of the photo-curing rapid prototyping machine is preferably 355 nm, 365 nm, 385 nm, 405 nm, and 420 nm.
  • a model baking method includes the following steps:
  • Step (1) The above-mentioned photo-cured three-dimensional prototype is coated with a refractory slurry to form an investment casting mold shell. After the first layer of the coated slurry is dried, it is coated again. This step is repeated 10- 20 times;
  • Step (2) It is immersed in a metal container containing refractory paste, and then put together in a sintering furnace to bake off the resin mold prototype, so that the cavity corresponding to the final three-dimensional part is left in the refractory shell. Structure; Finally, the molten metal or alloy is injected into the liquid, and the refractory shell is removed after cooling to obtain the final three-dimensional metal or alloy component.
  • the refractory slurry is made of ceramic slurry such as fused silica, alumina, and magnesia.
  • thermogravimetric analysis tests were performed on the solidified model. The results show that the moderate heat of the system is mainly divided into two stages. The first stage is at 120-250 ° C. The thermal decomposition in this stage is mainly the gas of inert low molecular weight substances.
  • the decomposition or decomposition leaves a void in the three-dimensional model, and the model expands to the void in the process of further increasing the temperature, which can prevent the cracking of the shell; the second stage is at 300-500 ° C, mainly the molecular chain breaks.
  • the opening of the chemical bonds between the atoms changes the large molecules into small molecules. This thermal weight loss characteristic can provide guidance for the process of the roasting process.
  • the roasting process includes: slowly heating up to 80-120 ° C at a rate of 2-10 ° C / h and holding for 4-12 hours; and then heating up to 120-250 ° C at a rate of 1-5 ° C / min, Incubate for 2-8 h; finally heat up to 700-1000 ° C at a rate of 1-5 ° C / min, and incubate for 2-8 hours to ensure that the resin does not have any residue.
  • the prototype was roasted, no tar-like residue or obvious ash was found in the shell, and the ash content was less than 0.5%.
  • an inert low-molecular-weight substance is added to the photo-curing system.
  • the inert substance does not participate in the photo-curing polymerization reaction, does not react with the functional groups in the components in the photosensitive system, and has good solubility in the photosensitive resin system.
  • gasification or decomposition at a lower temperature leaves a void in the three-dimensional model, and the model expands to the void in the process of further increasing the temperature, thereby preventing the shell from cracking.
  • a thermal weight loss analysis test is performed on the cured resin to provide guidance for subsequent firing processes.
  • the resin mold prototype was completely consumed, and no tar-like residue or obvious ash was found in the mold shell.
  • this method has the advantages of low cost, high efficiency, non-deformation, and can produce thinner castings.
  • the product is upgraded, only the CAD geometric model needs to be changed, and the casting can be obtained very conveniently.
  • the mold can greatly save the time for making the mold. It can achieve high-efficiency and high-precision rapid casting in the art casting, jewelry and other industries, and has a wide application prospect in the industrial fields such as aviation and civil parts.
  • a three-dimensional solid model is designed by the modeling software, and the model is sliced according to the designed solidified layer thickness using the slicing software.
  • the sliced file is imported into the 405nm light curing rapid prototyping machine (SLA or DLP) control software.
  • SLA or DLP light curing rapid prototyping machine
  • the system is placed under SLA or DLP for point-by-point / layer-by-layer exposure curing.
  • SLA or DLP rapid prototyping machine
  • the layer thickness is 20 ⁇ m, and the above steps are repeated. 3D layer-by-layer accumulation and accumulation to obtain a three-dimensional solid model.
  • the three-dimensional prototype is coated with refractory slurry fused silica to form an investment casting mold shell. After the first layer of the coated slurry is dried, it is coated again. This step is repeated 10 times, and it is immersed in a refractory container. Put the slurry in the metal container and put it together in a sintering furnace to bake the prototype of the resin mold.
  • the baking process includes: slowly heating to 80 ° C at a rate of 2 ° C / h and holding for 4 hours; then at 1 ° C / min heats up to 150 ° C for 2 h; finally heats up to 700 ° C at a rate of 1 ° C / min for 2 h, leaving the cavity structure corresponding to the final three-dimensional part in the refractory shell; finally The liquid molten alloy is injected, and the refractory shell is removed after cooling to obtain the final three-dimensional alloy part.
  • a three-dimensional solid model is designed by the modeling software.
  • the model is used to slice the model according to the designed solidified layer thickness.
  • the sliced file is imported into the 365nm light curing rapid prototyping machine (SLA or DLP) control software.
  • SLA or DLP light curing rapid prototyping machine
  • the system is placed under SLA or DLP for point-by-point / layer-by-layer exposure curing.
  • SLA or DLP rapid prototyping machine
  • the layer thickness is 50 ⁇ m. Repeat the above steps. 3D layer-by-layer accumulation and accumulation to obtain a three-dimensional solid model.
  • the three-dimensional prototype is coated with alumina slurry of refractory slurry to form an investment casting shell. After the first layer of slurry to be coated is dried, it is coated again. This step is repeated 20 times, and it is immersed in the refractory container. Put the slurry in the metal container and put it together in a sintering furnace to bake the resin mold prototype.
  • the baking process includes: slowly heating to 120 ° C at a rate of 10 ° C / h, holding for 12 hours; and then at 5 ° C.
  • a three-dimensional solid model is designed by the modeling software.
  • the slice software is used to slice the model according to the designed solidified layer thickness.
  • the sliced file is imported into the 385nm light curing rapid prototyping machine (SLA or DLP) control software.
  • SLA or DLP 385nm light curing rapid prototyping machine
  • the light is cured.
  • the system is placed under SLA or DLP for point-by-point / layer-by-layer exposure curing.
  • the layer thickness range is 75 ⁇ m. Repeat the above.
  • layer-by-layer accumulation is formed to obtain a three-dimensional solid model.
  • the three-dimensional prototype is coated with refractory slurry magnesia to form an investment casting mold shell. After the first layer of the coated slurry is dried, it is coated again. This step is repeated 15 times, and it is immersed in the refractory container. Put the slurry in a metal container and put it together in a sintering furnace to bake the prototype of the resin mold.
  • the baking process includes: slowly heating to 100 ° C at a rate of 6 ° C / h and holding for 8 hours; then at 3 ° C The heating rate is increased to 180 ° C / min for 5 hours, and the temperature is raised to 800 ° C at the rate of 3 ° C / min for 5 hours, so that the cavity structure corresponding to the final three-dimensional component is left in the refractory shell; Finally, the liquid molten metal is injected, and the refractory shell is removed after cooling to obtain the final three-dimensional metal part.
  • a three-dimensional solid model is designed by the modeling software.
  • the model is used to slice the model according to the designed solidified layer thickness.
  • the sliced file is imported into the 365nm light curing rapid prototyping machine (SLA or DLP) control software.
  • SLA or DLP light curing rapid prototyping machine
  • the system is placed under SLA or DLP for point-by-point / layer-by-layer exposure curing.
  • SLA or DLP rapid prototyping machine
  • the layer thickness range is 100 ⁇ m. Repeat the above.
  • layer-by-layer accumulation is formed to obtain a three-dimensional solid model.
  • the three-dimensional prototype is coated with refractory slurry fused silica to form an investment casting mold shell. After the first layer of the coated slurry is dried, it is coated again. This step is repeated 18 times, and it is immersed in a refractory container. Put the slurry in a metal container, and then put it together in a sintering furnace to bake the prototype of the wax mold.
  • the baking process includes: slowly heating to 110 ° C at a rate of 8 ° C / h, and holding it for 10h; then at 2 ° C / Heating at a rate of min to 200 ° C for 6 h; finally heating to 900 ° C at a rate of 4 ° C / min for 6 h, leaving the cavity structure corresponding to the final three-dimensional component in the refractory shell; finally The molten metal is injected and the refractory shell is removed after cooling to obtain the final three-dimensional metal part.
  • the invention can obtain a three-dimensional prototype with a fine structure, a certain mechanical property and an elongation at break by a light-curing rapid forming method; and the initial temperature of thermal weight loss is low during the firing process, the thermal weight loss curve is smooth, and the shell will not appear Cracking phenomenon; no tar-like residue or obvious ash was found in the mold shell after the roasting of the prototype, and the ash content was less than 0.5%.
  • the method has the advantages of low cost, high efficiency, non-deformation, and can produce thinner and more precise castings.
  • it is only necessary to change the CAD geometric model to obtain the casting mold very conveniently, which can greatly save the production of molds. In time, it can achieve efficient and high-precision rapid casting in the art casting, jewelry and other industries, and has a wide application prospect in the industrial fields such as aviation and civil parts.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Optics & Photonics (AREA)
  • Moulds For Moulding Plastics Or The Like (AREA)

