Summary of the invention
Main purpose of the present invention is for the deficiencies in the prior art, a kind of Feedstock of Powder Injection Molding preparation method and powder injection-molded production method are provided, the feeding preparing gained is used for powder injection-molded production, degreasing efficiency is higher, skimming processes is simple and easy to control, and skimming processes can not impact green body quality, and clean environment firendly.
For achieving the above object, the present invention is by the following technical solutions:
A kind of Feedstock of Powder Injection Molding preparation method, comprising:
The moulding powder calculating 80 ~ 94%, preferably 85 ~ 94% is by mass percentage put in banbury and carries out agitating heating, when powder is heated to 180 ~ 200 DEG C, add the binder component calculating 6 ~ 20%, preferably 6 ~ 15% by mass percentage, stirring 60 ~ 120min is continued according to melting temperature 175 ~ 195 DEG C, preferred banbury rotating speed 10 ~ 30 turns/min, obtains mixing uniform feeding;
Wherein said binding agent comprises the following component calculated by mass percentage: the atoleine of 5 ~ 10%, the naphthalene of 5 ~ 15%, 15 ~ 20% solid paraffin, 10 ~ 20% microwax, 15 ~ 20% Brazil wax, first high molecular polymer of 15 ~ 30%, second high molecular polymer of 10 ~ 20% and 1 ~ 5% surfactant, wherein said first high molecular polymer and described second high molecular polymer be selected from polyethylene, polypropylene, polyacrylate, acrylonitrile-butadiene-styrene copolymer any two.
Preferably:
Described surfactant is stearic acid, oleic acid, calcium stearate or dolomol, and described moulding powder is metal dust or ceramic powders.
Described method also comprises described mixing uniform feeding is obtained particle feeding by comminutor.
By quality proportioning, described moulding powder is the metal dust of 9.1kg, and described binding agent comprises atoleine 45g, stearic acid 45g, naphthalene 90g, solid paraffin 135g, microwax 180g, Brazil wax 90g, polyethylene 180g, polypropylene 135g.
Further, first described metal dust is dropped into agitating heating in banbury, when being heated to 190 DEG C, add described binding agent again, continue to stir 90min according to melting temperature 180 DEG C, rotating speed 15 turns/min, obtain described mixing uniform feeding.
By quality proportioning, described moulding powder is the zirconia ceramics powder of 8.5kg, and described binding agent comprises atoleine 75g, stearic acid 45g, naphthalene 225g, solid paraffin 225g, microwax 180g, Brazil wax 225g, polyethylene 375g, polypropylene 150g.
Further, first described zirconia ceramics powder is dropped into agitating heating in banbury, when being heated to 200 DEG C, add described binding agent again, continue to stir 120min according to melting temperature 190 DEG C, rotating speed 10 turns/min, obtain described mixing uniform feeding.
By quality proportioning, described moulding powder is the metal dust of 8.8kg, and described binding agent comprises atoleine 120g, stearic acid 12g, naphthalene 60g, solid paraffin 180g, microwax 168g, Brazil wax 240g, polyethylene 180g, polypropylene 240g.
Further, first described metal dust is dropped into agitating heating in banbury, when being heated to 200 DEG C, add described binding agent again, continue to stir 60min according to melting temperature 175 DEG C, rotating speed 30 turns/min, obtain described mixing uniform feeding.
On the other hand, a kind of powder injection-molded production method, comprising:
Injection moulding: by injection machine, the feeding prepared by described Feedstock of Powder Injection Molding preparation method is filled with die cavity through pressure effect, obtains green compact;
Degreasing sintered: sintering furnace put into by green compact injection moulding obtained, be preferably warming up to proper temperature to remove binding agent with 2 ~ 5 DEG C/min programming rate, and then be warming up to material sintering temperature and realize blank Densification, obtain finished product.
