CN113477923A - Preparation and sintering method of titanium alloy slurry for 3D printing - Google Patents
Preparation and sintering method of titanium alloy slurry for 3D printing Download PDFInfo
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- CN113477923A CN113477923A CN202110741231.8A CN202110741231A CN113477923A CN 113477923 A CN113477923 A CN 113477923A CN 202110741231 A CN202110741231 A CN 202110741231A CN 113477923 A CN113477923 A CN 113477923A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/22—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
- B22F3/225—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip by injection molding
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/10—Formation of a green body
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
- B33Y40/10—Pre-treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
- B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Abstract
The invention relates to a preparation and sintering method of titanium alloy slurry for 3D printing, and belongs to the field of additive manufacturing. The method comprises the steps of preparing a binder, preparing metal slurry, printing a sample prototype and sintering the sample. The method has the advantages that the N-methyl-2-pyrrolidone is used for replacing DBP and EGBE, so that the problems of high price, difficult manufacturing and long production period of the plasticizer can be well solved, the solid phase content is higher, PS can be dissolved, the metal solid phase content is improved, the self-supporting effect can be realized, and the sample piece is not deformed under the action of self gravity; the protective cover greatly reduces the requirement of processing equipment and saves cost. The processing method adopts the same method of processing parts, local materials are obtained, the method is simple and practical, and the cost and the difficulty of titanium alloy sintering are reduced.
Description
Technical Field
The invention belongs to the field of additive manufacturing, and particularly relates to a preparation and sintering method of titanium alloy metal slurry.
Background
3D printing technology, additive manufacturing technology, has received increasing attention as an emerging manufacturing strategy. Compared with other direct forming technologies, the slurry direct writing technology has the advantages of short production period, high efficiency, low cost, flexible production and rich raw material types, can be used for manufacturing metal, nonmetal, organic polymers and the like, and can be applied to the fields of biomedicine, electronics, optics and the like.
The titanium alloy has the advantages of strong corrosion resistance, low density, high strength and the like, and is widely applied to the fields of aerospace, biomedical treatment, high-end automobile parts and the like. The titanium alloy has stable property at normal temperature and is not easy to be oxidized, but has extremely active property at high temperature and is easy to generate violent oxidation reaction by oxygen in the air. This makes the processing conditions for titanium alloys very demanding and difficult to achieve. The method for processing the titanium alloy in the field of metal additive manufacturing comprises a selective laser melting SLM (Selective laser melting) method and an energy deposition method, but the SLM method has danger in the printing process, the processing cost is high, the residual stress exists due to small melting pool and high cooling speed, and the titanium alloy is oxidized to different degrees in the high-temperature sintering process of the two methods. At present, when titanium alloy is manufactured and processed in the welding field, an inert gas protection cover is added at a welding head to form a protection gas layer so as to isolate oxygen in air, and when the titanium alloy is manufactured and processed in a laser additive manufacturing mode, a metal protection cabin filled with inert gas is used for isolating the processing environment from the air, so that the processing without oxidation and nitridation is achieved, but the ideal effect is still not achieved.
The slurry direct-writing 3D printing technology can process titanium alloy artificial bones with external complex three-dimensional shapes and internal precise porous structures, and is widely applied to the field of biological medical treatment. The technology is characterized in that a three-dimensional structure is constructed by printing mixed slurry of titanium alloy and a binder at normal temperature, then sintering post-treatment is carried out in a high-temperature high-vacuum furnace, and the binder is removed in the post-treatment generally by adopting a high-temperature high-vacuum sintering mode to obtain a titanium alloy sample. However, because the sintering condition of titanium alloy is too harsh, high vacuum degree of Pa and high temperature of 1200-1400 ℃, and such high vacuum degree needs expensive vacuum machine set and high temperature furnace equipment with high temperature resistance and excellent sealing property, the equipment capable of pumping high vacuum to sinter titanium alloy at present comprises a diffusion pump and a mechanical pump and a molecular pump and a mechanical pump, but the molecular pump equipment is expensive in price and maintenance cost, is sensitive to particles or deposits, so that the requirements on the use environment and operation are higher, the ultimate vacuum degree and the vacuum cleaning environment of the diffusion pump are inferior to those of the molecular pump, but the diffusion pump equipment is cheap relative to the molecular pump, and can achieve the vacuum condition of sintering titanium alloy, but the two and the high temperature heating furnace pipe connected with the diffusion pump are poor in air tightness due to the difficult control factors such as small amount of air leakage, and the like, so that the surface of the titanium alloy sample piece is oxidized to cause sintering failure, the success rate of sintering is low, and the methods for manufacturing the titanium alloy have inevitable surface oxidation of the titanium alloy, so that a machined part is unusable. The quality of the metal paste, in which mainly the polymer acts as a binder, is directly affected by the quality of the forming manufacture, and the polymer is dissolved in an organic or non-organic solvent to form a colloidal binder. At present, the research of adding plasticizer Dibutyl phthalate (DBP) and ethylene glycol-butyl ether dispersant (2-butoxyyethonol, EGBE) and metal powder raw materials with certain proportion into polymer Polystyrene (PS) and Dichloromethane (DCM) as metal 3D printing slurry is relatively common, and the PS binder system, such as polylactic acid (PLA), polylactic-co-glycolic acid (PLGA), Polyethylene oxide (Polyethylene oxide, PEO) and the like, has the smallest carbon pollution introduced into the metal powder iron and no oxygen element introduced into PS during sintering, but the plasticizers DBP and EGBE are expensive, difficult to manufacture and have long production period, and under the condition that polymer PS is used as the same binder, the metal powder and proportion are utilized, there are few metal pastes that can meet the quality requirements without the addition of relatively expensive plasticizers.
