CN104057090A - Method for removing printing metal, ceramic product metal, ceramic powder and polymer mixed material and polymer from finished product - Google Patents
Method for removing printing metal, ceramic product metal, ceramic powder and polymer mixed material and polymer from finished product Download PDFInfo
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Abstract
The invention discloses a method for removing printing metal, ceramic product metal, mixed material of ceramic powder (as a material component) and a polymer adhesive agent and the polymer adhesive agent from a finished printing product. According to the method, the mixed material comprises components in a volume ratio as follows: 40%-70% of material components and 30%-60% of the polymer adhesive agent which comprises components in a mass ratio of 50%-95% of main materials removed at the lower temperature, 4.5%-46% of auxiliary materials removed at the higher temperature and 0.5%-4% of auxiliaries; the mixed material is subjected to mixing and banburying to obtain filaments, pipes, bars, balls and blocks for printing forming; and the finished product obtained by printing is subjected to molten decomposition, water decomposition or acid catalysis at the lower temperature to remove the main polymer adhesive agent, is subjected to molten decomposition at the higher temperature to remove the auxiliary polymer adhesive agent and the auxiliaries, and is sintered to obtain a target product. The printing material has a wide source, is low in price, reduces the cost greatly and facilitates development of 3D (three-dimensional) manufacture.
Description
Technical field
The present invention relates to a kind ofly with three-dimensional printing technology, print metal, pottery and multiple (mix) closes powder and high polymer binder mixing material product, then through removing high polymer binder, sintering, the manufacture method of acquisition metal, pottery and composite goods thereof.
Background technology
3 D-printing (3D manufacture) is the most popular current new manufacture, someone think its importance not second to personal computer in 1977 and nineteen ninety web browser, be called as the industrial revolution for the third time.Because it does not need mould, be mainly applicable to the quick manufacture of small lot (even single-piece), complex-shaped product.Its core technology mainly concentrates on equipment and two aspects of material.The material using at present mainly contains photo-curable ABS resinoid, land plaster and binding agent thereof, for laser sintered metal dust (kind seldom).ABS resinoid, land plaster goods, can only be as concept and adornment, and industry and life practical value are little, laser sintered metal dust, and a few is applicable also to only have titanium alloy etc.; Above-mentioned expensive for the material price of printing.These factors have all limited fast development and industrialization process that 3D manufactures.
So the 3D manufactured materials that exploitation is generally suitable for and material source is wide, price is low, is the importance that 3D manufactures development.
Summary of the invention
Metal of the present invention, pottery and multiple (mix) thereof are closed powder and high polymer binder mixing material, comprise metal, pottery and answer (mixing) and close the material system of powder and the adhesive composition two class materials of two or more high polymer binder composition.
In any mixing material, adopt which kind of metal, pottery and multiple (mix) thereof to close powder, by the material decision (hereinafter referred to as material component) of the target product regulation of manufacturing.Comprise: the mixture of a kind of metal dust or various metals powder, such as the mixture of iron powder, cobalt powder, molybdenum powder, chromium powder, niobium powder, nickel powder, manganese powder, tungsten powder, copper powder, aluminium powder etc. and two or more different proportion powder thereof; The alloy powder of various metals, such as powder of stainless steel, the low-alloy powder of the different trades mark; Ceramic powders, comprising: oxide ceramics, and such as zirconia, aluminium oxide etc., nitride ceramics, such as silicon nitride, aluminium nitride etc., carbide ceramics, such as carborundum etc.; Multiple (mixing) condensation material of cermet, such as iron plating aluminium oxide, iron plating zirconia, nickel plating aluminium oxide, nickel plating zirconia etc.
Selected high polymer binder, according to the difference of removal methods, is divided into following three classes:
Two kinds and two or more macromolecular material of the different meltings that, can remove by heating, decomposition temperature, can be wherein main component what remove compared with low melt decomposition temperature, in higher fusion and decomposition temperature, remove for auxiliary element, and the auxiliary component such as dispersant, plasticizer.
