CN114749682B - Isolation material, metal 3D printing part and preparation method thereof - Google Patents
Isolation material, metal 3D printing part and preparation method thereof Download PDFInfo
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- CN114749682B CN114749682B CN202210362342.2A CN202210362342A CN114749682B CN 114749682 B CN114749682 B CN 114749682B CN 202210362342 A CN202210362342 A CN 202210362342A CN 114749682 B CN114749682 B CN 114749682B
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- 238000010146 3D printing Methods 0.000 title claims abstract description 87
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 85
- 239000002184 metal Substances 0.000 title claims abstract description 85
- 239000000463 material Substances 0.000 title claims abstract description 72
- 238000002955 isolation Methods 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 55
- 239000000919 ceramic Substances 0.000 claims abstract description 49
- 229920005596 polymer binder Polymers 0.000 claims abstract description 45
- 239000002491 polymer binding agent Substances 0.000 claims abstract description 45
- 239000012188 paraffin wax Substances 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims description 57
- 238000007639 printing Methods 0.000 claims description 54
- 239000000203 mixture Substances 0.000 claims description 30
- 238000010438 heat treatment Methods 0.000 claims description 29
- 230000008569 process Effects 0.000 claims description 28
- 238000001816 cooling Methods 0.000 claims description 19
- 238000005238 degreasing Methods 0.000 claims description 17
- 238000002791 soaking Methods 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 14
- 238000005245 sintering Methods 0.000 claims description 14
- 239000012774 insulation material Substances 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 9
- 238000002844 melting Methods 0.000 claims description 9
- 230000008018 melting Effects 0.000 claims description 9
- 230000006835 compression Effects 0.000 claims description 8
- 238000007906 compression Methods 0.000 claims description 8
- 238000004804 winding Methods 0.000 claims description 8
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 6
- CYTYCFOTNPOANT-UHFFFAOYSA-N Perchloroethylene Chemical group ClC(Cl)=C(Cl)Cl CYTYCFOTNPOANT-UHFFFAOYSA-N 0.000 claims description 5
- 229950011008 tetrachloroethylene Drugs 0.000 claims description 5
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- 239000004793 Polystyrene Substances 0.000 claims description 4
- 235000021355 Stearic acid Nutrition 0.000 claims description 4
- 239000005038 ethylene vinyl acetate Substances 0.000 claims description 4
- 229920001903 high density polyethylene Polymers 0.000 claims description 4
- 239000004700 high-density polyethylene Substances 0.000 claims description 4
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 4
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 4
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 229920002223 polystyrene Polymers 0.000 claims description 4
- 239000008117 stearic acid Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 3
- 125000006850 spacer group Chemical group 0.000 claims description 2
- KFUSEUYYWQURPO-OWOJBTEDSA-N trans-1,2-dichloroethene Chemical group Cl\C=C\Cl KFUSEUYYWQURPO-OWOJBTEDSA-N 0.000 claims description 2
- 238000013461 design Methods 0.000 abstract description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 56
- 229910052786 argon Inorganic materials 0.000 description 28
- 238000005516 engineering process Methods 0.000 description 12
- 239000007789 gas Substances 0.000 description 12
- 238000004519 manufacturing process Methods 0.000 description 12
- 238000011049 filling Methods 0.000 description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 239000001257 hydrogen Substances 0.000 description 8
- 229910052739 hydrogen Inorganic materials 0.000 description 8
- 239000011810 insulating material Substances 0.000 description 6
- 239000011230 binding agent Substances 0.000 description 5
- 238000003754 machining Methods 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- 238000012545 processing Methods 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000008021 deposition Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 102100024452 DNA-directed RNA polymerase III subunit RPC1 Human genes 0.000 description 1
- 101000689002 Homo sapiens DNA-directed RNA polymerase III subunit RPC1 Proteins 0.000 description 1
- 238000012356 Product development Methods 0.000 description 1
- UQZIWOQVLUASCR-UHFFFAOYSA-N alumane;titanium Chemical compound [AlH3].[Ti] UQZIWOQVLUASCR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011990 functional testing Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000011664 nicotinic acid Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- B22F10/40—Structures for supporting workpieces or articles during manufacture and removed afterwards
- B22F10/43—Structures for supporting workpieces or articles during manufacture and removed afterwards characterised by material
-
- 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
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Materials Engineering (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention provides an isolation material, a metal 3D printing part and a preparation method thereof. The isolating material comprises the following components in percentage by volume: 58-65% of ceramic powder, 18-25% of polymer binder and 10-24% of paraffin. According to the invention, through the design of the isolation material, the prepared isolation material is suitable for preparing the metal 3D printing part, and further can be used for preparing the isolation layer between the support piece and the metal 3D printing part, so that the support piece and the metal 3D printing part can be rapidly separated.