Another aspect, a kind of powder injection-molded production method, comprising:
Feedstock preparation: the moulding powder calculating 80 ~ 94%, preferably 85 ~ 94% is by mass percentage put into agitating heating in banbury, add the binder component calculating 6 ~ 20%, preferably 6 ~ 15% by mass percentage, according to melting temperature 175 ~ 195 DEG C of mixing 60 ~ 120min, obtain mixing uniform feeding;
Wherein said binding agent comprises the following component calculated by mass percentage: the atoleine of 5 ~ 10%, the naphthalene of 5 ~ 15%, 15 ~ 20% solid paraffin, 10 ~ 20% microwax, 15 ~ 20% Brazil wax, first high molecular polymer of 15 ~ 30%, second high molecular polymer of 10 ~ 20% and 1 ~ 5% surfactant, wherein said first high molecular polymer and described second high molecular polymer be selected from polyethylene, polypropylene, polyacrylate, acrylonitrile-butadiene-styrene copolymer any two;
Injection moulding: by injection machine, feeding is filled with die cavity through pressure effect, obtains green compact;
Degreasing sintered: injection moulding to be obtained green compact and puts into sintering furnace, be warming up to proper temperature to remove binding agent with 2 ~ 5 DEG C/min programming rate, and then be warming up to material sintering temperature and realize blank Densification, obtain finished product.
Preferably:
Described surfactant is stearic acid, oleic acid, calcium stearate or dolomol, and described moulding powder is metal dust or ceramic powders.
Described method comprises and before the injection molding described mixing uniform feeding is obtained particle feeding by comminutor.
By quality proportioning, described moulding powder is the metal dust of 9.1kg, and described binding agent comprises atoleine 45g, stearic acid 45g, naphthalene 90g, solid paraffin 135g, microwax 180g, Brazil wax 90g, polyethylene 180g, polypropylene 135g.
Further, in the step of described feedstock preparation, first described metal dust is dropped into agitating heating in banbury, when being heated to 190 DEG C, add described binding agent again, continue to stir 90min according to melting temperature 180 DEG C, rotating speed 15 turns/min, obtain described mixing uniform feeding;
In described degreasing sintered step: vacuumize in sintering furnace and pass into protective atmosphere, rise to 600 DEG C with 5 DEG C/min programming rate, and then be warming up to 1380 DEG C with 10 DEG C/min and hold warm 120min.
By quality proportioning, described moulding powder is the metal dust of 8.8kg, and described binding agent comprises atoleine 120g, stearic acid 12g, naphthalene 60g, solid paraffin 180g, microwax 168g, Brazil wax 240g, polyethylene 180g, polypropylene 240g.
Further, in the step of described feedstock preparation, first described metal dust is dropped into agitating heating in banbury, when being heated to 195 DEG C, add described binding agent again, continue to stir 60min according to melting temperature 175 DEG C, rotating speed 30 turns/min, obtain described mixing uniform feeding;
In described degreasing sintered step: vacuumize in sintering furnace and pass into protective atmosphere, rise to 600 DEG C with 3.5 DEG C/min programming rate, and then be warming up to 1320 DEG C with 10 DEG C/min and hold warm 120min.
Beneficial effect of the present invention:
(1) Feedstock of Powder Injection Molding preparation method of the present invention is to the component of the material adopting different cracking temperature in binding agent, particularly low temperature pyrolyzer, adopt wax and the naphthalene of various different temperatures cracking, and each component is through adaptation.The feeding of gained being thus molded into green compact, by adopting suitable heating rate can realize progressively removing of the variety classes material of binding agent, thus realizing removing binding agent quickly through thermal decomposition form.Binding agent removes the time and can control all to remove in several hours clean.Comprise the component of multiple cracking temperature in binding agent, and content proportioning is effective, can takes off, without the need to prior solvent degreasing process by means of only heat.Whole skimming processes is simple and easy to control, and degreasing efficiency is also higher.
(2) gained feeding is used to carry out injection moulding, skimming processes is by controlling heating rate, the component of different cracking temperature is progressively decomposed in an orderly manner, unlikelyly produces a large amount of cracking volatilization gas instantaneously and occur the phenomenon that volume sharply expands, thus unlikely generation bulge defect in base substrate.Due to without the need to solvent removal process, therefore base substrate also can not produce swelling.Whole skimming processes is guaranteed to green body quality.
(3) injection moulding obtains in green compact, and binding agent can directly be removed by thermal decomposition form, does not need the acid catalyst to environmental effects, does not also need toxic solvent to carry out dissolving to component in binding agent and removes, clean environment firendly.
