CN103801696A - Method for preparing powder metallurgy complex shape part by using 3D printing mold - Google Patents
Method for preparing powder metallurgy complex shape part by using 3D printing mold Download PDFInfo
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- CN103801696A CN103801696A CN201410047509.1A CN201410047509A CN103801696A CN 103801696 A CN103801696 A CN 103801696A CN 201410047509 A CN201410047509 A CN 201410047509A CN 103801696 A CN103801696 A CN 103801696A
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- 238000005245 sintering Methods 0.000 claims description 13
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- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 3
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 3
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 3
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 3
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- -1 N-vinyl pyrrole ketone Chemical class 0.000 claims description 2
- 238000013461 design Methods 0.000 claims description 2
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- CEHHGEQOHMSYEE-UHFFFAOYSA-N n-methyl-n-prop-2-enoylprop-2-enamide Chemical compound C=CC(=O)N(C)C(=O)C=C CEHHGEQOHMSYEE-UHFFFAOYSA-N 0.000 claims description 2
- 238000007569 slipcasting Methods 0.000 claims description 2
- 238000000859 sublimation Methods 0.000 claims description 2
- 230000008022 sublimation Effects 0.000 claims description 2
- GFPUQEPTYWFAHI-UHFFFAOYSA-N 2-hydroxyethyl 2-methylprop-2-enoate;toluene Chemical compound CC1=CC=CC=C1.CC(=C)C(=O)OCCO GFPUQEPTYWFAHI-UHFFFAOYSA-N 0.000 claims 2
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- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 2
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- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 2
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Abstract
The invention provides a method for preparing a powder metallurgy complex shape part by using a 3D printing mold. A 3D printing technology and a gel-casting forming technology are combined, namely a 3D printer is used for printing a thin-wall hollow part minus mold in a complex shape, the gel-casting technology is used for preparing metal slurry, after a catalyst and an initiator are added, the metal slurry is injected into the part minus mold, the metal slurry is solidified and dried, then organic solvent is used for dissolving a plastic mold or the plastic mold is subjected to thermal decomposition to be removed, so that a formed part blank body is obtained, and after the part blank body is dried, degummed and sintered, the needed powder metallurgy part is obtained. The method is capable of being used for preparing powder metallurgy parts of any complex shape, even and small in part tissue, stable and reliable in technology, high in operability, short in consumed time, high in efficiency, low in cost and beneficial to industrial production for preparation of the powder metallurgy parts through the 3D printing technology.
Description
Technical field
The present invention relates to a kind of powder forming technology, belong to parts preparation field in powder metallurgical production technique, a kind of method of gel injection-moulding process forming powder metallurgy complicated shape part of combination 3D printing technique is particularly provided.
Background technology
The literature search of consulting nearly 10 years is known, 3D printing technique is the one of RP technique, also be called and increase material manufacture, its basic principle is by designing or the ready-made 3D model of mode such as scanning is cut into unlimited multiple section according to a certain reference axis one, then in layer print and be stacked into together by original position, forming a three-dimensional model in kind.Rapidly, wherein metal material direct forming technology becomes a large focus of research and application in 3D printing technique development at present.Metal 3D printing technique can be prepared the metal parts of complicated shape, but existing metal 3D printer cost is too expensive, and metal material direct forming long efficiency consuming time is extremely low, require high to feed metal powder, the good metal dust of demand superfine spherical degree, cost is higher, and printing precision is not high.
Gel casting technique is that organic monomer and solvent are mixed with to certain density premixed liquid, metal or ceramic powder suspension are in the concentrate suspension (slip) of wherein making low viscosity, high solid loading, after adding catalyst and initator, this concentrate suspension (slip) is injected to non-porous mould, under certain temperature conditions, organic polymer is monomer crosslinked aggregates into three-dimensional network shaped polymer gel, and makes powder particle original position bonding and solidify to form base substrate.Base substrate drying, come unstuck and sintering obtains part product.Metal parts prepared by gel casting technique is without casting flaws such as loose, shrinkage cavity, component segregations; There is evenly tiny microscopic structure, good mechanical properties; Be easy to add dystectic alloying element and prepare composite; Can realize easily the near-net-shape of complex component; In various metals manufacture of materials field as metallic magnetic material, biomedical embedded material, metal-based powder metallurgy structural member etc. all have broad application prospects.