Description
Technical Field
The invention belongs to the technical field of metal 3D printing, and particularly relates to an isolation material, a metal 3D printing part and a preparation method thereof.
Background
The 3D printing is based on the principle of discrete-stacking, and an object is constructed in a layer-by-layer superposition mode, so that the three-dimensional printing has the technical advantages that complex surface and special-shaped structures can be constructed, and the light-weight structural design of the traditional parts is realized. In particular, the metal 3D printing technology, which is one of the forefront and most potential technologies in the whole 3D printing system, is an important mark for the development of the 3D printing technology and is also an important development direction of the 3D printing in the future. In recent years, metal 3D printing is widely used in the aerospace field, and GE airlines use metal 3D printing to manufacture tens of thousands of fuel nozzles for engines each year; common electric companies are using 3D printed titanium aluminum for low pressure turbine blades; in addition, in the dental field of China and the water cooling channel field of the mold, metal 3D printing is also rapidly developed.
In 2020, the usage amount of 3D printing is also greatly improved in the field of automobiles, the highest application ratio of 3D printing in the automobile industry is calculated by data, the highest application ratio reaches 16.4%, and automobiles become the largest 3D printing application market. The application of the automobile field to 3D printing is mainly based on two aspects, firstly, the non-modeling characteristic of the automobile is utilized, and functional test samples, tool fixtures, inspection tools and the like are printed in the product development process and the assembly process, so that the product verification and production are accelerated; secondly, the characteristics of bionic structure, lattice structure, thin wall structure and integrated function structure can be manufactured by utilizing the method without being limited by the traditional manufacturing process, and the method provides greater design freedom degree with the product function as the guide for automobile designers, thereby realizing light weight to the maximum extent, and improving the fuel economy, the comfort and the like of the product.
In the forming process, the 3D printing is sequentially filled from bottom to top according to the layered outline of the digital model, so that the upper layer structure of the model is required to be supported by the lower layer part, and when some parts of the printed part are suspended or the included angle between the upper layer structure and the substrate is smaller than 45 degrees, a supporting structure (supporting piece) is usually required to be added to support the suspended parts of the printed part. For stability of the printed parts, the support is generally solid, and the support is connected to the printed parts and to the substrate, which subsequently needs to be machined and removed manually. Removing the physical support presents two problems: firstly, the processing cost is increased, the processing time is prolonged, and the post-treatment is complicated; secondly, once the support piece is removed, the support residue left on the printing part can influence the overall appearance, and the normal use of the printing part is more likely to be influenced.
At present, two major types of mainstream metal 3D printing technologies for the automobile field exist in the market, one type is powder bed melting technology, and in the process of printing and forming certain overhang structures on metal parts, structural collapse can occur in a molten pool formed by melting metal powder under the action of self gravity and capillary action, so that 3D printing failure is caused. Thus, the addition of solid supports is required for support, followed by a complex support removal process.