Disclosure of Invention
The invention provides a preparation and sintering method of titanium alloy slurry for 3D printing, which aims to solve the problem that titanium alloy is easy to oxidize when being manufactured and processed in the field of additive manufacturing at present.
The technical scheme adopted by the invention is that the method comprises the following steps:
(1) preparation of the Binder
Adding 3500 mass percent of polystyrene PS into dichloromethane DCM, adding colorless oily N-methyl-2-pyrrolidone NMP, standing for 48h for preparing metal slurry,
(2) preparation of Metal pastes
Mixing the prepared binder with metal titanium powder, wherein the mixing volume ratio of the polystyrene PS to the metal titanium powder is 1: 2.3-4, pouring the two into a ball milling tank for ball milling and mixing, wherein the mass ratio of the metal titanium powder added into the binder solution to the small balls is 1:1, mixing in a planetary ball mill for 20-30 minutes;
(3) printing a sample prototype
Filling the prepared slurry into an injector, printing by using a conical needle head, extruding metal slurry under the pressure of 0.3-0.4 MPa, naturally air-drying the printed sample prototype for 12-24 hours, and ensuring that the solvent in the sample prototype is completely evaporated to obtain a titanium alloy sample piece of harder metal and a binder;
(4) sintering of the sample
Before sintering, printing a protective cover made of the same material as the titanium alloy sample piece, covering the protective cover above the sample piece, wherein the sintering temperature is 1200-1300 ℃, the heat preservation time is 3-4 hours, and obtaining the titanium alloy which is not oxidized after the sample is sintered.
The volume fraction of the polystyrene PS with the mass fraction of 3500 in the step (1) of the invention is 20-30%.
In the step (1), the volume fraction of the N-methyl-2-pyrrolidone NMP is 0.2-0.5%.
In the step (1), the mass ratio of the polystyrene PS with the mass fraction of 3500, the dichloromethane DCM and the N-methyl-2-pyrrolidone NMP is 1: 1-2.5: 0.2-0.5.
The planetary ball mill in step (2) of the present invention mixes at a rotation speed of 600 r/min.
The inner diameter of the conical needle in the step (3) of the invention is 350 microns.
The parameters of the extruded metal slurry in the step (3) of the invention are as follows: the layer height is 0.20-0.25 mm, the printing speed is 10-15 mm/s, the filling rate is 50% -100%, and the extrusion width is automatically set by a printer.
In the step (4) of the invention, a tube furnace diffusion pump is used for sintering.
The invention has the following advantages:
the invention uses N-methyl-2-pyrrolidone (NMP) to replace DBP and EGBE, which can solve the problems of high price, difficult manufacture and long production period of the plasticizer, and the function of NMP in the PS binder system can be used as a dispersant to remove the static and space repulsion between molecules, so that the solid phase content is higher; but also can dissolve PS as a solvent of the PS, improves the solid content of metal, simultaneously has extremely low volatility of NMP, provides better fluidity for the extrusion of ink, can play a role in self-supporting, and does not deform a sample under the action of self gravity.
The protective cover greatly reduces the requirement of processing equipment and saves cost. The sintering success can be guaranteed only under the environment with Pa high vacuum and excellent air tightness, but under the condition of a protective cover, a very small amount of oxygen and oil gas is allowed. The protective cover can adapt to the shape of a workpiece to form effective protection, and can adapt to the material of the workpiece to realize targeted protection. The material of the protective cover is the same as that of the processed part, the processing method adopts the same method of the processed part, the materials are locally obtained, the method is simple and practical, and the sintering cost and the sintering difficulty of the titanium alloy are reduced.
