CN111117227A - Preparation method of polymer powder material for optical fiber laser sintering - Google Patents
Preparation method of polymer powder material for optical fiber laser sintering Download PDFInfo
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- CN111117227A CN111117227A CN201911403612.4A CN201911403612A CN111117227A CN 111117227 A CN111117227 A CN 111117227A CN 201911403612 A CN201911403612 A CN 201911403612A CN 111117227 A CN111117227 A CN 111117227A
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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
- B33Y70/00—Materials specially adapted for additive manufacturing
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- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention provides a preparation method of a high polymer powder material for optical fiber laser sintering, which comprises the following steps: adding the optical fiber absorbing material and a surfactant into an ethanol-water solution, heating to 30-40 ℃, stirring at the speed of 200-500rpm for 30-120min, performing suction filtration, drying and screening to obtain a surface-activated optical fiber absorbing material; adding polymer powder and a solvent into a reaction kettle, continuously stirring and heating to a set temperature, wherein the set temperature is 5-50 ℃ lower than the starting dissolving temperature of the polymer powder, and keeping the temperature for 30-120 min; adding the surface-activated optical fiber absorption material into a reaction kettle, continuously stirring and preserving heat for 30-180min, finally cooling the solution to room temperature, carrying out suction filtration, drying and screening, and then uniformly mixing with the inorganic nano particles and the powder antioxidant to obtain the polymer powder material for optical fiber laser sintering. The polymer powder material for optical fiber laser sintering provided by the invention has high absorption efficiency on optical fiber energy and good mechanical properties of a workpiece, and is particularly suitable for a selective optical fiber laser sintering process.
Description
Technical Field
The invention relates to the field of additive manufacturing, in particular to a preparation method of a high polymer powder material for optical fiber laser sintering.
Background
Selective laser sintering is a method for manufacturing three-dimensional objects by selectively fusing layers of powder, which allows to obtain a three-dimensional entity without using tooling, by laser sintering only a plurality of superposed layers of powder according to a three-dimensional image of the object to be produced. The process is primarily accomplished using thermoplastic polymers. Patents US6136948 and WO9606881 describe in detail such a method of manufacturing three-dimensional objects using powdered polymers.
The existing mainstream selective laser sintering mainly uses CO with the wavelength of 10.6 microns2The manufacturing accuracy of the laser and the three-dimensional part is related to the size of a laser spot, the smaller the laser spot is, the higher the manufacturing accuracy is, and the size of the laser spot is in direct proportion to the wavelength and the laser modulus. In the manufacture of three-dimensional parts, for finer features, CO is used2Laser sintering tends to be difficult to achieve the desired results. The fiber laser can use smaller laser spots, realizes the manufacturing of polyamide three-dimensional objects by using laser with smaller focusing spots, and improves the manufacturing precision.
The absorption efficiency of the polymer material to the fiber laser is very low due to its physical properties, and in order to improve the absorption of the polymer material to the fiber laser energy, the conventional method is to mix the polymer powder material and the fiber absorption powder material to improve the absorption capacity of the polymer material to the fiber laser. The prior literature adopts a mechanical mixing method to mix the polymer powder material and the optical fiber absorbing material, but the optical fiber absorbing material and the polymer powder material are not firmly adsorbed, and are separated in the transportation, storage and use processes of the material, so that the actual use effect is seriously reduced.
Disclosure of Invention
The invention aims to improve the absorption efficiency and effect of high polymer materials on optical fiber laser energy, improve the stability of the materials in the processes of transportation, storage and use and make the materials more suitable for a selective optical fiber laser sintering molding process.
The invention provides a preparation method of a high polymer powder material for optical fiber laser sintering, which comprises the following steps:
step one, adding the optical fiber absorbing material and a surfactant into an ethanol-water solution, heating to 30-40 ℃, stirring at the speed of 200-500rpm for 30-120min, performing suction filtration, drying and screening to obtain the surface-activated optical fiber absorbing material;
adding the polymer powder and the solvent into a reaction kettle, continuously stirring and heating to a set temperature, wherein the set temperature is 5-50 ℃ lower than the starting dissolving temperature of the polymer powder, and keeping the temperature for 30-120 min;
and step three, adding the surface-activated optical fiber absorption material into the reaction kettle, continuously stirring and preserving heat for 30-180min, finally cooling the solution to room temperature, carrying out suction filtration, drying and screening, and then uniformly mixing with the inorganic nano particles and the powder antioxidant to obtain the polymer powder material for optical fiber laser sintering.
