CN103801696B - 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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- CN103801696B CN103801696B CN201410047509.1A CN201410047509A CN103801696B CN 103801696 B CN103801696 B CN 103801696B CN 201410047509 A CN201410047509 A CN 201410047509A CN 103801696 B CN103801696 B CN 103801696B
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- Powder Metallurgy (AREA)
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, especially
The method that there is provided a kind of Gel-casting process formed powder metallurgy complicated shape part of combination 3D printing technique.
Background technology
The literature search consulted nearly 10 years understands, 3D printing technique is one kind of Rapid Prototyping technique, also referred to as increases material system
Make, its ultimate principle is that one is cut into infinitely according to a certain coordinate axess by the mode ready-made 3D model such as design or scanning
Multiple sections, then in layer print and are stacked into together by original position, form a stereomodel in kind.
3D printing technique quickly grows at present, and wherein metal material direct forming technology becomes a big focus of research and application.Gold
Belong to the metal parts that 3D printing technique can prepare complicated shape, but existing metal 3D printer cost is prohibitively expensive, metal material
Expect that direct forming takes long extremely inefficient, feed metal powder is had high demands, the good metal dust of demand superfine spherical degree, become
This is higher, and printing precision is not high.
Gel casting technique is that organic monomer and solvent are configured to certain density premixed liquid, metal or ceramics
End is suspended in the concentrate suspension wherein making low viscosity, high solid loading（Slip）, after adding catalyst and initiator, by this
Plant concentrate suspension（Slip）In injection non-multi punch die, in a certain temperature conditions, organic polymer is monomer crosslinked to be aggregated into
Three-dimensional network shaped polymer gel, and so that powder particle is bondd in situ and solidify to form base substrate.Base substrate drying, degumming and sintering
Obtain part product.The casting flaws such as the metal parts of gel casting technique preparation is no loose, shrinkage cavity, component segregation；Tool
There are uniformly tiny microscopic structure, good mechanical properties；It is easy to add dystectic alloying element and prepare composite；Permissible
Conveniently realize the near-net-shape of complex component；In various metals material production field such as metallic magnetic material, biomedical implantation material
Material, metal-based powder metallurgy structural member etc. all have broad application prospects.
The present invention provides 3D printing technique attached gel injection molding and forming technology to prepare the side of powder metallurgy complicated shape part
Method, is printed the component die of hollow, then prepares powdered metal parts by gel injection molding and forming technology using 3D printing equipment,
By the feature manufacturing flexibly and saving raw material of 3D printing technique and gel injection molding and forming technology, can prepare arbitrarily complicated
The powdered metal parts of shape, the tiny good mechanical properties of part even tissue, time-consuming compared with common metal 3D printing technique
Short efficiency high, relatively low to metal dust granularity and shape need, low cost and Product Precision are high.Yet there are no and beaten using 3D
Die tool prepares the relevant report of powdered metal parts method.
Content of the invention
It is an object of the invention to provide a kind of method preparing powder metallurgy complicated shape part using 3D printing mould,
Print part minus model in advance using 3D printing technique, recycle the gel injection molding and forming technology system of metal dust slip
For the parison going out powdered metal parts, drying degumming, sintering can be made into the powdered metal parts of spatial complex shape, part essence
Degree is higher, functional, and process stabilizing is reliable, strong operability, takes short efficiency high, and cost is relatively low.Concrete technology flow process and ginseng
Number is as follows：
1. print die：Using 3D printing technique print space complicated shape, particularly there is the part of inner chamber complicated shape
Space minus mould, mould hollow and there is certain thickness and rigidity；
2. metal slip preparation：Prepare metal slip using solubility colloidal sol, add the dispersant of 0.01wt ~ 0.2wt%
Improve slip mobility, adjust pH value with ammonia；
3. slip casting：The catalyst of 0.01wt% ~ 0.3wt% and drawing of 0.01wt% ~ 0.5wt% is added in metal slip
Send out agent, by the method for negative pressure of vacuum, pressure pouring or vibrations, the part that metal slip is poured into hollow is born after stirring
In pattern tool, in the presence of catalyst and initiator, organic monomer cross-linked polymeric becomes three-dimensional network shaped polymer gel, and makes
Metal powder granulates bond in situ and solidify to form base substrate, and part blanks are vacuum dried 2 ~ 8 hours under the conditions of 60 DEG C ~ 150 DEG C；
4. remove mould：Mould of plastics can be made in the part blanks immersion organic solvent with mould of plastics to dissolve and to go
Remove, ABS plastic mould can be dissolved using tetrahydrofuran solvent, PLA mould of plastics then can use acetone, chloroform, dichloromethane etc.
