CN111070668A - Method for preparing pore-diameter-controllable nano porous structure workpiece by fused deposition molding technology - Google Patents
Method for preparing pore-diameter-controllable nano porous structure workpiece by fused deposition molding technology Download PDFInfo
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- CN111070668A CN111070668A CN201911307631.7A CN201911307631A CN111070668A CN 111070668 A CN111070668 A CN 111070668A CN 201911307631 A CN201911307631 A CN 201911307631A CN 111070668 A CN111070668 A CN 111070668A
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- 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
- B29C64/118—Processes of additive manufacturing using only liquids or viscous materials, e.g. depositing a continuous bead of viscous material using filamentary material being melted, e.g. fused deposition modelling [FDM]
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- 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
- B29C64/30—Auxiliary operations or equipment
- B29C64/386—Data acquisition or data processing for additive manufacturing
- B29C64/393—Data acquisition or data processing for additive manufacturing for controlling or regulating additive manufacturing processes
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- 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
- B29C64/40—Structures for supporting 3D objects during manufacture and intended to be sacrificed after completion thereof
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- 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
- B29C67/00—Shaping techniques not covered by groups B29C39/00 - B29C65/00, B29C70/00 or B29C73/00
- B29C67/20—Shaping techniques not covered by groups B29C39/00 - B29C65/00, B29C70/00 or B29C73/00 for porous or cellular articles, e.g. of foam plastics, coarse-pored
- B29C67/202—Shaping techniques not covered by groups B29C39/00 - B29C65/00, B29C70/00 or B29C73/00 for porous or cellular articles, e.g. of foam plastics, coarse-pored comprising elimination of a solid or a liquid ingredient
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y50/00—Data acquisition or data processing for additive manufacturing
- B33Y50/02—Data acquisition or data processing for additive manufacturing for controlling or regulating additive manufacturing processes
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- Optics & Photonics (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
Abstract
The invention relates to a method for preparing a pore-diameter-controllable nano porous structure workpiece by adopting a fused deposition molding technology, which comprises the following steps: preparing silicon dioxide microspheres according to a preset particle size; uniformly mixing a material to be molded with the silicon dioxide microspheres to obtain a mixture; filling the mixture into a high-molecular pipe to obtain a material-containing pipe; carrying out fused deposition molding printing on the material-containing pipe to obtain a molded part containing silicon dioxide microspheres; dissolving the silica microspheres in the molded part containing the silica microspheres by using a solvent to obtain a nano porous structure molded part with the pore diameter being the same as the preset particle diameter; the method realizes the controllable aperture of the porous structure part and the directional manufacture of the nanometer level pores; meanwhile, by using the high-molecular pipe, the selection range of the molding material of the fused deposition molding technology is widened, the applicability is strong, and a new method is provided for the rapid preparation of the composite material and the foaming material.
Description
Technical Field
The invention belongs to the technical field related to material processing and forming, and particularly relates to a method for preparing a pore-size-controllable nano porous structure workpiece by adopting a fused deposition forming technology.
Background
Fused Deposition Modeling (FDM) is a technique in which a filament of material, such as a thermoplastic, wax or metal, is melt deposited at a fixed rate and following a predetermined trajectory for each layer of the article by extruding the filament from a heated nozzle. And when one layer is finished, the workbench descends one layer thickness to carry out superposition deposition on a new layer, and the steps are repeated to finally realize the deposition molding of the part.
The nano porous structure product refers to a material with a structure of nano-scale holes on the surface or inside, has the characteristics of low density, high specific surface area, high porosity, high specific strength, high adsorbability and the like, is widely applied to the aspects of sensors, separation, noise elimination, filtration, catalysis, adsorption and the like, and at present, the distribution of the holes and the size of the holes of the nano porous structure product are not easy to regulate and control according to actual requirements, so that a method for preparing the nano porous structure product with controllable hole diameter by combining a fused deposition molding technology is urgently needed in the field.