Further preferably, the mass parts of the components in the step one are as follows: 1-100 parts of optical fiber absorbing material, 1-10 parts of surfactant, 100 parts of ethanol in ethanol-water solution, and 5-20 parts of water.
Further preferably, the mass parts of the components in the second and third steps are as follows: 100 parts of polymer powder, 500 parts of solvent 200-500 parts, 0.1-10 parts of surface-activated optical fiber absorption material, 0.1-1 part of inorganic nano-particles and 0.1-2 parts of powder antioxidant.
Further preferably, the optical fiber absorption material is one or more of carbon black, graphite, graphene, carbon nanotubes, carbon fibers, metal powder or metal oxide powder.
Further preferably, the average particle size of the optical fiber absorbing material is not more than 30 μm.
Further preferably, the surfactant is one or more of a silane coupling agent, a titanate coupling agent, an organic acid salt and an organic acid ester.
Further preferably, the polymer powder is one or more of polyamide, polyurethane, polyolefin, polycarbonate, thermoplastic polyester, polystyrene, polyphenylene sulfide, polyether ether copper, polyether ketone and polyformaldehyde.
More preferably, the polymer powder has an average particle diameter of 5 to 200 μm.
Further preferably, the solvent is one or more of N, N-dimethylformamide, N-dimethylacetamide, ethanol, water, propanol, butanol, ethylene glycol, butanone, tetrahydrofuran, dichloromethane, chloroform, formic acid, acetic acid, toluene, xylene, phenol, tetrachloroethane, or α -chloronaphthalene.
Further preferably, the mixing process in the third step is specifically: mixing part of the polymer powder and the powder additive for 1-5min at the rotating speed of 1200-1500r/min to obtain a pre-dispersed powder material; and mixing the pre-dispersed powder material and the rest high molecular powder for 5-180min at the rotating speed of 100-500r/min to obtain the high molecular powder material.
The invention provides a preparation method of a polyamide powder material for optical fiber laser sintering, which has the following beneficial effects:
(1) the polymer powder is heated in the solvent to 5 ℃ below the initial dissolving temperature and is kept warm for a period of time, the surface of the powder particle is in a softened and relaxed state, the surface-activated optical fiber absorption material is added at the moment, the optical fiber absorption material is easier to generate interaction with chemical functional groups on the surface of the powder particle, meanwhile, the polymer material is easier to be embedded into gaps on the surface of the powder particle, in the cooling process, the surface of the powder particle gradually shrinks, and finally, the optical fiber absorption material is attached to the surface of the powder particle to grow into a whole, so that the optical fiber absorption material is firmly and uniformly distributed on the surface of the powder particle, and cannot be separated in the transportation, storage and use processes, and the absorption efficiency and the effect of the polymer powder on optical fiber laser are improved.
(2) The optical fiber material is coated on the surface of the high polymer material and embedded into the gap on the surface of the powder particles, so that the absorption and conduction of the material to the optical fiber energy are improved, and meanwhile, due to the characteristics of the optical fiber material, the optical fiber material can also be used as a component in the material to improve the mechanical property of the material and endow the material with new properties.
(3) The invention does not need to dissolve high molecular powder, does not need high pressure condition, has low requirement on production equipment, can repeatedly recycle the solvent, and has simple and feasible process.
Detailed Description
The present invention is described in further detail below by way of specific examples.
Example 1
4000g of ethanol, 400g of water, 200g of potassium dodecyl phosphate and 200g of 700-mesh carbon black are added into water bath equipment, the temperature is set to be 35 ℃, the stirring speed is 350rpm, the stirring time is 60min, and then the surface activated carbon black is obtained through suction filtration, drying and screening.
Adding 5kg of PA1212 material and 15kg of ethylene glycol into a 20L reaction kettle, heating at a stirring speed of 100rpm to raise the temperature of the material to 110 ℃, preserving the heat for 60min at the temperature, then adding 150g of activated carbon black into the material, preserving the heat for 90min at the temperature of 110 ℃, stopping heating, continuously stirring to reduce the temperature of the material to room temperature, taking out the material, carrying out centrifugal separation, and drying to obtain a PA1212 powder sample.