Drawings
FIG. 1 is a drawing of a sample titanium alloy sintered without a protective cover according to the present invention;
FIG. 2 is a drawing of a sample titanium alloy sintered with a protective cap according to the present invention;
FIG. 3 is a view of the outer surface of the boot of the present invention after sintering;
fig. 4 is a view of the inside surface of the sintered boot of the present invention.
Detailed Description
Example 1
(1) Preparation of the Binder
Adding 3500 mass percent of polystyrene PS into dichloromethane DCM, adding a proper amount of colorless oily N-methyl-2-pyrrolidone NMP, standing for 48h to prepare metal slurry, wherein the volume percent of the PS is 20 percent, the volume percent of the NMP is 0.2 percent, and the mass ratio of the PS to the DCM to the NMP is 1:1: 0.2;
(2) preparation of Metal pastes
Mixing the prepared binder with metal titanium powder, wherein the mixing volume ratio of the polystyrene PS to the metal titanium powder is 1: and 2.3, pouring the two into a ball milling tank for ball milling and mixing, wherein the mass ratio of the metal titanium powder added into the binder solution to the small balls is 1:1, mixing for 20 minutes in a planetary ball mill at the rotating speed of 600 r/min;
(3) printing a sample prototype
The prepared paste was loaded into a syringe, printed using a conical needle with an internal diameter of 350 microns, and the metal paste was extruded at a pressure of 0.3MPa, printing the extrusion parameters: the layer height is 0.20mm, the printing speed is 10mm/s, the filling rate is 50%, the extrusion width is automatically set by a printer, the printed sample prototype is naturally air-dried for 12 hours, the solvent in the prototype is ensured to be completely evaporated, and a titanium alloy sample piece of harder metal and binder is obtained;
(4) sintering of the sample
Printing a protective cover made of the same material as the titanium alloy sample piece before sintering, covering the protective cover above the sample piece, sintering by using a tube furnace diffusion pump, wherein the sintering temperature is 1200 ℃, the heat preservation time is 3 hours, and obtaining the titanium alloy which is not oxidized after the sample is sintered.
Example 2
(1) Preparation of the Binder
Adding 3500 mass percent of polystyrene PS into dichloromethane DCM, adding a proper amount of colorless oily N-methyl-2-pyrrolidone NMP, standing for 48h to prepare metal slurry, wherein the volume percent of the PS is 25 percent, the volume percent of the NMP is 0.4 percent, and the mass ratio of the PS, the DCM and the NMP is 1:1.5: 0.4;
(2) preparation of Metal pastes
Mixing the prepared binder with metal titanium powder, wherein the mixing volume ratio of the polystyrene PS to the metal titanium powder is 1: and 3.2, pouring the two into a ball milling tank for ball milling and mixing, wherein the mass ratio of the metal titanium powder added into the binder solution to the small balls is 1:1, mixing for 25 minutes in a planetary ball mill at the rotating speed of 600 r/min;
(3) printing a sample prototype
The prepared paste was loaded into a syringe, printed using a conical needle with an internal diameter of 350 microns, and the metal paste was extruded at a pressure of 0.35MPa, printing the extrusion parameters: the layer height is 0.22mm, the printing speed is 12mm/s, the filling rate is 75%, the extrusion width is automatically set by a printer, the printed sample prototype is naturally air-dried for 18 hours, the solvent in the prototype is ensured to be completely evaporated, and a titanium alloy sample piece of harder metal and binder is obtained;
(4) sintering of the sample
Printing a protective cover made of the same material as the titanium alloy sample piece before sintering, covering the protective cover above the sample piece, sintering by using a tube furnace diffusion pump, wherein the sintering temperature is 1250 ℃, the heat preservation time is 3.5 hours, and obtaining the titanium alloy which is not oxidized after the sample is sintered.
Example 3
(1) Preparation of the Binder
Adding 3500 mass percent of polystyrene PS into dichloromethane DCM, adding a proper amount of colorless oily N-methyl-2-pyrrolidone NMP, standing for 48h to prepare metal slurry, wherein the volume percent of the PS is 30 percent, the volume percent of the NMP is 0.5 percent, and the mass ratio of the PS, the DCM and the NMP is 1:2.5: 0.5;
(2) preparation of Metal pastes
Mixing the prepared binder with metal titanium powder, wherein the mixing volume ratio of the polystyrene PS to the metal titanium powder is 1: and 4, pouring the two into a ball milling tank for ball milling and mixing, wherein the mass ratio of the metal titanium powder added into the binder solution to the small balls is 1:1, mixing for 30 minutes in a planetary ball mill at the rotating speed of 600 r/min;
(3) printing a sample prototype
The prepared paste was loaded into a syringe, printed using a conical needle with an internal diameter of 350 microns, and the metal paste was extruded at a pressure of 0.4MPa, printing the extrusion parameters: the layer height is 0.25mm, the printing speed is 15mm/s, the filling rate is 100%, the extrusion width is automatically set by a printer, the printed sample prototype is naturally air-dried for 24 hours, the solvent in the prototype is ensured to be completely evaporated, and a titanium alloy sample piece of harder metal and binder is obtained;
(4) sintering of the sample
Printing a protective cover made of the same material as the titanium alloy sample piece before sintering, covering the protective cover above the sample piece, sintering by using a tube furnace diffusion pump, wherein the sintering temperature is 1300 ℃, the heat preservation time is 4 hours, and obtaining the titanium alloy which is not oxidized after the sample is sintered.