Disclosure of Invention
In view of the above problems, the present invention has been made to provide a method for preparing a pore-size-controllable nanoporous structural article using fused deposition modeling techniques that overcomes or at least partially solves the above problems.
The embodiment of the invention provides a method for preparing a pore-diameter-controllable nano porous structure workpiece by combining a fused deposition modeling technology, which comprises the following steps:
preparing silicon dioxide microspheres according to a preset particle size;
uniformly mixing a material to be molded with the silicon dioxide microspheres to obtain a mixture;
filling the mixture into a high-molecular pipe to obtain a material-containing pipe;
carrying out fused deposition molding printing on the material-containing pipe to obtain a molded part containing silicon dioxide microspheres;
and dissolving the silica microspheres in the molded part containing the silica microspheres by using a solvent to obtain the molded part with the nano-porous structure, wherein the pore diameter of the molded part is the same as the preset particle diameter.
Optionally, the material to be molded includes a solid material or a liquid material.
Optionally, the solid material comprises a filamentous material or a powder material, and the filling rate of the solid material in the material-containing pipe is 0-100%.
Optionally, a curing agent is added into the liquid material, the curing speed of the liquid material is the same as the printing speed, and the filling rate of the liquid material in the material-containing pipe is 100%.
Optionally, the solid material comprises one of: polyvinylidene fluoride, trifluoroethylene, polyvinylidene fluoride-trifluoroethylene copolymer, vinylidene fluoride-tetrafluoroethylene copolymer, lignin, chitosan and cellulose.
Optionally, the liquid material includes one of: polydimethylsiloxane, polyvinyl alcohol resin and molten polyethylene glycol.
Optionally, the material of the polymer pipe includes one of the following: PA, PE, PP, PVDF, PLA, ABS, PTFE.
Optionally, the solvent comprises at least one of: sodium hydroxide solution, potassium hydroxide solution.
Optionally, the printing temperature of the fused deposition modeling printing is 0 ℃ to 600 ℃.
Based on the same inventive concept, the embodiment of the invention also provides a pore-diameter-controllable nano porous structure workpiece, which is prepared by the method.
One or more technical solutions in the embodiments of the present invention have at least the following technical effects or advantages:
1. according to the method for preparing the pore-size-controllable nano porous structure workpiece by combining the fused deposition modeling technology, the silica microspheres are prepared according to the preset particle size, and then the silica microspheres in the molded workpiece are dissolved and removed, so that the nano porous structure workpiece with the pore size same as the preset particle size is obtained, the pore size is controllable, and the directional manufacturing of nano-grade pores can be realized; meanwhile, the polymer pipe is used, so that the forming material is widened from the existing wire material to a solid material or a liquid material, the selection range of the forming material by the fused deposition forming technology is widened, and the applicability is strong; also provides a new method for the rapid preparation of the composite material and the foaming material;
2. the method for preparing the pore-size-controllable nano porous structure workpiece by combining the fused deposition modeling technology provided by the embodiment of the invention has the advantages of simple process, easiness in implementation and lower cost.
The foregoing description is only an overview of the technical solutions of the present invention, and the embodiments of the present invention are described below in order to make the technical means of the present invention more clearly understood and to make the above and other objects, features, and advantages of the present invention more clearly understandable.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. In the drawings:
FIG. 1 is a schematic flow chart of a method for preparing a pore-size-controllable nanoporous structure by combining fused deposition modeling.
Detailed Description
The present invention will be described in detail below with reference to specific embodiments and examples, and the advantages and various effects of the present invention will be more clearly apparent therefrom. It will be understood by those skilled in the art that these specific embodiments and examples are for the purpose of illustrating the invention and are not to be construed as limiting the invention.