Taking 1kg of the powder, 16g of fumed silica with the average particle size of 20nm and 30g of hindered phenol antioxidant, putting the powders into a mixing device, mixing for 3min at the rotating speed of 1400rpm, and mixing the pre-dispersed powder and the rest 3kgPA1212 powder for 30min at the rotating speed of 350 rpm.
Comparative example 1
Adding 5kg of PA1212 material and 15kg of ethylene glycol into a 20L reaction kettle, heating at a stirring speed of 100rpm to raise the temperature of the material to 110 ℃, keeping the temperature at the temperature for 150min, stopping heating, continuously stirring to reduce the temperature of the material to room temperature, taking out the material, performing centrifugal separation, and drying to obtain a PA1212 powder sample.
Taking 1kg of the powder, 16g of fumed silica with the average particle size of 20nm and 30g of hindered phenol antioxidant, putting the powders into a mixing device, mixing for 3min at the rotating speed of 1400rpm, and mixing the pre-dispersed powder and the rest 3kgPA1212 powder for 30min at the rotating speed of 350 rpm.
Example 2
4000g of ethanol, 400g of water, 200g of potassium dodecyl phosphate and 400g of 700-mesh carbon fiber powder are added into water bath equipment, the temperature is set to be 35 ℃, the stirring speed is 350rpm, the stirring time is 60min, and then the carbon fiber powder with activated surfaces is obtained through suction filtration, drying and screening.
Adding 5kg of PA1212 material and 15kg of ethylene glycol into a 20L reaction kettle, heating at a stirring speed of 100rpm to raise the temperature of the material to 110 ℃, preserving the heat for 60min at the temperature, then adding 350g of activated carbon fiber powder into the material, preserving the heat for 90min at the temperature of 110 ℃, stopping heating, continuously stirring to reduce the temperature of the material to room temperature, taking out the material, carrying out centrifugal separation, and drying to obtain a PA1212 powder sample.
Taking 1kg of the powder, 16g of fumed silica with the average particle size of 20nm and 30g of hindered phenol antioxidant, putting the powders into a mixing device, mixing for 3min at the rotating speed of 1400rpm, and mixing the pre-dispersed powder and the rest 3kgPA1212 powder for 30min at the rotating speed of 350 rpm.
Example 3
Adding 3000g of ethanol, 300g of water, 102200g of titanate coupling agent and 150g of 700-mesh antimony oxide into water bath equipment, setting the temperature at 35 ℃, the stirring speed at 350rpm, and the stirring time at 60min, and then carrying out suction filtration, drying and screening to obtain the surface-activated carbon fiber powder.
Adding 5kg of PA1212 material and 15kg of ethylene glycol into a 20L reaction kettle, heating at a stirring speed of 100rpm to raise the temperature of the material to 110 ℃, preserving the heat for 60min at the temperature, then adding 100g of activated antimony oxide into the material, preserving the heat for 90min at the temperature of 110 ℃, stopping heating, continuously stirring to reduce the temperature of the material to room temperature, taking out the material, carrying out centrifugal separation, and drying to obtain a PA1212 powder sample.
Taking 1kg of the powder, 16g of fumed silica with the average particle size of 20nm and 30g of hindered phenol antioxidant, putting the powders into a mixing device, mixing for 3min at the rotating speed of 1400rpm, and mixing the pre-dispersed powder and the rest 3kgPA1212 powder for 30min at the rotating speed of 350 rpm.
Example 4
4000g of ethanol, 400g of water, 100g of silane coupling agent KH-570200g and 700-mesh carbon nano tube are added into water bath equipment, the temperature is set to be 35 ℃, the stirring speed is 350rpm, the stirring time is 60min, and then the carbon fiber powder with activated surfaces is obtained through suction filtration, drying and screening.
Adding 5kg of PA1212 material and 15kg of ethylene glycol into a 20L reaction kettle, heating at a stirring speed of 100rpm to raise the temperature of the material to 110 ℃, preserving the heat for 60min at the temperature, then adding 50g of activated carbon nanotubes into the material, preserving the heat for 90min at the temperature of 110 ℃, stopping heating, continuously stirring to reduce the temperature of the material to room temperature, taking out the material, carrying out centrifugal separation, and drying to obtain a PA1212 powder sample.
Taking 1kg of the powder, 16g of fumed silica with the average particle size of 20nm and 30g of hindered phenol antioxidant, putting the powders into a mixing device, mixing for 3min at the rotating speed of 1400rpm, and mixing the pre-dispersed powder and the rest 3kgPA1212 powder for 30min at the rotating speed of 350 rpm.