When the titanium alloy is sintered by using the diffusion pump tube furnace, a protective cover made of the same material as the sample is added above the titanium alloy sample loaded into the corundum boat, the protective cover is printed by 3D to adapt to the shape and the material of a workpiece, and the protective cover is used for absorbing polluted gas in a furnace cavity in the sintering process to protect the workpiece.
As shown in fig. 1 and 2, the two samples are titanium alloy after sintering, and it can be seen visually that: FIG. 1 is a titanium alloy sample sintered without a protective cover, showing surface oxidation; FIG. 2 is a titanium alloy sample sintered with a protective cap, without surface oxidation; fig. 3 and 4 are views of the outer surface and the inner surface of the protective cover, which show that the protective cover is oxidized while ensuring successful sintering of the sample therein, and fig. 4 shows that the degree of oxidation of the sintering furnace is limited, and the protective covers with different pores and sizes can be customized according to the properties of the sample and the sintering furnace so as to ensure successful sintering. The method is not only suitable for titanium alloy, but also suitable for other metal materials as long as the material is the same as the protected sample piece or the activity is higher than that of the sample piece.
Claims (8)
1. A method of preparing and sintering a titanium alloy paste for 3D printing, comprising the steps of:
(1) preparation of the Binder
Adding 3500 mass percent of polystyrene PS into dichloromethane DCM, adding colorless oily N-methyl-2-pyrrolidone NMP, standing for 48h for preparing metal slurry,
(2) preparation of Metal pastes
Mixing the prepared binder with metal titanium powder, wherein the mixing volume ratio of the polystyrene PS to the metal titanium powder is 1: 2.3-4, pouring the two into a ball milling tank for ball milling and mixing, wherein the mass ratio of the metal titanium powder added into the binder solution to the small balls is 1:1, mixing in a planetary ball mill for 20-30 minutes;
(3) printing a sample prototype
Filling the prepared slurry into an injector, printing by using a conical needle head, extruding metal slurry under the pressure of 0.3-0.4 MPa, naturally air-drying the printed sample prototype for 12-24 hours, and ensuring that the solvent in the sample prototype is completely evaporated to obtain a titanium alloy sample piece of harder metal and a binder;
(4) sintering of the sample
Before sintering, printing a protective cover made of the same material as the titanium alloy sample piece, covering the protective cover above the sample piece, wherein the sintering temperature is 1200-1300 ℃, the heat preservation time is 3-4 hours, and obtaining the titanium alloy which is not oxidized after the sample is sintered.
2. The method of preparing and sintering a titanium alloy paste for 3D printing according to claim 1, wherein: the volume fraction of the polystyrene PS with the mass fraction of 3500 in the step (1) is 20 to 30 percent.
3. The method of preparing and sintering a titanium alloy paste for 3D printing according to claim 1, wherein: the volume fraction of the N-methyl-2-pyrrolidone NMP in the step (1) is 0.2-0.5%.
4. The method of preparing and sintering a titanium alloy paste for 3D printing according to claim 1, wherein: the mass ratio of the polystyrene PS with the mass fraction of 3500, the dichloromethane DCM and the N-methyl-2-pyrrolidone NMP in the step (1) is 1: 1-2.5: 0.2-0.5.
5. The method of preparing and sintering a titanium alloy paste for 3D printing according to claim 1, wherein: and (3) mixing the materials in the step (2) by the planetary ball mill at the rotating speed of 600 r/min.
6. The method of preparing and sintering a titanium alloy paste for 3D printing according to claim 1, wherein: the inner diameter of the conical needle in the step (3) is 350 microns.
7. The method of preparing and sintering a titanium alloy paste for 3D printing according to claim 1, wherein: the parameters of the extruded metal slurry in the step (3) are as follows: the layer height is 0.20-0.25 mm, the printing speed is 10-15 mm/s, the filling rate is 50% -100%, and the extrusion width is automatically set by a printer.
8. The method of preparing and sintering a titanium alloy paste for 3D printing according to claim 1, wherein: and (4) sintering by using a tube furnace diffusion pump.
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