The described main component high polymer binder removing compared with low melt decomposition temperature comprises: one or more compositions of paraffin, Brazil wax, polyformaldehyde, ethylene ethyl acrylate, ethylene-vinyl acetate copolymer, SAN resin, ABS resin etc.
The described auxiliary element high polymer binder removing in higher fusion and decomposition temperature comprises: the TPO materials such as polyethylene (PE), polypropylene (PP), polyvinyl butyral, polybutylene terephthalate (PBT), PETG, polystyrene, nylon etc.
The auxiliary agents such as described dispersant, plasticizer comprise: stearic acid, polyisobutene, PIBA, polyisobutenyl succimide, Tissuemat E, polypropylene wax etc.
Two, can remove main component in lower temperature hydrolysis, then remove auxiliary element through higher temperature heat, and the auxiliary agent such as dispersant, plasticizer forms minute.
The main component macromolecular material that described lower temperature hydrolysis removes comprises: caprolactam (CPL), polybutylene terephthalate (PBT) (PBT), polyethyleneglycol diacrylate, DPG first mystery acetate, 2-Pyrrolidone, polybutylene terephthalate (PBT) etc., the kinds such as preferred caprolactam (CPL), polybutylene terephthalate (PBT) (PBT).
The auxiliary element macromolecular material that described higher fusion and decomposition temperature removes comprises: the TPO materials such as polyethylene (PE), polypropylene (PP), polyvinyl butyral, polybutylene terephthalate (PBT), PETG, polystyrene, nylon etc., the kinds such as preferably polyethylene (PE), polypropylene (PP).
The auxiliary agents such as described dispersant, plasticizer comprise: stearic acid, polyisobutene, PIBA, polyisobutenyl succimide Tissuemat E, polypropylene wax etc.
Three, acid catalysis removes main component at a lower temperature, then removes auxiliary element through higher temperature fusion and decomposition, and the auxiliary agent such as dispersant, plasticizer forms minute.
The main component macromolecular material that described acid catalysis at a lower temperature removes comprises: polyformaldehyde, PETG, ethyl cellulose, acetate fiber, hydroxypropyl cellulose, collodion cotton, ethene-butylene cellulose etc.
The described auxiliary element macromolecular material removing in higher fusion and decomposition temperature comprises: the TPO materials such as polyethylene (PE), polypropylene (PP), polyvinyl butyral, polybutylene terephthalate (PBT), PETG, polystyrene, nylon etc., the kinds such as preferably polyethylene (PE), polypropylene (PP).
The auxiliary agents such as described dispersant, plasticizer comprise: stearic acid, polyisobutene, PIBA, polyisobutenyl succimide Tissuemat E, polypropylene wax etc.
In mixing material of the present invention, the volume of material component and macromolecular material system component forms: material component accounts for 40-70%, and high polymer binder system component accounts for 60-30%.
In high polymer binder system component of the present invention, by mass percentage, the macromolecular material of main component accounts for 50-95%; The macromolecular material of auxiliary element accounts for 46-4.5%; The auxiliary agent such as dispersant, plasticizer accounts for 4-0.5%.
The mixing method of mixing material of the present invention is: first by auxiliary dispersants, plasticizer, the macromolecular material of auxiliary element and the mixing of material component are extremely even, then adds the macromolecular material mixing of main component to even.
Mixing equipment is common on the market mixer, kneader, banbury, screw extruder, spiral filament forming machine, forming machine etc.
A kind of for printing the preparation method of the high polymer binder of metal, ceramic and metal, ceramic powders mixing material, it is characterized in that, processing step comprises as follows: 1. first by high polymer binder system component mass ratio, the macromolecular material of the auxiliary element of 46-4.5% will be accounted for, account for 4-0.5% auxiliary material dispersant, plasticizer, mix with the material component that accounts for volume ratio 40-70%, 110-275 ℃ of banburying to evenly; 2. press high polymer binder system component mass ratio, 1. the macromolecular material that accounts for the main component of 50-95% added, 60-230 ℃ of banburying to evenly; 3. the uniform mixing material of banburying is extruded in screw extruder; 4. according to the difference of 3D printer, by mixing forming materials, be silk (line) shape, bar-shaped, tubulose, particle, cylindrical or rectangle etc.