Example 5
4000g of ethanol, 400g of water, 100g of silane coupling agent KH-570200g and 700-mesh carbon nano tube are added into water bath equipment, the temperature is set to be 35 ℃, the stirring speed is 350rpm, the stirring time is 60min, and then the carbon fiber powder with activated surfaces is obtained through suction filtration, drying and screening.
Adding 5kg of polyurethane material, 10kg of water and 5kg of N, N-dimethylacetamide into a 20L reaction kettle, heating at the stirring speed of 100rpm to raise the temperature of the material to 50 ℃, preserving the heat at the temperature for 60min, then adding 50g of activated carbon nanotubes into the material, preserving the heat at the temperature of 50 ℃ for 60min, stopping heating, continuously stirring to reduce the temperature of the material to room temperature, taking out the material, carrying out centrifugal separation, and drying to obtain a polyurethane powder sample.
Taking 1kg of the powder, 16g of fumed silica with the average particle size of 20nm and 30g of hindered phenol antioxidant, putting the powders into a mixing device, mixing the powders at the rotating speed of 1400rpm for 3min, and mixing the pre-dispersed powder and the rest 3kg of polyurethane powder at the rotating speed of 350rpm for 30 min.
Comparative example 2
Adding 5kg of polyurethane material, 10kg of water and 5kg of N, N-dimethylacetamide into a 20L reaction kettle, heating at the stirring speed of 100rpm to raise the temperature of the material to 50 ℃, preserving the heat at the temperature for 120min, stopping heating, continuously stirring to reduce the temperature of the material to room temperature, taking out the material, centrifugally separating, and drying to obtain a polyurethane powder sample.
Taking 1kg of the powder, 16g of fumed silica with the average particle size of 20nm and 30g of hindered phenol antioxidant, putting the powders into a mixing device, mixing the powders at the rotating speed of 1400rpm for 3min, and mixing the pre-dispersed powder and the rest 3kg of polyurethane powder at the rotating speed of 350rpm for 30 min.
Example 6
4000g of ethanol, 400g of water, KH-570200g of silane coupling agent and 75g of graphene with 700 meshes are added into water bath equipment, the temperature is set to be 35 ℃, the stirring speed is 350rpm, the stirring time is 60min, and then the carbon fiber powder with activated surfaces is obtained through suction filtration, drying and screening.
Adding 5kg of PBT powder, 5kg of phenol and 15kg of tetrachloroethane into a 20L reaction kettle, heating at the stirring speed of 100rpm to raise the temperature of the materials to 100 ℃, preserving the heat for 60min at the temperature, then adding 50g of activated graphene into the materials, preserving the heat for 120min at the temperature of 100 ℃, stopping heating, continuously stirring to reduce the temperature of the materials to room temperature, taking out the materials, carrying out centrifugal separation, and drying to obtain a PBT powder sample.
Taking 1kg of the powder, 16g of fumed silica with the average particle size of 20nm and 30g of hindered phenol antioxidant, putting the powders into a mixing device, mixing for 3min at the rotating speed of 1400rpm, and mixing the pre-dispersed powder and the rest 3kg of PBT powder for 30min at the rotating speed of 350 rpm.
Comparative example 3
Adding 5kg of PBT powder, 5kg of phenol and 15kg of tetrachloroethane into a 20L reaction kettle, heating at the stirring speed of 100rpm to raise the temperature of the materials to 100 ℃, keeping the temperature at the temperature for 180min, stopping heating, continuously stirring to reduce the temperature of the materials to room temperature, taking out the materials, centrifugally separating, and drying to obtain a PBT powder sample.
Taking 1kg of the powder, 16g of fumed silica with the average particle size of 20nm and 30g of hindered phenol antioxidant, putting the powders into a mixing device, mixing for 3min at the rotating speed of 1400rpm, and mixing the pre-dispersed powder and the rest 3kg of PBT powder for 30min at the rotating speed of 350 rpm.
The powder materials prepared in examples 1-6 and comparative examples 1-3 were sintered on a eosinophilia department Flight fiber laser device using a standard material sintering bag, and the mechanical properties of the parts were tested by observing the sintering phenomenon.
The various performance test data are shown in the following table.
As can be seen from the table, the polymer material can effectively absorb the laser energy of the optical fiber after the optical fiber absorbing material is added, and meanwhile, the mechanical property of the material is higher than that of the conventional CO due to the synergistic effect of the material on the absorption of the laser energy of the optical fiber and the optical fiber absorbing material caused by the addition of the absorbent2The performance of the laser sintered product is slightly improved.