Another type is a 3D printing technology developed based on injection molding of metal powder, which is called MIM 3D printing in general, and is an indirect 3D printing, and in addition to the molding of the printing process, the technology is subjected to post-treatment processes such as degreasing and sintering. MIM 3D printing includes two types: the first is the binder spraying technology, since the binder spraying technology has no temperature change in the printing link, the internal stress of the material is small, the self-support can be realized by means of powder, after the printing is finished, the powder support can be easily removed, but in the post-treatment sintering process, the binder volatilizes, the size of the printed part can be contracted, the restraint of a supporting piece is avoided, and the deformation problem of the part is easy to occur; the second is the fused deposition technology, the supporting materials added by the existing fused deposition technology are often the same as the printing materials, but the filling mode and the filling rate are different, the supporting parts are relatively sparse, after printing, in order to prevent deformation, the supporting parts are not removed firstly, and after degreasing and sintering, the supporting parts are removed manually by machining, which is similar to the mode of removing the supporting parts by the powder bed melting technology, and the problems of complicated process and the risks of failure are also existed.
Therefore, how to overcome the problems of complicated and possibly failure risk of the existing metal 3D printing and removing support members, so that the printed parts, the support members and the printed parts and the substrate are quickly separated, and the subsequent machining and manual support member removing procedures are simplified, and the technical problem to be solved is urgent.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide an isolation material, a metal 3D printing part and a preparation method thereof. According to the invention, through the design of the components of the isolation material, the prepared isolation material is suitable for preparing metal 3D printing parts of fused deposition type, and is further used for preparing an isolation layer between the support piece and the metal 3D printing parts, so that the support piece and the metal 3D printing parts are separated.
To achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides an insulation material comprising the following components in percentage by volume:
58-65% of ceramic powder, 18-25% of polymer binder and 10-24% of paraffin.
According to the invention, through the design of the components of the isolation material, the ceramic powder, the polymer binder and the paraffin are further matched for use, and the prepared isolation material can be used for preparing an isolation layer between the support piece and the metal 3D printing part, so that the support piece and the metal 3D printing part can be rapidly separated, and the metal 3D printing part with the target appearance is obtained.
In the metal 3D printing process, filling is sequentially carried out from bottom to top according to the layered outline of the digital model, so that the upper layer structure of the model is required to be supported by the lower layer part, and when some parts of the printed part are suspended or the included angle between the upper layer structure and the substrate is smaller than 45 degrees, a supporting structure (supporting piece) is usually required to be added to support the suspended parts of the printed part. For stability of the printed parts, the support is generally solid and is of the same material as the printed parts, with the support being connected to the printed parts and to the substrate, and subsequently being removed by machining and manually. Since the support is the same material as the printed part and is interconnected, the removal of the solid support presents two problems: firstly, the processing cost is increased, the processing time is prolonged, and the post-treatment is complicated; secondly, once the support piece is removed, the support material residue left on the printing part can influence the overall appearance, and the normal use of the printing part is more likely to be influenced.
Therefore, the invention separates the support piece from the printing part by adding the isolation layer between the support piece and the printing part, and solves the problems that the support piece is difficult to remove or is not clean to remove.
It should be noted that, the process of separating the support and the printing part includes degreasing soaking and vacuum sintering, in the degreasing soaking process, part of the polymer binder and paraffin will be removed, and since the ceramic material is insoluble in the solvent, and the polymer binder and paraffin are only partially removed, the rest of the isolation material remains between the support and the printing part and maintains the original shape, and the suspended part of the printing part can be supported, so that the suspended part of the printing part is prevented from losing support and collapsing; and then, completely removing the polymer binder and the paraffin wax through a vacuum sintering process, wherein the melting point of the ceramic powder is far higher than the sintering temperature, so that the ceramic powder cannot be removed and is not fused with the metal material of the body, and the printing part and the support piece can be separated, thereby being convenient for the separation of the printing part and the support piece.
In the present invention, the ceramic powder may be 58%, 59%, 60%, 61%, 62%, 63%, 64%, 65% or the like by volume in the insulating material.
The volume percent of the polymeric binder may be 18%, 19%, 20%, 21%, 22%, 23%, 24%, 25%, etc.
The paraffin may be 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%, 21%, 22%, 23% or 24% by volume, etc.
The following is a preferred technical scheme of the present invention, but not a limitation of the technical scheme provided by the present invention, and the following preferred technical scheme can better achieve and achieve the objects and advantages of the present invention.
As a preferred embodiment of the present invention, the ceramic powder is selected from A1 2 O 3 、ZrO 2 Or SiO 2 Any one or a combination of at least two of these.