(4) obtained green compact directly can enter sintering furnace, realize degreasing and sinter completing in same equipment, reduce solvent degreasing to thermal debinding process, and degreasing is to the carrying of sintering process, thus the injury that minimizing green compact cause in handling process, catalysis degreasing green compact of comparing especially are easy especially to be produced bad in transportation.
(5) powder injection-molded production method of the present invention eliminates pre-degreasing process, simplifies powder injection forming production technology, saves the required pre-degreasing equipment of powder injection forming simultaneously;
Preferred embodiment can obtain more advantages, such as among feedstock preparation process, first moulding powder is carried out the feeding melting temperature 5 ~ 10 DEG C be heated above subsequently, can guarantee that binding agent adds the mixing initial stage temperature of rear guarantee, make binding agent rapid melting, reduce binding agent mixing process and cause macromolecular substances mechanical breaking in binding agent due to temperature deficiency, cause Binder Properties to decline.
Detailed description of the invention
Below embodiments of the present invention are elaborated.It is emphasized that following explanation is only exemplary, instead of in order to limit the scope of the invention and apply.
According to various embodiments of the present invention, Feedstock of Powder Injection Molding is preparation method comprise: put in banbury by the moulding powder calculating 85 ~ 94% by mass percentage and carry out agitating heating, when powder is heated to 180 ~ 200 DEG C, add the binder component calculating 6 ~ 15% by mass percentage, pressure banbury pressure head, according to banbury rotating speed 10 ~ 30 turns/min, melting temperature 175 ~ 195 DEG C continues stirring 60 ~ 120min, obtain mixing uniform feeding, preferably, described mixing uniform feeding is also obtained particle feeding by comminutor by described method further.Wherein, described binding agent comprises the following component calculated by mass percentage: the atoleine of 5 ~ 10%, the naphthalene of 5 ~ 15%, 15 ~ 20% solid paraffin, 10 ~ 20% microwax, 15 ~ 20% Brazil wax, first high molecular polymer of 15 ~ 30%, second high molecular polymer of 10 ~ 20% and 1 ~ 5% surfactant, wherein said first high molecular polymer and described second high molecular polymer be selected from polyethylene, polypropylene, polyacrylate, acrylonitrile-butadiene-styrene copolymer any two.Described surfactant can be stearic acid, oleic acid, calcium stearate or dolomol.Described moulding powder can be metal dust or ceramic powders.
The present invention proposes a kind of Feedstock of Powder Injection Molding preparation method obtaining injection moulding feeding based on brand-new binder component and powder banburying.For the wax-based binder that conventional method uses, the wax content as wherein more (more than 60%), then generally first need pass through solvent degreasing, just removes all the other components by hot decylization joint after utilizing dissolution with solvents waxy component.Otherwise take off as directly carried out heat, a large amount of wax material moment cracking volatilizations, causes green compact to occur bulge defect a large amount of for generation gas.When this is also existing binding agent degreasing, after solvent degreasing, first just carry out the reason of thermal debinding.The present invention adopts the binding agent improving waxy component to carry out shaping feeding making, adopt the wax of various different cracking temperature, and each waxy component is uniformly distributed as far as possible, utilize and produce Feedstock of Powder Injection Molding as auxiliary agent, in injection molding technique, coordinate the control of heating rate, progressively heat is de-in order to realize shaping green compact, thus solvent degreasing link can be omitted, and the defect of the volumetric expansion of unlikely generation base substrate, bulge.
In binder component, select the many kinds of substance that cracking temperature is different, the cracking temperature of such as naphthalene is at 200 ~ 250 DEG C, the cracking temperature of atoleine is at 230 ~ 270 DEG C, the cracking temperature of solid paraffin is at 250 ~ 300 DEG C, the cracking temperature of microwax is at 280 ~ 320 DEG C, the cracking temperature of Brazil wax is at 250 ~ 350 DEG C, polymer is Pintsch process material, and also select the polymer of two kinds of different cracking temperatures, the component of each material is as far as possible dispersed simultaneously opens, thus during hot decylization joint, by controlling heating rate, heat up with a constant programming rate (2 ~ 5 DEG C/min), thus when reaching different temperatures, the cracking volatilization at different temperatures of each component, each component is progressively decomposed in an orderly manner, and all unlikelyly in decomposable process produce a large amount of cracking volatilization gas instantaneously and occur the phenomenon that volume sharply expands, thus also can not produce bubbly defect by means of only the degreasing of thermal debinding process.This binding agent, can remove totally by means of only heat is de-, degreasing process is simple and easy to control, and 120 ~ 300min gets final product complete degreasing, and degreasing efficiency is also higher.Whole skimming processes can not impact green body quality, and clean environment firendly.