The invention provides 3D printing technique attached gel injection molding and forming technology and prepare the method for powder metallurgy complicated shape part, utilize 3D printing device to print the component die of hollow, prepare powdered metal parts by gel injection molding and forming technology again, the manufacture that relies on 3D printing technique and gel injection molding and forming technology flexibly and save raw-material feature, can prepare the powdered metal parts of any complicated shape, the tiny good mechanical properties of part even tissue, compared with printing technique with common metal 3D, fugitive rate consuming time is high, lower to metal dust granularity and shape need, cost is low and Product Precision is high.Yet there are no the relevant report of utilizing 3D print die to prepare powdered metal parts method.
Summary of the invention
The object of the present invention is to provide a kind of 3D of utilization print die to prepare the method for powder metallurgy complicated shape part, utilize 3D printing technique to print in advance part minus model, the gel injection molding and forming technology of recycling metal dust slip is prepared the parison of powdered metal parts, the powdered metal parts that drying is come unstuck, sintering can be made into spatial complex shape, element precision is higher, functional, process stabilizing is reliable, strong operability, fugitive rate consuming time is high, and cost is lower.Concrete technology flow process and parameter are as follows:
1. print die: utilize 3D printing technique print space complicated shape, particularly have the part space minus mould of inner chamber complicated shape, mould hollow and there is certain thickness and rigidity;
2. metal Pulp preparation: utilize solubility colloidal sol to prepare metal slip, add the dispersant of 0.01wt ~ 0.2wt% to improve slip mobility, regulate pH value with ammoniacal liquor;
3. slip casting: add the catalyst of 0.01wt% ~ 0.3wt% and the initator of 0.01wt% ~ 0.5wt% in metal slip, method by negative pressure of vacuum, pressure pouring or vibrations after stirring is poured into metal slip in the part minus mould of hollow, under the effect of catalyst and initator, organic monomer cross-linked polymeric becomes three-dimensional network shaped polymer gel, and make metal powder granulates original position bonding and solidify to form base substrate, the vacuum drying 2 ~ 8 hours under 60 ℃ ~ 150 ℃ conditions of part base substrate;
4. remove mould: the part base substrate with mould of plastics can be immersed in organic solvent, mould of plastics is dissolved to be removed, ABS plastic mould can use tetrahydrofuran solvent to dissolve, PLA mould of plastics can use acetone, chloroform, carrene equal solvent to dissolve and remove, and can be also 10 by being placed in vacuum with the part base substrate of ABS plastic mould or PLA mould of plastics
-2~ 10
-3in the vacuum drying oven of Pa, heating and thermal insulation in 80 ℃ ~ 300 ℃ temperature ranges, mould of plastics is subject to heat sublimation, until mould removes completely, thereby obtains the part base substrate of complicated shape;
5. dry and come unstuck: the vacuum drying 2 ~ 8 hours under 60 ℃ ~ 150 ℃ temperature conditions of part base substrate, under air, protective atmosphere or vacuum condition, part base substrate is carried out to degumming process for 1 ~ 4 hour 200 ℃ ~ 600 ℃ insulations subsequently;
6. sintering: under protective atmosphere or vacuum condition, carry out sintering according to the optimum sintering process condition of base substrate metal or alloy powder and parameter (100 ℃ ~ 1500 ℃).