Preferably, the ceramic powder comprises A1 2 O 3 、ZrO 2 And SiO 2 In the ceramic powder, A1 is calculated by taking the volume of the ceramic powder as 100 percent 2 O 3 46 to 57% by volume (for example, 46%, 47%, 48%, 49%, 50%, 51%, 52%, 53%, 54%, 55%, 56% or 57%, etc.), of ZrO in the ceramic powder 2 24-32% (e.g. 24%, 25%, 26%, 27%, 28%, 29%, 30%, 31)% or 32%, etc.), siO in the ceramic powder 2 The volume percentage of (a) is 11-30% (for example, 11%, 12%, 14%, 16%, 18%, 20%, 22%, 24%, 26%, 28%, 30%, etc.).
Preferably, D of the ceramic powder 50 The particle size is 3 to 5. Mu.m, for example, 3. Mu.m, 3.2. Mu.m, 3.4. Mu.m, 3.6. Mu.m, 3.8. Mu.m, 4.2. Mu.m, 4.4. Mu.m, 4.6. Mu.m, 4.8. Mu.m, 5. Mu.m, etc.
In the present invention, the ceramic powder has a bulk density of 45 to 55% (for example, 45%, 46%, 47%, 48%, 49%, 50%, 51%, 52%, 53%, 54%, 55%, etc.), and a tap density of 60 to 80% (for example, 60%, 62%, 64%, 66%, 68%, 70%, 72%, 74%, 76%, 78%, 80%, etc.).
As a preferable technical scheme of the invention, the polymer binder comprises the following components in percentage by mass based on 100% by mass of the polymer binder: polystyrene 58-65% (e.g., 58%, 59%, 60%, 61%, 62%, 63%, 64%, or 65%, etc.), high density polyethylene 6-10% (e.g., 6%, 7%, 8%, 9%, or 10%, etc.), ethylene-vinyl acetate copolymer 7-12% (e.g., 7%, 8%, 9%, 10%, 11%, or 12%, etc.), polyethylene glycol 8-26% (e.g., 8%, 10%, 12%, 14%, 16%, 18%, 20%, 22%, 24%, or 26%, etc.), and stearic acid 3-5% (e.g., 3%, 3.5%, 4%, 4.5%, or 5%, etc.).
According to the invention, through the design of the components of the polymer binder, the components are further matched for use, and the prepared isolation material can be partially removed in the soaking degreasing process, but the original shape of the isolation material in the 3D printing process can be maintained, so that the collapse of the printed part is avoided, the polymer binder can be completely removed in the vacuum sintering process, and the ceramic powder is isolated between the support piece and the printed part, so that the separation of the support piece and the printed part is facilitated.
In the invention, the polymer binder is prepared by the following method, which comprises the following steps:
and uniformly mixing all the components of the polymer binder to obtain the polymer binder.
In a second aspect, the present invention provides a method for preparing the insulation material according to the first aspect, the method comprising the steps of:
(1) Placing ceramic powder, a polymer binder and paraffin into a high-speed stirrer for mixing to obtain a mixture;
(2) And (3) adding the mixture obtained in the step (1) into a screw extruder, extruding the wire through a die, and winding the wire into a coiled wire through a disc device to obtain the isolation material.
In a preferred embodiment of the present invention, the temperature of the mixture is 155 to 185℃and may be, for example, 155℃160℃165℃170℃175℃180℃or 185 ℃.
Preferably, the mixing time is 110-150 min, for example, 110min, 115min, 120min, 125min, 130min, 135min, 140min, 145min or 150min, etc.
Preferably, the mixing further comprises a post-treatment step.
Preferably, the post-treatment is carried out by cooling to room temperature.
In the present invention, the room temperature was 25 ℃.