Throughout the specification, unless otherwise specifically noted, terms used herein should be understood as having meanings as commonly used in the art. Accordingly, unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. If there is a conflict, the present specification will control.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
It should be further noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
In order to solve the technical problems, the technical scheme in the embodiment of the invention has the following general idea:
the embodiment of the invention provides a method for preparing a pore-diameter-controllable nano porous structure workpiece by combining a fused deposition modeling technology, which comprises the following steps:
preparing silicon dioxide microspheres according to a preset particle size;
uniformly mixing a material to be molded with the silicon dioxide microspheres to obtain a mixture;
filling the mixture into a high-molecular pipe to obtain a material-containing pipe;
carrying out fused deposition molding printing on the material-containing pipe to obtain a molded part containing silicon dioxide microspheres;
and dissolving the silica microspheres in the molded part containing the silica microspheres by using a solvent to obtain the molded part with the nano-porous structure, wherein the pore diameter of the molded part is the same as the preset particle diameter.
The solvent reacts with the silica to dissolve the silica, and the positions occupied by the silica microspheres originally become pores with corresponding sizes. The size of the pores can be directionally controlled by controlling the size of the silica.
In some alternative embodiments, the material to be formed comprises a solid material or a liquid material.
The solid material or the liquid material cannot be directly printed through FDM originally, but is filled in the pipe, and when the pipe is extruded and fed by a wire feeding gear of a printer, the filled solid material and the filled liquid material are synchronously extruded, so that the solid material and the liquid material are printed.
In some alternative embodiments, the solid state material includes, but is not limited to, one of: polyvinylidene fluoride, trifluoroethylene, polyvinylidene fluoride-trifluoroethylene copolymer, vinylidene fluoride-tetrafluoroethylene copolymer, lignin, chitosan and cellulose.
In some alternative embodiments, the liquid material includes, but is not limited to, one of: polydimethylsiloxane, polyvinyl alcohol resin, molten polyethylene glycol, and the like.
In some optional embodiments, the solid material comprises a filamentous material or a powder material, and the filling rate of the solid material in the material-containing pipe is 0-100%.
The powder filled inside is not compacted, and a gap exists between the powder and the powder, and the filling rate can be between 0 and 100 percent according to the bulkiness of the powder; if the wire is inserted inside, the filling rate can be adjusted between 0 and 100% according to the size of the wire.
In some optional embodiments, a curing agent (which may be cured without the curing agent, such as polyethylene glycol, and may be cured at room temperature) is added to the liquid material, the curing speed of the liquid material is the same as the printing speed, and the filling rate of the liquid material in the material-containing tube is 100%.
In this example, the curing agent needs to be added to the liquid material for the following reasons: to form an article, the liquid material needs to be capable of being cured after being extruded from the nozzle, and therefore a material capable of being cured is used.
In the present embodiment, the curing speed of the liquid material is defined to be the same as the printing speed because: the curing speed of the liquid material and the printing speed should be matched, if the curing speed is too high, the extruded material is cured before falling onto a printer hot table, and a spray head is easily blocked, so that the printing process is influenced; if the curing speed is too slow, the extruded liquid material needs a long time to be cured, the liquid material is difficult to shape on a smooth hot table due to the ductility of the liquid material, in addition, FDM works based on the layer-by-layer stacking principle, and if the next layer is printed, the upper layer is not cured, the next layer loses support, and the forming is difficult.
In this example, the filling rate of the liquid material was 100%, because: due to the ductility of the liquid material, the pipe can be filled only, and the filling rate is 100 percent.
In this embodiment, the selection and the amount of the curing agent are determined according to the type of the liquid material, and the composition of the liquid material and the curing agent includes, but is not limited to, the following mixture ratio (mass ratio):
polydimethylsiloxane main agent: curing agent is 10: 1-60: 1;
yield 7148AB glue a: the glue B is 1: 1-2: 1;
hensmei epoxy LY 1564: curing agent 22962 at 4: 1-10: 1;
hensmei epoxy resin GY 250: curing agent 265-1 ═ 2: 1-5: 1;
hensmei epoxy resin GY 250: the curing agent 100 is 1: 1-2: 1.