Described 3D prints component die and comprises:
1) use 3D sculpting software to design the part minus mould threedimensional model of desired structure shape, after its hierarchy slicing is processed, consider the contraction situation between base substrate and material object, by geometric center, layered plane being carried out to many-sided two dimension and calculate, is shrinkage ratio K=1.1 ~ 1.3 by mold former in 110% ~ 130%() ratio amplification;
2) the threedimensional model parameter of part minus mould is imported in 3D printing device, print and have certain wall thickness and intensity, spatial complex shape, particularly has the part minus mould of inner chamber complicated shape;
3) print part minus mould material therefor and can be ABS plastic or PLA plastics, when printing, printer nozzle temperature is 100 ℃ ~ 300 ℃, and part minus mould synusia thickness is 0.05mm ~ 0.5mm.
Describedly prepare metal slip by gel injection molding and forming technology and comprise following operation:
1) by organic monomer hydroxyethyl methacrylate and solvent toluene by volume the ratio of 0.6 ~ 1.5:1 mix, and add the benzoyl peroxide of 0.01wt% ~ 0.5wt%, stir, be mixed with the premixed liquid that organic monomer concentration is 30vol% ~ 60vol%;
2) metal dust of particle size range 5 ~ 120 μ m, granularmetric composition the best is added in premixed liquid, stir and fully make the slip that solid concentration is 30vol% ~ 68vol%, add the dispersant of 0.01wt% ~ 0.2wt% to improve slip mobility;
Or comprise following operation:
1) by organic monomer acrylamide, methyl diacrylamine or N-vinyl pyrrole ketone and deionized water in mass ratio the ratio of 0.2 ~ 0.25:1 mix, and add the crosslinking agent N of 0.001wt% ~ 0.2wt%, N '-methylene-bisacrylamide, be stirred to completely and dissolve, join to obtain the organic monomer concentration premixed liquid that is 20wt% ~ 25wt%;
2) metal dust of particle size range 5 ~ 120 μ m, granularmetric composition the best is added in premixed liquid, stir and fully make the metal slip that solid concentration is 30vol% ~ 60vol%, add the dispersant of 0.01wt% ~ 0.2wt% to improve slip mobility, and use ammoniacal liquor to regulate the pH value of slurry.
Compared with prior art, the present invention has following beneficial effect:
(1) the invention provides a kind of method that the 3D of utilization printing technique attached gel injection molding and forming technology is prepared powdered metal parts.Can prepare the powdered metal parts of any complicated shape, fugitive rate consuming time is high, and the powdered metal parts precision of preparation is high, and even tissue is tiny, good mechanical properties;
(2), according to the different requirements of part performance, can add flexibly various alloying elements;
(3) to prepare powdered metal parts reliable and stable for this method, and strong operability is repeatable high, can make 3D print and prepare powdered metal parts suitability for industrialized production.
The specific embodiment
Embodiment 1: utilize 3D print die and gel injection molding and forming technology to prepare iron-base part
(1) print die: utilize 3D printing device to print the part minus model of complicated shape, printing raw material is ABS plastic;
(2) metal Pulp preparation: 50ml organic monomer hydroxyethyl methacrylate is dissolved in 50ml toluene solvant, and adds the crosslinking agent benzoyl peroxide of 0.1g, stir, be mixed with the premixed liquid that organic monomer concentration is 50vol%; The iron powder that is 50 μ m by particle mean size adds in premixed liquid, stirs and fully makes the slip that solid concentration is 60vol%, adds the dispersant oleic acid of 0.01wt% to improve slip mobility;
(3) vacuum injection molding: the catalyst n that adds 0.06wt% in iron powder slip, N '-dimethylaniline, is injected into iron powder slip in the part minus mould of hollow, after curing reaction completes by type vacuum injecting and forming machine after stirring fully, put into vacuum drying chamber, 80 ℃ are dried 6 hours;
(4) dissolve the demoulding: use tetrahydrofuran solvent that the ABS plastic mould of iron-base part base substrate outside is dissolved and removed, obtain iron-base part base substrate;
(5) body drying and coming unstuck: the vacuum drying 6 hours at 80 ℃ of iron-base part base substrate, under nitrogen atmosphere, iron-base part base substrate was carried out to degumming process in 1 hour 600 ℃ of insulations subsequently;
(6) sintering: under nitrogen atmosphere, iron-base part base substrate carries out sintering for 2 hours 1180 ℃ of insulations, finally obtains fine and close iron-base part, meets the requirement of properties of product.