As a preferred embodiment of the present invention, the temperature of the feeding section of the screw extruder is 25 to 50 ℃ (e.g., 25 ℃, 30 ℃, 35 ℃, 40 ℃, 45 ℃, 50 ℃), etc.), the temperature of the compression section is 100 to 130 ℃ (e.g., 100 ℃, 105 ℃, 110 ℃, 115 ℃, 120 ℃, 125 ℃, 130 ℃), etc.), the temperature of the homogenizing section is 120 to 160 ℃ (e.g., 120 ℃, 125 ℃, 130 ℃, 135 ℃, 140 ℃, 145 ℃, 150 ℃, 155 ℃, 160 ℃, etc.), the temperature of the die head is 155 to 185 ℃ (e.g., 155 ℃, 160 ℃, 165 ℃, 170 ℃, 175 ℃, 180 ℃, 185 ℃, etc.), the temperature of the die section is 155 to 185 ℃ (e.g., 155 ℃, 160 ℃, 165 ℃, 170 ℃, 175 ℃, 180 ℃, 185 ℃, etc.).
Preferably, the filament diameter of the extruded filament is 1.6 to 2.4mm, for example, 1.6mm, 1.7mm, 1.8mm, 1.9mm, 2mm, 2.1mm, 2.2mm, 2.3mm, 2.4mm, or the like.
In the invention, the preparation method of the isolation material specifically comprises the following steps:
(1) Placing ceramic powder, a polymer binder and paraffin wax into a high-speed stirrer, and mixing for 110-150 min at 155-185 ℃ to obtain a mixture;
(2) And (3) adding the mixture obtained in the step (1) into a screw extruder, extruding wires through a die, winding wires through a disc device, and collecting the wires into coiled wires to obtain the isolation material, wherein the temperature of a feeding section of the screw extruder is 20-50 ℃, the temperature of a compression section is 100-130 ℃, the temperature of a homogenizing section is 120-160 ℃, the temperature of a machine head is 155-185 ℃, the temperature of the die section is 155-185 ℃, and the wire outlet diameter is 1.6-2.4 mm.
In a third aspect, the present invention provides a method for preparing a metal 3D printed part, the method comprising the steps of:
(A) Adopting a 3D printer with two 3D printing nozzles, firstly using a first nozzle, printing a printing material on a lower support piece according to a digital model of a metal 3D printing part, then heating and melting an isolation material through a second nozzle of the printer under control of a computer, printing a layer of isolation layer on the lower support piece, printing the metal part above the isolation layer by adopting the printing material, and continuing to repeat the above process when encountering a part needing to be supported until the printing according to the digital model of the metal 3D printing part is completed, so as to obtain a green mould;
(B) Soaking and degreasing the green mould obtained in the step (A), and drying to obtain a brown mould;
(C) Vacuum sintering the palm die obtained in the step (B) to remove the supporting piece, thereby obtaining the metal 3D printing part;
wherein the insulation material comprises the insulation material according to the first aspect.
In the preparation method of the metal 3D printing part, the upper layer structure and the lower layer structure of the printing part and the supporting piece are made of the same material, and the upper layer structure and the lower layer structure of the printing part and the supporting piece are printed through the same nozzle of the 3D printer.
As a preferred embodiment of the present invention, the temperature of the nozzle for printing the separator by the 3D printer is 200 to 240 ℃ (for example, 200 ℃, 205 ℃, 210 ℃, 215 ℃, 220 ℃, 225 ℃, 230 ℃, 235 ℃, 240 ℃) or the like), and the thermal bed temperature of the 3D printer is 85 to 110 ℃ (for example, 85 ℃, 90 ℃, 95 ℃, 100 ℃, 105 ℃, 110 ℃ or the like).
Preferably, the thickness of the isolation layer is 0.05 to 0.15mm, for example, 0.05mm, 0.06mm, 0.07mm, 0.08mm, 0.09mm, 0.10mm, 011mm, 0.12mm, 0.13mm, 014mm or 0.15mm.
In the present invention, each time the separator is printed using the 3D printer, the thickness of the separator is independently selected from 0.05 to 0.15mm (for example, 0.05mm, 0.06mm, 0.07mm, 0.08mm, 0.09mm, 0.10mm, 011mm, 0.12mm, 0.13mm, 014mm, or 0.15 mm).
As a preferable technical scheme of the invention, the soaking degreasing solvent is tetrachloroethylene and/or trans-1, 2-dichloroethylene.