The invention is characterized in, by after the moulding of mixing file printing, need, according to the difference of high polymer binder system, take the different process such as heat fusing decomposition, hydrolysis, acid catalysis, high polymer binder in printing shaping product is removed, then obtain final manufactured goods through sintering.The equipment that removes high polymer binder can adopt vacuum drying oven, heating furnace, and agglomerating plant can adopt vacuum drying oven, steel (net) band sintering furnace, push rod sintering furnace etc.Taking off and sintering can carry out continuously in same equipment, also can in distinct device, separately carry out.
Removing main and auxiliary high polymer binder and sintering comprises the steps:
1. remove the main component macromolecular material of fusion and decomposition, hydrolysis, acid catalyzed decomposition at a lower temperature.Be divided three classes:
1. remove the main component macromolecular material of fusion and decomposition at a lower temperature, this temperature range is 145-280 ℃, and the time of removing is 8-16 hour;
2. remove the main component macromolecular material of hydrolysis at a lower temperature, this temperature range is 100-200 ℃, and the time of removing is 2-10 hour;
3. remove the main component macromolecular material of acid catalyzed decomposition at a lower temperature, this temperature range is 100-200 ℃, and the time of removing is 2-8 hour.
2. remove the auxiliary element macromolecular material that heat fusing decomposes under higher temperature.This temperature range is 280-500 ℃, and the time of removing is 2-7 hour.
3. sintering.Sintering carries out under higher temperature, concrete sintering temperature, time, according to the material component materials of institute's sintering, determines.
Embodiment
Embodiment mono-
Print and manufacture iron-based goods.Material material carbonyl iron dust and fusion and decomposition high polymer binder system combinations mixing material.The carbonyl iron dust of volume ratio 60%, high polymer binder system combinations volume accounts for 40%, wherein: the polypropylene of mass ratio 7%, 3% Tissuemat E, in mixer, premix is 1 hour, puts into kneader and mediates 1 hour at 230 ℃, evenly put into the ABS resin of high polymer binder system combinations mass ratio 90%, at 220 ℃, mediate 1 hour, discharging proceeds to banbury banburying 0.5 hour at 220 ℃, obtains mixing material; Again mixing material is proceeded to extruder, extrude the mixing material silk of diameter 1.75mm, cooling coiling is standby; The silk of reeling is printed to the goods that obtain designing in advance for hot melt 3D; Goods are put into vacuum drying oven, at 280 ℃, remove 8 hours, remove the main component macromolecular material of fusion and decomposition at a lower temperature, at 460 ℃, remove 5 hours, remove the auxiliary element macromolecular material that heat fusing decomposes under higher temperature; The sintering that heats up in vacuum drying oven is incubated 6 hours at 1250 ℃, is cooled to normal temperature, obtains printing pure iron based articles.
Embodiment bis-
Print and manufacture stainless steel products.Material material 316L powder of stainless steel and acid catalysis remove the high polymer binder system combinations mixing material of main component.The 316L powder of stainless steel of volume ratio 65%, high polymer binder system combinations volume accounts for 35%, wherein: the low density polyethylene (LDPE) of mass ratio 5%, 3% PIBA premix 1 hour in mixer, put into kneader and mediate 1 hour at 220 ℃, evenly put into high polymer binder system combinations mass ratio 92% PETG, at 160 ℃, mediate 1 hour, discharging proceeds to banbury banburying 0.5 hour at 165 ℃, obtains mixing material; Again mixing material is proceeded to extruder, extrude the mixing material silk of diameter 3mm, cooling coiling is standby; The silk of reeling is printed to the goods that obtain designing in advance for hot melt 3D; Goods are put into acid catalysis and remove stove, under the catalysis of 180 ℃ of nitric acid mists, remove 3 hours, remove the main component macromolecular material in acid catalyzed decomposition, at 480 ℃, remove 5 hours, remove the auxiliary element macromolecular material that heat fusing decomposes under higher temperature; The goods that remove after high polymer binder are sent into sintering in continuous fritting furnace with guipure, and at 1360 ℃, sintering is 8 hours, obtains printing stainless steel products.