In some optional embodiments, the material of the polymer tubing comprises one of: PA, PE, PP, PVDF, PLA, ABS, PTFE.
The material of the polymer pipe can be made into a pipe, and the pipe is a consumable material commonly used for FDM printing and has wide source. However, the tube described in this embodiment is not limited to the above-mentioned ones, and can be customized as needed, and only needs to be melted within the printing temperature range and solidified again after being extruded from the nozzle.
In this embodiment, the outer diameter of the polymer tube should match the size of the throat of the FDM printer (the size of the throat of the FDM printer is generally 1.75mm-3mm), and the inner diameter of the polymer tube should be greater than 0 mm.
The external diameter of polymer tubular product can not exceed the size of printer choke, otherwise unable feeding, and the external diameter undersize can also lead to unable feeding because of can't be pressed from both sides tightly by the feeding gear. The inner diameter of the polymer pipe is larger than 0mm, otherwise, the material to be formed cannot be filled into the polymer pipe.
In some optional embodiments, the fused deposition modeling print has a print temperature of 0 ℃ to 600 ℃.
The temperature is too low, and the pipe and the filling material are not melted and cannot be extruded from the spray head; the temperature is too high to exceed the decomposition temperature or operating temperature conditions of the material, causing the material to decompose or render the material ineffective.
In some alternative embodiments, the solvent comprises at least one of: sodium hydroxide solution, potassium hydroxide solution.
The solvent can achieve a good corrosion effect in a short time.
In this embodiment, the method for preparing the silica microspheres includes, but is not limited to, one of the following:
methods, super-gravity methods, micro-emulsion methods, chemical vapor deposition methods, pulverization methods, sputtering methods, precipitation methods.
The microsphere synthesized by the method has easily controlled size and easily functionalized surface, wherein
The silicon dioxide microspheres prepared by the method have better uniformity, higher sphericity and more moderate particle size.
Based on the same inventive concept, the embodiment of the invention also provides a pore-diameter-controllable nano porous structure workpiece, which is prepared by the method.
In the field of nano-generators, the porous structure has a decisive influence on the performance of the generator. The output performance of the piezoelectric and triboelectric nano-generator can be greatly improved by a proper porous structure, and the increase of the performance of the nano-generator is not facilitated by too large or too small pore diameter and porosity.
Example 1
The method for preparing the part with the controllable nano porous structure by adopting the fused deposition modeling technology with the polymer pipe as the carrier is used for carrying out 3D printing on the polydimethylsiloxane material, and mainly comprises the following steps:
(1) and feeding the PA pipe which can reach a molten state within the printing temperature range of the fused deposition modeling printer, cannot be decomposed and has an outer diameter meeting the wire feeding requirement of the spray head of the fused deposition modeling printer into the spray head of the fused deposition modeling printer based on the fused deposition principle for clamping. Hensmei epoxy LY 1564: curing agent 22962
(2) By passing
The method synthesizes the silica microspheres with the diameter of 200 nm.
(3) The silica microspheres are doped into Hensman epoxy LY1564 mixed with curing agent 22962, wherein the mass ratio of the curing agent 22962 to the Hensman epoxy LY1564 is 1: 1.
(4) And (4) adding the material mixed in the step (3) into an inner hole of the PA pipe by using a boosting device, wherein the filling rate is 100%.
(5) In the printing process, the polymer tube material injected with the liquid material is heated and melted in the nozzle, the nozzle extrudes the melted material at a predetermined pressure while moving along the cross-sectional profile and the filling trajectory of the desired product, the melted material is bonded with the previous layer and rapidly solidified in the air, and so on to form the desired product.
(6) And (3) corroding the silicon dioxide microspheres in the solution by using a sodium hydroxide solution to obtain a porous structural part with uniformly distributed apertures of 200 nm.