Embodiment 2: utilize 3D print die and gel injection molding and forming technology to prepare titanium structural member
(1) print die: utilize 3D printing device to print the part model of complicated shape with inner chamber, printing raw material is PLA plastics;
(2) metal Pulp preparation: 50g organic monomer acrylamide and 200ml deionized water are mixed, and add the crosslinking agent N of 0.2g, N '-methylene-bisacrylamide, is stirred to completely and dissolves, joins to obtain the organic monomer concentration premixed liquid that is 20wt%; The titanium valve that is 30 μ m by particle mean size adds in premixed liquid, stirs and fully makes the slip that solid concentration is 55vol%, adds the dispersant oleic acid of 0.02wt% to improve slip mobility, and uses ammoniacal liquor that pH value is adjusted to 10;
(3) pressure casting: to the 0.08wt% catalyst n adding in metal slip, N, N ', the initiator ammonium persulfate of N '-tetramethylethylenediamine and 0.1wt%, after stirring, by applying certain pressure, slip is injected in the component die of hollow, after curing reaction completes, put into vacuum drying chamber, 100 ℃ are dried 4 hours;
(4) remove mould: it is 10 that the titanium structural member base substrate with PLA mould of plastics is put into vacuum
-2in the vacuum drying oven of Pa, in 200 ℃ of insulations 2 hours, PLA mould of plastics is distilled to remove completely;
(5) come unstuck: under argon shield atmosphere, titanium structural member base substrate carries out degumming process for 2 hours 400 ℃ of insulations,
Sintering: under argon shield atmosphere, by 3 hours sintering of 1250 ℃ of insulations of titanium structural member base substrate, finally obtain fine and close titanium structural member, meet properties of product requirement.
Claims (5)
1. utilize 3D print die to prepare a method for powder metallurgy complicated shape part, it is characterized in that:
Step 1, print die: utilize 3D printing technique print space complicated shape, particularly have the part minus mould of inner chamber complicated shape;
Step 2, metal Pulp preparation: utilize solubility colloidal sol to prepare metal slip, and add the dispersant of 0.01wt% ~ 0.2wt%;
Step 3, slip casting: in metal slip, add the catalyst of 0.01wt% ~ 0.3wt% and the initator of 0.01wt% ~ 0.5wt%, by specific process, metal slip is injected to the minus component die that 3D prints, after metal slip solidifies completely, in mould, obtain complex parts base substrate;
Step 4, removal minus mould: with an organic solvent the minus mould of plastics of part base substrate outside is dissolved and removed, or make mould of plastics thermal decomposition to remove, obtain the part base substrate of complicated shape;
Step 5, dry and come unstuck: after the vacuum drying of part base substrate, under air, protective atmosphere or vacuum condition, part base substrate, 200 ℃ ~ 600 ℃ insulations 1 ~ 4 hour, is removed the colloid in part base substrate;
Step 6, sintering: under protective atmosphere or vacuum condition, sintering under the metal dust optimum sintering process condition that part base substrate is used at part, obtains required powdered metal parts.
2. a kind of 3D of utilization print die as claimed in claim 1 is prepared the method for powder metallurgy complicated shape part, it is characterized in that, described print die comprises:
(1) design part minus mold former by 3D sculpting software, and the threedimensional model of part minus mould is carried out to hierarchy slicing processing, consider the sintering shrinkage problem between base substrate and material object, by geometric center, layered plane is carried out to many-sided two dimension and calculate, the threedimensional model of part minus mould is amplified in 110% ~ 130% ratio;
(2) threedimensional model parameter is imported in 3D printing device, printing wall thickness is the complicated shape part minus mould of 0.05mm ~ 4mm;
(3) raw material of 3D printing component die are selected according to part material performance requirement, choice for use ABS plastic or PLA plastics, and the synusia thickness of component die is 0.05mm ~ 0.5mm, when printing, printer nozzle temperature is 100 ℃ ~ 300 ℃.