Preferably, the soaking degreasing temperature is 80-120 ℃, which can be 80 ℃, 85 ℃, 90 ℃, 95 ℃, 100 ℃, 105 ℃, 110 ℃, 115 ℃, 120 ℃ or the like.
Preferably, the soaking degreasing time is 12-24 h, for example, 12h, 14h, 16h, 18h, 20h, 22h or 24h, etc.
Preferably, the drying temperature is 60 to 70 ℃, and 60 ℃, 61 ℃, 62 ℃, 63 ℃, 64 ℃, 65 ℃, 66 ℃, 67 ℃, 68 ℃, 69 ℃, 70 ℃ or the like can be used.
Preferably, the drying time is 6 to 12 hours, and may be, for example, 6 hours, 7 hours, 8 hours, 9 hours, 10 hours, 11 hours, 12 hours, or the like.
The vacuum sintering process in the invention is as follows: placing the palm mould prepared in the step (B) in a vacuum furnace, firstly raising the temperature from room temperature to 250-350 ℃ at a heating rate of 5-8 ℃/min, and preserving the temperature for 5-6 h, wherein pure argon is required to be introduced into the furnace during heating and preserving the temperature, the purity of the argon is 99.999%, and the flow rate of the argon is 60-80L/min; then heating to 800-900 ℃ at a heating rate of 4-6 ℃/min, and preserving heat for 6-8 h, wherein no gas is filled in the stage; heating to 1210-1400 ℃ at a heating rate of 3-5 ℃/min, preserving heat for 8-10 h, and filling argon and hydrogen mixed gas into the furnace at the stage, wherein the volume ratio of the argon to the hydrogen is 5:95, and the gas flow is 60-80L/min; finally cooling to room temperature at a cooling rate of 5-8 ℃/min, cooling along with the furnace, and always filling pure argon into the furnace in the cooling stage, wherein the argon flow is 40-60L/min.
In a fourth aspect, the invention provides a metal 3D printed part prepared by the preparation method according to the third aspect.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, through the design of the components of the isolation material and the design of the components of the polymer binder, the prepared isolation material is suitable for preparing the metal 3D printing part, and can be further used for preparing the isolation layer between the support piece and the metal 3D printing part so as to quickly separate the support piece and the metal 3D printing part, the support piece cannot have residues on the metal 3D printing part, and meanwhile, the shape of the metal 3D printing part cannot collapse in the process of removing the support piece.
Detailed Description
To facilitate understanding of the present invention, examples are set forth below. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof.
Some of the component sources in the examples and comparative examples are as follows:
A1 2 O 3 : new material of Yumu with purity of 99.5%, D 50 The particle size is 4 mu m;
ZrO 2 : new material of Yumu with purity of 99.9%, D 50 The particle size is 4 mu m;
SiO 2 : universal chemical industry with purity of 99.9%, D 50 The grain diameter is 3 mu m;
polystyrene: macro plasticization;
high density polyethylene: the excellent cable chemical industry;
ethylene-vinyl acetate copolymer: the excellent cable chemical industry;
polyethylene glycol: brocade source chemistry;
stearic acid: three chemical industry plants in Tianjin.
Example 1
The embodiment provides an isolation material, a metal 3D printing part and a preparation method thereof, wherein the isolation material comprises the following components in percentage by volume:
62% of ceramic powder, 23% of polymer binder and 15% of paraffin wax;
wherein the specific composition of the ceramic powder is shown in the following table 1, based on 100% of the volume of the ceramic powder; the mass of the polymer binder was 100%, and the specific composition of the polymer binder is shown in table 2 below.
The preparation method of the isolation material comprises the following steps:
(1) Placing ceramic powder, a polymer binder and paraffin wax into a high-speed stirrer, and mixing at 166 ℃ for 140min to obtain a mixture;
(2) And (3) adding the mixture obtained in the step (1) into a screw extruder, extruding wires through a die, winding wires through a disc device, and collecting the wires into coiled wires to obtain the isolation material, wherein the temperature of a feeding section of the screw extruder is 25 ℃, the temperature of a compression section is 120 ℃, the temperature of a homogenizing section is 145 ℃, the temperature of a machine head is 172 ℃, the temperature of the die section is 172 ℃, and the diameter of the wires is 1.8mm.