Example 2
The method for preparing the part with the controllable nano porous structure by adopting the fused deposition modeling technology with the ABS pipe as the carrier is used for carrying out 3D printing on the polyvinylidene fluoride material, and mainly comprises the following steps:
(1) and feeding the ABS pipe which can reach a molten state within the printing temperature range of the fused deposition modeling printer, is not decomposed and has an outer diameter meeting the wire feeding requirement of the spray head of the fused deposition modeling printer into the spray head of the fused deposition modeling printer based on the fused deposition principle for clamping.
(2) By passing
The method synthesizes the silica microspheres with the diameter of 200 nm.
(3) Silica microspheres were doped into polyvinylidene fluoride.
(4) And (4) adding the material mixed in the step (3) into an inner hole of the ABS pipe by using a boosting device, wherein the filling rate is 50%.
(5) In the printing process, the polymer tube material injected with the liquid material is heated and melted in the nozzle, the nozzle extrudes the melted material at a predetermined pressure while moving along the cross-sectional profile and the filling trajectory of the desired product, the melted material is bonded with the previous layer and rapidly solidified in the air, and so on to form the desired product.
(6) And (3) corroding the silicon dioxide microspheres in the solution by using a potassium hydroxide solution to obtain a porous structural part with uniformly distributed apertures of 200 nm.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (10)
1. A method for preparing a pore-diameter-controllable nano porous structure workpiece by combining a fused deposition modeling technology is characterized by comprising the following steps:
preparing silicon dioxide microspheres according to a preset particle size;
uniformly mixing a material to be molded with the silicon dioxide microspheres to obtain a mixture;
filling the mixture into a high-molecular pipe to obtain a material-containing pipe;
carrying out fused deposition molding printing on the material-containing pipe to obtain a molded part containing silicon dioxide microspheres;
and dissolving the silica microspheres in the molded part containing the silica microspheres by using a solvent to obtain the molded part with the nano-porous structure, wherein the pore diameter of the molded part is the same as the preset particle diameter.
2. The method of claim 1, wherein the material to be formed comprises a solid material or a liquid material.
3. The method of claim 2, wherein the solid material comprises a filamentous material or a powder material, and the filling rate of the solid material in the tube is 0-100%.
4. The method for preparing the pore-size-controllable nano-porous structural part by combining the fused deposition modeling technology as claimed in claim 2, wherein a curing agent is added into the liquid material, the curing speed of the liquid material is the same as the printing speed, and the filling rate of the liquid material in the material-containing pipe is 100%.
5. The method of claim 2, wherein the solid material comprises one of: polyvinylidene fluoride, trifluoroethylene, polyvinylidene fluoride-trifluoroethylene copolymer, vinylidene fluoride-tetrafluoroethylene copolymer, lignin, chitosan and cellulose.
6. The method of claim 2, wherein the liquid material comprises one of: polydimethylsiloxane, polyvinyl alcohol resin and molten polyethylene glycol.
7. The method for preparing a pore-size-controllable nano-porous structural member by combining fused deposition modeling technology as claimed in claim 1, wherein the material of the polymer tube comprises one of the following: PA, PE, PP, PVDF, PLA, ABS, PTFE.
8. The method of claim 1, wherein the solvent comprises at least one of the following: sodium hydroxide solution, potassium hydroxide solution.
9. The method for preparing a pore size-controllable nanoporous structural element by fused deposition modeling according to claim 1, wherein the fused deposition modeling is printed at a temperature of 0 ℃ to 600 ℃.
10. A pore-controllable nanoporous structural article obtainable by the process according to any one of claims 1 to 9.
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| CN112403121A (en) * | 2020-11-21 | 2021-02-26 | 西安热工研究院有限公司 | Fused deposition modeling 3D printing dioxin removal bag cage and preparation method thereof |
| CN114589919A (en) * | 2020-12-04 | 2022-06-07 | 中国石油化工股份有限公司 | 3D printing equipment |
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| CN114589919A (en) * | 2020-12-04 | 2022-06-07 | 中国石油化工股份有限公司 | 3D printing equipment |
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