Claims (10)
1. A preparation method of a polymer powder material for optical fiber laser sintering is characterized by comprising the following steps:
step one, adding the optical fiber absorbing material and a surfactant into an ethanol-water solution, heating to 30-40 ℃, stirring at the speed of 200-500rpm for 30-120min, performing suction filtration, drying and screening to obtain the surface-activated optical fiber absorbing material;
adding the polymer powder and the solvent into a reaction kettle, continuously stirring and heating to a set temperature, wherein the set temperature is 5-50 ℃ lower than the starting dissolving temperature of the polymer powder, and keeping the temperature for 30-120 min;
and step three, adding the surface-activated optical fiber absorption material into the reaction kettle, continuously stirring and preserving heat for 30-180min, finally cooling the solution to room temperature, carrying out suction filtration, drying and screening, and then uniformly mixing with the inorganic nano particles and the powder antioxidant to obtain the polymer powder material for optical fiber laser sintering.
2. The method for preparing the polymer powder material for optical fiber laser sintering according to claim 1, wherein the first step comprises the following components in parts by weight: 1-100 parts of optical fiber absorbing material, 1-10 parts of surfactant, 100 parts of ethanol in ethanol-water solution, and 5-20 parts of water.
3. The method for preparing the polymer powder material for optical fiber laser sintering according to claim 2, wherein the second and third steps comprise the following components in parts by mass: 100 parts of polymer powder, 500 parts of solvent 200-500 parts, 0.1-10 parts of surface-activated optical fiber absorption material, 0.1-1 part of inorganic nano-particles and 0.1-2 parts of powder antioxidant.
4. The method for preparing the polymer powder material for optical fiber laser sintering according to claim 3, wherein the optical fiber absorption material is one or more of carbon black, graphite, graphene, carbon nanotubes, carbon fibers, metal powder or metal oxide powder.
5. The method of claim 4, wherein the average particle size of the optical fiber absorbing material is not more than 30 μm.
6. The method for preparing the polymer powder material for optical fiber laser sintering according to claim 5, wherein the surfactant is one or more of a silane coupling agent, a titanate coupling agent, an organic acid salt and an organic acid ester.
7. The method for preparing polymer powder material for optical fiber laser sintering according to claim 6, wherein the polymer powder is one or more of polyamide, polyurethane, polyolefin, polycarbonate, thermoplastic polyester, polystyrene, polyphenylene sulfide, polyether ether copper, polyether ketone and polyformaldehyde.
8. The method for preparing a polymer powder material for optical fiber laser sintering according to claim 7, wherein the polymer powder has an average particle diameter of 5 to 200 μm.
9. The method for preparing a polymer powder material for optical fiber laser sintering according to claim 8, wherein the solvent is one or more of N, N-dimethylformamide, N-dimethylacetamide, ethanol, water, propanol, butanol, ethylene glycol, butanone, tetrahydrofuran, dichloromethane, chloroform, formic acid, acetic acid, toluene, xylene, phenol, tetrachloroethane, and α -chloronaphthalene.
10. The method for preparing the polymer powder material for optical fiber laser sintering according to claim 9, wherein the mixing process in the third step is specifically as follows: mixing part of the polymer powder and the powder additive for 1-5min at the rotating speed of 1200-1500r/min to obtain a pre-dispersed powder material; and mixing the pre-dispersed powder material and the rest high molecular powder for 5-180min at the rotating speed of 100-500r/min to obtain the high molecular powder material.
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Cited By (4)
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| CN111995865A (en) * | 2020-07-28 | 2020-11-27 | 湖南华曙高科技有限责任公司 | Polymer material, preparation method thereof and manufacturing method of polymer product |
| CN112123755A (en) * | 2020-07-28 | 2020-12-25 | 湖南华曙高科技有限责任公司 | Metal polymer composite material, preparation method thereof and manufacturing method of metal polymer composite part |
| CN112440472A (en) * | 2020-10-28 | 2021-03-05 | 湖南华曙高科技有限责任公司 | Method for low-temperature sintering of high-molecular composite powder material |
| CN113751704A (en) * | 2021-07-28 | 2021-12-07 | 北京科技大学 | Tungsten alloy for selective laser sintering printing film coating, preparation and printing method |
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