3. a kind of 3D of utilization print die as claimed in claim 1 is prepared the method for powder metallurgy complicated shape part, it is characterized in that, described metal Pulp preparation comprises:
According to the performance of metal, the sol system adopting in the preparation process of sol solutions has two kinds, is respectively hydroxyethyl methacrylate-toluene gel rubber system and aqueous gel system:
Described hydroxyethyl methacrylate-toluene gel rubber system preparation process:
Step 1, by organic monomer hydroxyethyl methacrylate and solvent toluene by volume the ratio of 0.6 ~ 1.5:1 mix, and add the crosslinking agent benzoyl peroxide of 0.01wt% ~ 0.5wt%, stir, be mixed with the premixed liquid of organic monomer hydroxyethyl methacrylate concentration 30vol% ~ 60vol%;
Step 2, the metal dust of particle size range 5 ~ 120 μ m, granularmetric composition the best is added in premixed liquid, stir and make the metal slip that solid concentration is 30vol% ~ 68vol%, add the dispersant of 0.01wt% ~ 0.2wt% to improve slip mobility;
Described aqueous gel system preparation process:
Step 1, by organic monomer acrylamide, methyl diacrylamine or N-vinyl pyrrole ketone and deionized water in mass ratio the ratio of 0.2 ~ 0.25:1 mix, and add the crosslinking agent N of 0.001wt% ~ 0.2wt%, N '-methylene-bisacrylamide, be stirred to completely and dissolve, join to obtain the organic monomer concentration premixed liquid that is 20wt% ~ 25wt%;
Step 2, the metal dust of particle size range 5 ~ 120 μ m, granularmetric composition the best is added in premixed liquid, stir and fully make the metal slip that solid concentration is 30vol% ~ 60vol%, add the dispersant of 0.01wt% ~ 0.2wt% to improve slip mobility, and use ammoniacal liquor to regulate pH value.
4. a kind of 3D of utilization print die as claimed in claim 1 is prepared the method for powder metallurgy complicated shape part, it is characterized in that, described specific process is in metal slip, to add the catalyst of 0.01wt% ~ 0.3wt% and the initator of 0.01wt% ~ 0.5wt%, after stirring, adopt the method for negative pressure of vacuum, pressurization or vibrations degasification, metal slip is injected to part minus mould, remove the bubble in slip, and make it to be full of completely whole part minus dies cavity.
5. the 3D of utilization print die as claimed in claim 1 is prepared the method for powder metallurgy complicated shape part, it is characterized in that, described organic solvent is for dissolving ABS plastic or PLA plastics completely, and avoid the organic solvent of the organic matter dissolving in base substrate, the organic solvent of ABS plastic mould is oxolane, the organic solvent of PLA mould of plastics is acetone, chloroform, carrene, all can not dissolve the organic matter in part base substrate through testing above organic solvent;
Described thermal decomposition is to be 10 by being placed in vacuum with the part base substrate of ABS plastic mould or PLA mould of plastics
-2~ 10
-3in the vacuum drying oven of Pa, heating and thermal insulation in 80 ℃ ~ 300 ℃ temperature ranges, mould of plastics is subject to heat sublimation, until mould is removed completely.
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|---|---|---|---|
| CN201410047509.1A CN103801696B (en) | 2014-02-11 | 2014-02-11 | Method for preparing powder metallurgy complex shape part by using 3D printing mold |
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|---|---|---|---|
| CN201410047509.1A CN103801696B (en) | 2014-02-11 | 2014-02-11 | Method for preparing powder metallurgy complex shape part by using 3D printing mold |
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| CN103801696B CN103801696B (en) | 2017-02-08 |
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