It should be noted that, the selection of said components and the design of content thereof are one of emphasis of the inventive method.Cracking temperature due to component each in binding agent is not all determined value, specifically uncontrollable in which temperature cracking, as a certain constituent content large percentage, such as microwax content is bigger than normal, when may appear at 300 DEG C all there is cracking in microwax and Brazil wax, will produce a large amount of gas like this and finally cause bubbly defect.Therefore, as improper in constituent content design, then the temperature affecting the de-process of heat controls, the final quality affecting the de-efficiency of heat and the de-rear product of heat.The binding agent that the present invention uses relates to the selection of component, the collocation of content, the adjustment of temperature-rise period, degreasing efficiency and product quality, and front and back correlate affects, and finally determines the binding agent of said components and content, have significant advantage through large quantity research.
Example 1
Take 1000 order 9.1kg316L metal dusts; add in banbury and carry out stirring and heating; be heated to 190 DEG C; add binder component: atoleine 45g; stearic acid 45g, naphthalene 90g, solid paraffin 135g; microwax 180g; Brazil wax 90g, polyethylene 180g, polypropylene 135g; then banbury pressure head is depressed; melting temperature 180 DEG C is set, rotor speed 15 turns/min, after continuing to stir 90min; feeding will be mixed take out, be made for injection molding feeding by dual-screw pelletizer.
316L metal feedstock is injected into through forming machine the green part sample that thickness is 2mm.Directly put into powder metallurgy vacuum sintering furnace, when heat is de-, controls in-furnace temperature and be warming up to 600 DEG C from room temperature with programming rate 2.5 DEG C/min.When heating up with this speed, volumetric expansion and bubbling phenomenon in green part, can not be produced, and can remove clean when being warming up to 600 DEG C completely.Then be directly warming up to 1380 DEG C and hold warm 180min, being met performance requirement finished product.
Example 2
Take the zirconia ceramics powder that 8.5kg diameter is 50nm; add in banbury and carry out stirring and heating; be heated to 200 DEG C; add binder component: atoleine 75g; stearic acid 45g, naphthalene 225g, solid paraffin 225g; microwax 180g; Brazil wax 225g, polyethylene 375g, polypropylene 150g; then banbury pressure head is depressed; melting temperature 190 DEG C is set, rotor speed 10 turns/min, after continuing to stir 120min; feeding will be mixed take out, be made for injection molding feeding by singe screw comminutor.
Zirconia ceramics feeding is injected into through forming machine the green part sample that thickness is 2mm.Directly put into ceramic air sintering furnace, when heat is de-under nitrogen atmosphere protection, controls in-furnace temperature and be warming up to 600 DEG C from room temperature with programming rate 3.5 DEG C/min.When heating up with this speed, volumetric expansion and bubbling phenomenon in green part, can not be produced, and can remove clean when being warming up to 600 DEG C completely.Then be directly warming up to 1450 DEG C and hold warm 180min, being met performance requirement finished product.
Example 3
Take 1000 order 8.8kg 17-4PH metal dusts; add in banbury and carry out stirring and heating; be heated to 195 DEG C; add binder component: atoleine 120g; stearic acid 12g, naphthalene 60g, solid paraffin 180g; microwax 168g; Brazil wax 240g, polyethylene 180g, polypropylene 240g; then banbury pressure head is depressed; melting temperature 175 DEG C is set, rotor speed 30 turns/min, after continuing to stir 60min; feeding will be mixed take out, be made for injection molding feeding by dual-screw pelletizer.
316L metal feedstock is injected into through forming machine the green part sample that thickness is 2mm.Directly put into powder metallurgy vacuum sintering furnace, when heat is de-, controls in-furnace temperature and be warming up to 600 DEG C from room temperature with programming rate 5 DEG C/min.When heating up with this speed, volumetric expansion and bubbling phenomenon in green part, can not be produced, can remove clean when being warming up to 600 DEG C completely.Then be directly warming up to 1320 DEG C and hold warm 120min, being met performance requirement finished product.