Embodiment tri-
Print and manufacture ceramic.Material material oxidation zirconium powder end and hydrolysis remove the high polymer binder system combinations mixing material of main component.The Zirconium oxide powder of volume ratio 58%, high polymer binder system combinations volume accounts for 42%, wherein: the low density polyethylene (LDPE) of mass ratio 8%, 3% polyisobutene premix 1 hour in mixer, put into kneader and mediate 1 hour at 220 ℃, evenly put into high polymer binder system combinations mass ratio 89% caprolactam, at 80 ℃, mediate 1 hour, discharging proceeds to banbury banburying 0.5 hour at 85 ℃, obtains mixing material; Again mixing material is proceeded to extruder, extrude the mixing material silk of diameter 1.75mm, cooling coiling is standby; The silk of reeling is printed to the goods that obtain designing in advance for hot melt 3D; Goods are put into hydrolysis and remove stove, at 150 ℃, import water vapour and remove 4 hours, remove the main component macromolecular material of hydrolysis, at 480 ℃, remove 5 hours, remove the auxiliary element macromolecular material that heat fusing decomposes under higher temperature; The goods that remove after high polymer binder are sent into sintering in push pedal sintering furnace, and at 1500 ℃, sintering is 6 hours, obtains printing zircite product.
Embodiment tetra-
Print and manufacture low-alloy goods.The high polymer binder system combinations mixing material of material material Fe4Ni powder and fusion and decomposition.Carbonyl iron dust, the carbonyl nickel powder of the Fe4Ni(mass ratio 96:4 of volume ratio 59%) powder, high polymer binder system combinations volume accounts for 41%, wherein: the low density polyethylene (LDPE) of mass ratio 8%, 3% polypropylene wax premix 1 hour in mixer, put into kneader and mediate 1 hour at 220 ℃, evenly put into high polymer binder system combinations mass ratio 89% polyformaldehyde, at 160 ℃, mediate 1 hour, discharging proceeds to banbury banburying 0.5 hour at 165 ℃, obtains mixing material; Again mixing material is proceeded to extruder, extrude the mixing material silk of diameter 3mm, cooling coiling is standby; The silk of reeling is printed to the goods that obtain designing in advance for hot melt 3D; Goods are put into 180 ℃, vacuum removal stove and remove 6 hours, remove the main component macromolecular material in lower temperature fusion and decomposition, at 500 ℃, remove 4 hours, remove the auxiliary element macromolecular material that heat fusing decomposes under higher temperature; The goods that remove after high polymer binder are sent into sintering in continuous fritting furnace with guipure, and at 1260 ℃, sintering is 8 hours, obtains printing alloy product.
Claims (11)
1. one kind supplies to print metal, the pottery of metal, ceramic and mixing material and the removal methods of high polymer binder in printing shaping product that (mixing) closes powder (material material) and high polymer binder again thereof
.
2. mixing material described in claim 1, metal, pottery and multiple (mixing) thereof are closed powder (material material) volume ratio and are accounted for 40-70%, and high polymer binder volume accounts for 60-30%.