Solvent dissolving removes, and also the part blanks with ABS plastic mould or PLA mould of plastics can be placed in vacuum is 10-2~10- 3In the vacuum drying oven of Pa, heating and thermal insulation in 80 DEG C ~ 300 DEG C temperature ranges, mould of plastics is subject to heat sublimation, until mould goes completely
Remove, thus obtaining the part blanks of complicated shape；
5. it is dried and degumming：Part blanks are vacuum dried 2 ~ 8 hours under 60 DEG C ~ 150 DEG C temperature conditionss, subsequently in sky
Under gas, protective atmosphere or vacuum condition, part blanks are carried out degumming process in 1 ~ 4 hour in 200 DEG C ~ 600 DEG C insulations；
6. sinter：Under protective atmosphere or vacuum condition, according to the optimum sintering process bar of base substrate metal or alloy powder
Part and parameter（100℃~1500℃）It is sintered.
Described 3D printing component die includes：
1）Design the part minus mould threedimensional model of desired structure shape using 3D sculpting software, be layered and cut
It is considered to contraction situation between base substrate and material object after piece is processed, layered plane is carried out by many two dimension meters by geometric center
Calculate, mold former is pressed 110% ~ 130%（I.e. shrinkage ratio K=1.1 ~ 1.3）Scaling；
2）The threedimensional model parameter of part minus mould is imported in 3D printing equipment, prints and there is certain wall thickness and strong
Degree, spatial complex shape, particularly there is the part minus mould of inner chamber complicated shape；
3）Printing part minus mould material therefor can be ABS plastic or PLA plastics, and during printing, printer nozzle temperature is
100 DEG C ~ 300 DEG C, part minus mould synusia thickness is 0.05mm ~ 0.5mm.
Described metal slip is prepared by gel injection molding and forming technology include following operation：
1）By organic monomer hydroxyethyl methylacrylate and solvent toluene by volume 0.6 ~ 1.5:1 ratio mixing is all
Even, and add the benzoyl peroxide of 0.01wt% ~ 0.5wt%, stir, be configured to organic monomer concentration be 30vol% ~
The premixed liquid of 60vol%；
2）Metal dust optimal to 5 ~ 120 μm of particle size range, granularmetric composition is added in premixed liquid, stirring is fully made solid
Phase content is the slip of 30vol% ~ 68vol%, and the dispersant adding 0.01wt% ~ 0.2wt% is to improve slip mobility；
Or operate including following：
1）By organic monomer acrylamide, methyl diacrylamine or N- vinyl pyrrole ketone and deionized water in mass ratio
0.2~0.25:1 ratio mix homogeneously, and add the cross-linking agent N of 0.001wt% ~ 0.2wt%, N '-methylene-bisacrylamide,
Stir to being completely dissolved, join to obtain the premixed liquid for 20wt% ~ 25wt% for the organic monomer concentration；
2）Metal dust optimal to 5 ~ 120 μm of particle size range, granularmetric composition is added in premixed liquid, stirring is fully made solid
Phase content be 30vol% ~ 60vol% metal slip, add 0.01wt% ~ 0.2wt% dispersant to improve slip mobility, and
Adjust the pH value of slurry using ammonia.
Compared with prior art, the present invention has following beneficial effect：
（1）Present invention offer is a kind of to prepare powdered metal parts using 3D printing technique attached gel injection molding and forming technology
Method.The powdered metal parts of arbitrarily complicated shape can be prepared, time-consuming short efficiency high, the powdered metal parts high precision of preparation,
Even tissue is tiny, good mechanical properties；
（2）According to the difference requirement of part performance, can flexibly add various alloying elements；
（3）It is reliable and stable that this method prepares powdered metal parts, strong operability, repeatable high, and 3D printing can be made to prepare
Powdered metal parts industrialized production.