Comparative example 1:
The binding agent used in feedstock preparation method comprises the solid paraffin of 20%, the microwax of 25%, the Brazil wax of 15%, the polyethylene of 20%, the polypropylene of 15%, the stearic acid of 5%.Said components content is all in mass fraction.The binding agent used relative to embodiment lacks atoleine and naphthalene component.
Above-mentioned binding agent and metal dust (316 powder) are mixed with feeding, are injected into the green part sample that thickness is 2mm.When heat is de-, through repeatedly testing, only can with programming rate 0.4 DEG C/min from room temperature to 600 DEG C, ability is unlikely produces volumetric expansion and bubbling phenomenon in green part, and can remove clean completely.After heat is de-, is directly in stove, be warming up to sintering temperature (1380 DEG C) with 5 DEG C/min to sinter equally, cools to room temperature with the furnace after insulation 2H, obtain product.
Also namely above-mentioned binding agent is the fastest de-with 0.4 DEG C/min intensification heat, and the shortest 1500min could remove completely totally and guarantee that heat takes off does not affect green part quality.Whole debinding rate is too slow, discontented sufficient actual application value.
Comparative example 2:
The binding agent used in feedstock preparation method comprises the naphthalene of 20%, the microwax of 25%, the Brazil wax of 15%, the polyethylene of 20%, the polypropylene of 15%, the stearic acid of 5%.Said components content is all in mass fraction.The binding agent used relative to embodiment lacks atoleine and solid paraffin component.
Above-mentioned binding agent and metal dust (316 powder) are mixed with feeding, are injected into the green part sample that thickness is 2mm.When heat is de-, through repeatedly testing, only can with programming rate 0.5 DEG C/min from room temperature to 600 DEG C, ability is unlikely produces volumetric expansion and bubbling phenomenon in green part, and can remove clean completely.After heat is de-, is directly in stove, be warming up to sintering temperature (1380 DEG C) with 5 DEG C/min to sinter equally, cools to room temperature with the furnace after insulation 2H, obtain product.
Also namely above-mentioned binding agent is the fastest de-with 0.5 DEG C/min intensification heat, and the shortest 1200min could remove completely totally and guarantee that heat takes off does not affect green part quality.That debinding rate is too slow equally, discontented sufficient actual application value.
Comparative example 3
The binding agent used in feedstock preparation method comprises the atoleine of 20%, the naphthalene of 25%, the microwax of 15%, the polyethylene of 20%, the polypropylene of 15%, the stearic acid of 5%.Said components content is all in mass fraction.The binding agent used relative to embodiment lacks solid paraffin and Brazil wax component.
Above-mentioned binding agent and metal dust (316 powder) are mixed with feeding, are injected into the green part sample that thickness is 2mm.When heat is de-, through repeatedly testing, only can with programming rate 0.7 DEG C/min from room temperature to 600 DEG C, ability is unlikely produces volumetric expansion and bubbling phenomenon in green part, and can remove clean completely.After heat is de-, is directly in stove, be warming up to sintering temperature (1380 DEG C) with 5 DEG C/min to sinter equally, cools to room temperature with the furnace after insulation 2H, obtain product.
Also namely above-mentioned binding agent is the fastest de-with 0.7 DEG C/min intensification heat, and the shortest 858min could remove completely totally and guarantee that heat takes off does not affect green part quality.That debinding rate is too slow equally, discontented sufficient actual application value.
By the contrast of embodiment and 3 comparative examples, can learn that the de-efficiency of heat is lower, in the comparative example of some change of component, also can remove completely as binding agent although final, but efficiency does not slowly have actual application value.Use the binding agent of component proportion of the present invention to make green part, finally could be warming up to 600 DEG C with 2 ~ 5 DEG C/min, with such one faster speed carry out heat take off, clean and unlikely damage green part can be removed completely, just there is actual application value.