3. described in claim 2, volume ratio accounts for 40-70% metal, pottery and multiple (mixing) thereof are closed powder kind, the material of being stipulated by the target product of manufacturing determines, comprise: the mixture of a kind of metal dust or various metals powder, such as the mixture of iron powder, cobalt powder, molybdenum powder, chromium powder, niobium powder, nickel powder, manganese powder, tungsten powder, copper powder, aluminium powder etc. and two or more different proportion powder thereof; The alloy powder of various metals, such as powder of stainless steel, the low-alloy powder of the different trades mark; Ceramic powders, comprising: oxide ceramics, and such as zirconia, aluminium oxide etc., nitride ceramics, such as silicon nitride, aluminium nitride etc., carbide ceramics, such as carborundum etc.; Multiple (mixing) condensation material of cermet, such as iron plating aluminium oxide, iron plating zirconia, nickel plating aluminium oxide, nickel plating zirconia etc.
4. described in claim 2, volume ratio accounts for the binding agent of 60-30%, main high polymer binder by accounting for binding agent mass percent 50-95% and removing in lower temperature fusion and decomposition or water decomposition or acid catalysis, accounts for the assistant high molecular binding agent that binding agent mass percent 46-4.5% removes in higher temperature fusion and decomposition; The auxiliary material such as dispersant, plasticizer that account for binding agent mass percent 4-0.5% form.
5. described in claim 4, account for the main high polymer binder that binding agent mass percent 50-95% removes at lower temperature, be divided three classes:
1. the main high polymer binder removing in lower temperature fusion and decomposition, comprises one or more compositions of paraffin, Brazil wax, polyformaldehyde, ethylene ethyl acrylate, ethylene-vinyl acetate copolymer, SAN resin, ABS resin etc.;
2. the main high polymer binder removing in lower temperature hydrolysis, comprise caprolactam (CPL), polybutylene terephthalate (PBT) (PBT), polyethyleneglycol diacrylate, DPG first mystery acetate, 2-Pyrrolidone, polybutylene terephthalate (PBT) etc., the kinds such as preferred caprolactam (CPL), polybutylene terephthalate (PBT) (PBT);
3. the main high polymer binder removing in lower temperature acid catalysis comprises: polyformaldehyde, PETG, ethyl cellulose, acetate fiber, hydroxypropyl cellulose, collodion cotton, ethene-butylene cellulose etc.
6. described in claim 4, account for the assistant high molecular binding agent that binding agent mass percent 46-4.5% removes in higher temperature fusion and decomposition, comprise the TPO materials such as polyethylene (PE), polypropylene (PP), one or more compositions of polyvinyl butyral, polybutylene terephthalate (PBT), PETG, polystyrene, nylon etc.
7. described in claim 4, account for binding agent mass percent 4-0.5% dispersant, plasticizer auxiliary material, comprise stearic acid, polyisobutene, PIBA, polyisobutenyl succimide Tissuemat E, polypropylene wax etc.
8. a kind of by metal described in claim 1, pottery and multiple (mixing) thereof are closed the mixing material of powder and high polymer binder two class materials compositions, be characterised in that for printing shaping product are not collapsed because removing of high polymer binder is inhomogeneous in removing the process of macromolecular material, guarantee the complete and even intensity of goods, when producing mixing material, the assistant high molecular binding agent first fusion and decomposition under higher temperature being removed, auxiliary agent mixes with material material, mediate and banburying, be added in again the main high polymer binder banburying that lower temperature fusion and decomposition or water decomposition or acid catalysis remove, be shaped to silk (line) shape, bar-shaped, tubulose, particle, cylindrical or rectangle etc., for 3D, print.
9. described in claim 1 after the moulding of mixing file printing, need remove the contained high polymer binder of products formed, the high polymer binder analyte that removes is recyclable, condensation, extraction and application, environmental friendliness.
10. mixing file printing products formed described in claim 1, when three dimensional design, must consider to remove the contraction after high polymer binder, amplifies the size of printing shaping product by shrinkage rates.
Described in 11. claims 1, mixing file printing products formed, is characterised in that and removes after high polymer binder, need carry out sintering according to the performance of material material, makes it reach the performance requirement of target product regulation material material.
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