Abstract

L'invention concerne un moule en résine pour moulage rapide par photodurcissement, comprenant, en pourcentages en poids : une résine photosensible à hauteur de 60 à 95 % en poids, et une substance inerte à faible poids moléculaire à hauteur de 5 à 40 %, la résine photosensible comprenant de 10 à 70 % en poids d'un oligomère actif, de 20 à 70 % en poids d'un diluant actif, de 0,2 à 6 % en poids d'un photoinitiateur, le reste étant constitué d'un agent auxiliaire fonctionnel. L'invention concerne également un procédé de préparation d'un système de photodurcissement, un processus de moulage par photodurcissement et un procédé de cuisson d'un moule. Un procédé de moulage utilisant le moule en résine présente les avantages d'avoir un faible coût et un rendement élevé, de ne pas être susceptible de se déformer, et de pouvoir produire un moulage plus fin.
PCT/CN2018/091850 2018-06-19 2018-06-19 Formulation prototype de moule en résine pour moulage rapide par photodurcissement et son procédé de moulage par remplacement Ceased WO2019241911A1 (fr)

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PCT/CN2018/091850 WO2019241911A1 (fr) 2018-06-19 2018-06-19 Formulation prototype de moule en résine pour moulage rapide par photodurcissement et son procédé de moulage par remplacement

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PCT/CN2018/091850 WO2019241911A1 (fr) 2018-06-19 2018-06-19 Formulation prototype de moule en résine pour moulage rapide par photodurcissement et son procédé de moulage par remplacement

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CN117445131A (zh) * 2023-11-07 2024-01-26 西安交通大学 一种复杂陶瓷构件的电子束固化成形方法、材料及设备
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US12564876B2 (en) 2021-04-27 2026-03-03 Ppg Industries Ohio, Inc. Co-reactive additive manufacturing compositions and articles for use in investment casting
CN117362049A (zh) * 2023-09-26 2024-01-09 哈尔滨工业大学重庆研究院 一种陶瓷粉体的改性方法、微波介质陶瓷浆料及其制备方法和应用
CN117445131A (zh) * 2023-11-07 2024-01-26 西安交通大学 一种复杂陶瓷构件的电子束固化成形方法、材料及设备
CN121006015A (zh) * 2025-10-27 2025-11-25 吉林大学 一种用于建立骨不连动物模型的隔离器及其制备方法

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