On the other hand, the present invention also provides the powder injection-molded production work method of a kind of energy Rapid Thermal degreasing, and in various embodiments, the method can comprise the following steps:
Feedstock preparation: the moulding powder calculating 80 ~ 94%, preferably 85 ~ 94% is by mass percentage put into agitating heating in banbury, add the binder component calculating 6 ~ 20%, preferably 6 ~ 15% by mass percentage, according to melting temperature 175 ~ 195 DEG C of mixing 60 ~ 120min, obtain mixing uniform feeding;
Wherein said binding agent comprises the following component calculated by mass percentage: the atoleine of 5 ~ 10%, the naphthalene of 5 ~ 15%, 15 ~ 20% solid paraffin, 10 ~ 20% microwax, 15 ~ 20% Brazil wax, first high molecular polymer of 15 ~ 30%, second high molecular polymer of 10 ~ 20% and 1 ~ 5% surfactant, wherein said first high molecular polymer and described second high molecular polymer be selected from polyethylene, polypropylene, polyacrylate, acrylonitrile-butadiene-styrene copolymer any two;
Injection moulding: by injection machine, feeding is filled with die cavity through pressure effect, obtains green compact;
Degreasing sintered: injection moulding to be obtained green compact and puts into sintering furnace, be warming up to proper temperature to remove organic binder bond with 2 ~ 5 DEG C/min programming rate, and then be warming up to material sintering temperature and realize blank Densification, obtain finished product.Described proper temperature is especially good with 600 DEG C, can certainly be other temperature within the specific limits, as 550,650 DEG C etc.
Example 1
The first step, feedstock preparation: take 1000 order 9.1kg316L metal dusts; add in banbury and carry out stirring and heating; be heated to 190 DEG C; add binder component: atoleine 45g; stearic acid 45g, naphthalene 90g, solid paraffin 135g; microwax 180g; Brazil wax 90g, polyethylene 180g, polypropylene 135g; then banbury pressure head is depressed; melting temperature 180 DEG C is set, rotor speed 15 turns/min, after continuing to stir 90min; feeding will be mixed take out, be made for injection molding feeding by dual-screw pelletizer.
Second step, injection moulding: utilize mold injects to become Mobile phone card reincarnation base through forming machine in good for granulation 316L material, the mouth of a river is removed after taking out from mould by green compact, then puts on ceramic post sintering tool.
3rd step, degreasing sintered: the green compact be well placed carefully to be sent in sintering furnace, vacuumizes in sintering furnace and pass into protective atmosphere, rise to 600 DEG C with 5 DEG C/min programming rate, and then be warming up to 1380 DEG C with 10 DEG C/min and hold warm 120min; Obtain the mobile phone Kato of the 316L material meeting instructions for use.
Example 2
The first step, feedstock preparation: take 1000 order 8.8kg 17-4PH metal dusts; add in banbury and carry out stirring and heating; be heated to 195 DEG C; add binder component: atoleine 120g; stearic acid 12g, naphthalene 60g, solid paraffin 180g; microwax 168g; Brazil wax 240g, polyethylene 180g, polypropylene 240g; then banbury pressure head is depressed; melting temperature 175 DEG C is set, rotor speed 30 turns/min, after continuing to stir 60min; feeding will be mixed take out, be made for injection molding feeding by dual-screw pelletizer.
Second step, injection moulding: utilize mold injects to be shaped test bars green compact through forming machine good for granulation 17-4 feeding, the mouth of a river is removed after taking out from mould by green compact, then puts on ceramic post sintering tool.
3rd step, degreasing sintered: the green compact be well placed carefully to be sent in sintering furnace, vacuumizes in sintering furnace and pass into protective atmosphere, rise to 600 DEG C with 3.5 DEG C/min programming rate, and then be warming up to 1320 DEG C with 10 DEG C/min and hold warm 120min; Obtain the batten that can be used for carrying out mechanical test.
In another, the present invention also provides a kind of powder injection-molded production work method, the method comprises aforesaid injection moulding step and degreasing sintered step, wherein, and the feeding that the feeding used in injection moulding step can adopt the feedstock preparation method of aforementioned any embodiment to prepare.
Above content combines concrete/preferred embodiment further description made for the present invention, can not assert that specific embodiment of the invention is confined to these explanations.For general technical staff of the technical field of the invention; without departing from the inventive concept of the premise; its embodiment that can also describe these makes some substituting or modification, and these substitute or variant all should be considered as belonging to protection scope of the present invention.