Specific embodiment
Embodiment 1：Prepare iron-base part using 3D printing mould and gel injection molding and forming technology
（1）Print die：Print the part minus model of complicated shape using 3D printing equipment, print raw material and mould for ABS
Material；
（2）Prepared by metal slip：50ml organic monomer hydroxyethyl methylacrylate is dissolved in 50ml toluene solvant,
And add the cross-linking agent benzoyl peroxide of 0.1g, stir, be configured to the premixed liquid that organic monomer concentration is 50vol%；Will
Particle mean size is that 50 μm of iron powder adds in premixed liquid, and the slip that solid concentration is 60vol% is fully made in stirring, adds
The dispersant Oleic acid of 0.01wt% is to improve slip mobility；
（3）Vacuum injection molding：Add the catalyst n of 0.06wt% in iron powder slip, N '-dimethyl aniline, after stirring fully
By type vacuum injecting and forming machine, iron powder slip is injected in the part minus mould of hollow, after the completion of reaction to be solidified, puts into vacuum
In drying baker, 80 DEG C of dryings 6 hours；
（4）The dissolving demoulding：Using tetrahydrofuran solvent, the ABS plastic mould dissolving outside iron-base part base substrate is removed,
Obtain iron-base part base substrate；
（5）Body drying and degumming：Iron-base part base substrate is vacuum dried 6 hours at 80 DEG C, subsequently in nitrogen atmosphere
Under, degumming process was carried out to iron-base part base substrate in 1 hour in 600 DEG C of insulations；
（6）Sintering：Under nitrogen atmosphere, iron-base part base substrate is sintered in 1180 DEG C of insulations for 2 hours, and final acquisition is fine and close
Iron-base part, meet the requirement of properties of product.
Embodiment 2：Prepare titanium structural member using 3D printing mould and gel injection molding and forming technology
（1）Print die：Print the part model that complicated shape carries inner chamber using 3D printing equipment, printing raw material is
PLA plastics；
（2）Prepared by metal slip：By 50g organic monomer acrylamide and 200ml deionized water mix homogeneously, and add
The cross-linking agent N of 0.2g, N '-methylene-bisacrylamide, stir to being completely dissolved, join organic monomer concentration be 20wt% pre-
Mixed liquid；The titanium valve that particle mean size is 30 μm adds in premixed liquid, and the slip that solid concentration is 55vol% is fully made in stirring, plus
The dispersant Oleic acid entering 0.02wt% is to improve slip mobility, and is adjusted pH value to 10 using ammonia；
（3）Pressure casting：To in metal slip add 0.08wt% catalyst n, N, N ', N '-tetramethylethylenediamine and
The initiator ammonium persulfate of 0.1wt%, makes slip be injected into the component die of hollow by applying certain pressure after stirring
In, after the completion of reaction to be solidified, put in vacuum drying oven, 100 DEG C of dryings 4 hours；
（4）Remove mould：It is 10 that titanium structural member base substrate with PLA mould of plastics is put into vacuum-2The vacuum drying oven of Pa
In, it is incubated 2 hours in 200 DEG C, so that PLA mould of plastics is distilled to remove completely；
（5）Degumming：Under argon atmosphere, titanium structural member base substrate carries out degumming process in 2 hours in 400 DEG C of insulations,
Sintering：Under argon atmosphere, by titanium structural member base substrate 3 hours sintering of 1250 DEG C of insulations, final acquisition is fine and close
Titanium structural member, meet properties of product require.
Claims (5)
1. a kind of using 3D printing mould prepare powder metallurgy complicated shape part method it is characterised in that：
Step one, print die：Print the part minus mould with inner chamber complicated shape using 3D printing technique；
Step 2, the preparation of metal slip：Prepare metal slip using solubility colloidal sol, and add dividing of 0.01wt%-0.2wt%
Powder Oleic acid；
Step 3, slip casting：In metal slip add 0.01wt%-0.3wt% catalyst n, N '-dimethyl aniline or
N, N, N ', the initiator ammonium persulfate of N '-tetramethylethylenediamine and 0.01wt%-0.5wt%, is poured by vacuum injection molding or pressurization
Metal slip is injected in the minus component die of 3D printing by the method for casting, obtains multiple after metal slip is fully cured in mould
Miscellaneous part blanks；
Step 4, removal minus mould：Using organic solvent, the minus mould of plastics dissolving outside part blanks is removed, or make
Mould of plastics thermally decomposes to remove, and obtains the part blanks of complicated shape；
Step 5, drying and degumming：After part blanks vacuum drying, under air, protective atmosphere or vacuum condition, by part base
Body is incubated 1-4 hour at 200 DEG C -600 DEG C, by the colloid removing in part blanks；
Step 6, sintering：Under protective atmosphere or vacuum condition, the metal dust that part blanks are used in part most preferably burns
Sinter under knot process conditions, obtain required powdered metal parts.