The preparation method of the metal 3D printing part comprises the following steps:
(A) Adopting a 3D printer with two 3D printing nozzles, firstly using a first nozzle, printing a printing material on a lower support piece according to a digital model of a metal 3D printing part, then heating and melting an isolation material through a second nozzle of the printer under control of a computer, printing a layer of isolation layer on the lower support piece, printing the metal part above the isolation layer by adopting the printing material, and continuing to repeat the above process when encountering a part needing to be supported until the printing according to the digital model of the metal 3D printing part is completed, so as to obtain a green mould, wherein the temperature of the nozzle of the 3D printer is 210 ℃, the temperature of a hot bed is 90 ℃, and the thickness of each layer of isolation layer is 0.075mm;
(B) Soaking the green mould obtained in the step (A) in tetrachloroethylene for 20 hours at 90 ℃ for soaking degreasing, and drying at 63 ℃ for 8 hours to obtain a brown mould;
(C) Placing the palm mould obtained in the step (B) in a vacuum furnace, raising the temperature from 25 ℃ to 320 ℃ at a heating rate of 6 ℃/min, and preserving the heat for 6 hours, wherein pure argon is required to be introduced into the furnace during heating and preserving the heat, the purity of the argon is 99.999%, and the argon introducing flow is 64L/min; then heating to 850 ℃ at a heating rate of 4 ℃/min, and preserving heat for 6.5 hours, wherein no gas is filled in the stage; heating to 1250 ℃ at a heating rate of 3 ℃/min, preserving heat for 10 hours, and filling argon and hydrogen mixed gas into the furnace at the stage, wherein the volume ratio of the argon to the hydrogen is 5:95, and the gas flow is 60L/min; and finally, cooling to 25 ℃ at a cooling rate of 6 ℃/min, cooling along with the furnace, and filling pure argon into the furnace at the cooling stage, wherein the argon flow is 45L/min, so as to finish vacuum sintering, and removing the support piece to obtain the metal 3D printing part.
Example 2
The embodiment provides an isolation material, a metal 3D printing part and a preparation method thereof, wherein the isolation material comprises the following components in percentage by volume:
59% of ceramic powder, 20% of polymer binder and 21% of paraffin wax;
wherein the specific composition of the ceramic powder is shown in the following table 1, based on 100% of the volume of the ceramic powder; the mass of the polymer binder was 100%, and the specific composition of the polymer binder is shown in table 2 below.
The preparation method of the isolation material comprises the following steps:
(1) Placing ceramic powder, polymer binder and paraffin wax into a high-speed stirrer, and mixing at 171 ℃ for 130min to obtain a mixture;
(2) And (3) adding the mixture obtained in the step (1) into a screw extruder, extruding wires through a die, winding wires through a disc device, and collecting the wires into coiled wires to obtain the isolation material, wherein the temperature of a feeding section of the screw extruder is 40 ℃, the temperature of a compression section is 110 ℃, the temperature of a homogenizing section is 130 ℃, the temperature of a machine head is 160 ℃, the temperature of the die section is 160 ℃, and the diameter of the wires is 2mm.