2. a kind of method preparing powder metallurgy complicated shape part using 3D printing mould as claimed in claim 1, it is special
Levy and be, described print die includes：
(1) part minus mold former is designed by 3D sculpting software, and the threedimensional model of part minus mould is carried out
Hierarchy slicing processes the sintering shrinkage problem it is considered between base substrate and material object, by geometric center, layered plane is carried out many-side
Two dimension calculating, the threedimensional model of part minus mould is pressed 110%-130% scaling；
(2) threedimensional model parameter is imported in 3D printing equipment, print the complicated shape part that wall thickness is 0.05mm-4mm and bear
Pattern has；
(3) raw material of 3D printing component die is selected according to part material performance requirement, select using ABS plastic or
PLA plastics, the synusia thickness of component die is 0.05mm-0.5mm, and during printing, printer nozzle temperature is 100 DEG C -300 DEG C.
3. a kind of method preparing powder metallurgy complicated shape part using 3D printing mould as claimed in claim 1, it is special
Levy and be, described metal slip preparation includes：
According to the performance of metal, the sol system adopting in the preparation process of sol solutionses has two kinds, respectively hydroxyethyl methacrylate
Ethyl ester-toluene gel rubber system and aqueous gel system：
Described hydroxyethyl methylacrylate-toluene gel rubber system preparation process：
Step one, by organic monomer hydroxyethyl methylacrylate and solvent toluene 0.6-1.5 by volume:1 ratio mixing is all
Even, and add the cross-linking agent benzoyl peroxide of 0.01wt%-0.5wt%, stir, be configured to organic monomer metering system
The premixed liquid of sour hydroxyl ethyl ester concentration 30vol%-60vol%；
Step 2, optimal to particle size range 5-120 μm, granularmetric composition metal dust is added in premixed liquid, stir and make
Solid concentration is the metal slip of 30vol%-68vol%, and the dispersant Oleic acid adding 0.01wt%-0.2wt% is to improve material
Slurry mobility；
Described aqueous gel system preparation process：
Step one, organic monomer acrylamide, methyl diacrylamine or N- vinyl pyrrole ketone and deionized water are pressed quality
Compare 0.2-0.25:1 ratio mix homogeneously, and add the cross-linking agent N of 0.001wt%-0.2wt%, N '-methylene bisacrylamide acyl
Amine, stirs to being completely dissolved, and joins to obtain the premixed liquid for 20wt%-25wt% for the organic monomer concentration；
Step 2, optimal to particle size range 5-120 μm, granularmetric composition metal dust is added in premixed liquid, stirring is fully made
Solid concentration is the metal slip of 30vol%-60vol%, and the dispersant Oleic acid adding 0.01wt%-0.2wt% is to improve material
Slurry mobility, and adjust pH value using ammonia.
4. a kind of method preparing powder metallurgy complicated shape part using 3D printing mould as claimed in claim 1, it is special
Levy and be, described slip casting is the method using negative pressure of vacuum, pressurization or vibrations degasification, and metal slip is injected part minus
In mould, remove the bubble in slip, and be allowed to be completely filled with whole part minus dies cavity.
5. the method preparing powder metallurgy complicated shape part using 3D printing mould as claimed in claim 1, its feature exists
In described organic solvent is to be completely dissolved ABS plastic or PLA plastics, and avoids the Organic substance dissolving in base substrate is organic molten
Agent, the organic solvent of ABS plastic mould is oxolane, and the organic solvent of PLA mould of plastics is acetone, chloroform, dichloro
Methane, all will not dissolve the Organic substance in part blanks through testing above organic solvent；
Described thermal decomposition is that the part blanks with ABS plastic mould or PLA mould of plastics are placed in vacuum for 10-2-10- 3In the vacuum drying oven of Pa, heating and thermal insulation in 80 DEG C of -300 DEG C of temperature ranges, mould of plastics is subject to heat sublimation, until mould goes completely
Remove.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410047509.1A CN103801696B (en) | 2014-02-11 | 2014-02-11 | Method for preparing powder metallurgy complex shape part by using 3D printing mold |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410047509.1A CN103801696B (en) | 2014-02-11 | 2014-02-11 | Method for preparing powder metallurgy complex shape part by using 3D printing mold |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103801696A CN103801696A (en) | 2014-05-21 |
| CN103801696B true CN103801696B (en) | 2017-02-08 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201410047509.1A Expired - Fee Related 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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