The preparation method of the metal 3D printing part comprises the following steps:
(A) Adopting a 3D printer with two 3D printing nozzles, firstly using a first nozzle, printing a printing material on a lower support piece according to a digital model of a metal 3D printing part, then heating and melting an isolation material through a second nozzle of the printer under control of a computer, printing a layer of isolation layer on the lower support piece, printing the metal part above the isolation layer by adopting the printing material, and continuing to repeat the above process when encountering a part needing to be supported until the printing according to the digital model of the metal 3D printing part is completed, so as to obtain a green mould, wherein the temperature of the nozzle of the 3D printer is 220 ℃, the temperature of a hot bed is 110 ℃, and the thickness of each isolation layer is 0.125mm;
(B) Soaking the green mould obtained in the step (A) in tetrachloroethylene for 14 hours at 110 ℃ for soaking degreasing, and drying for 8 hours at 65 ℃ to obtain a brown mould;
(C) Placing the palm mould obtained in the step (B) in a vacuum furnace, raising the temperature from 25 ℃ to 350 ℃ at a heating rate of 8 ℃/min, and preserving the heat for 6 hours, wherein pure argon is required to be introduced into the furnace during heating and preserving the heat, the purity of the argon is 99.999%, and the argon introducing flow is 70L/min; then heating to 800 ℃ at a heating rate of 5 ℃/min, and preserving heat for 7 hours, wherein no gas is filled in the stage; heating to 1360 ℃ at a heating rate of 5 ℃/min, preserving heat for 8 hours, and filling argon and hydrogen mixed gas into the furnace at the stage, wherein the volume ratio of the argon to the hydrogen is 5:95, and the gas flow is 70L/min; and finally, cooling to 25 ℃ at a cooling rate of 8 ℃/min, cooling along with the furnace, and filling pure argon into the furnace at the cooling stage, wherein the argon flow is 60L/min, so as to finish vacuum sintering, and removing the support piece to obtain the metal 3D printing part.
Example 3
The embodiment provides an isolation material, a metal 3D printing part and a preparation method thereof, wherein the isolation material comprises the following components in percentage by volume:
65% of ceramic powder, 18% of polymer binder and 17% of paraffin;
wherein the specific composition of the ceramic powder is shown in the following table 1, based on 100% of the volume of the ceramic powder; the mass of the polymer binder was 100%, and the specific composition of the polymer binder is shown in table 2 below.
The preparation method of the isolation material comprises the following steps:
(1) Placing ceramic powder, polymer binder and paraffin wax into a high-speed stirrer, and mixing at 180 ℃ for 110min to obtain a mixture;
(2) And (3) adding the mixture obtained in the step (1) into a screw extruder, extruding wires through a die, winding wires through a disc device, and collecting the wires into coiled wires to obtain the isolation material, wherein the temperature of a feeding section of the screw extruder is 50 ℃, the temperature of a compression section is 130 ℃, the temperature of a homogenizing section is 150 ℃, the temperature of a machine head is 180 ℃, the temperature of the die section is 180 ℃, and the diameter of the wires is 2.2mm.
The preparation method of the metal 3D printing part comprises the following steps:
(A) Adopting a 3D printer with two 3D printing nozzles, firstly using a first nozzle, printing a printing material on a lower support piece according to a digital model of a metal 3D printing part, then heating and melting an isolation material through a second nozzle of the printer under control of a computer, printing a layer of isolation layer on the lower support piece, printing the metal part above the isolation layer by adopting the printing material, and continuing to repeat the above process when encountering a part needing to be supported until the printing according to the digital model of the metal 3D printing part is completed, so as to obtain a green mould, wherein the temperature of the nozzle of the 3D printer is 230 ℃, the temperature of a hot bed is 100 ℃, and the thickness of each isolation layer is 0.10mm;
(B) Soaking the green mould obtained in the step (A) in tetrachloroethylene for 16 hours at 100 ℃ for soaking degreasing, and then drying at 70 ℃ for 6 hours to obtain a brown mould;
(C) Placing the palm mould obtained in the step (B) in a vacuum furnace, raising the temperature from 25 ℃ to 270 ℃ at a heating rate of 5 ℃/min, and preserving the heat for 5 hours, wherein pure argon is required to be introduced into the furnace during the heating and the heat preservation, the purity of the argon is 99.999%, and the flow of the argon is 80L/min; then heating to 900 ℃ at a heating rate of 6 ℃/min, and preserving heat for 8 hours, wherein no gas is filled in the stage; heating to 1300 ℃ at a heating rate of 4 ℃/min, preserving heat for 8 hours, and filling argon and hydrogen mixed gas into the furnace at the stage, wherein the volume ratio of the argon to the hydrogen is 5:95, and the gas flow is 65L/min; and finally, cooling to 25 ℃ at a cooling rate of 5-8 ℃/min, cooling along with the furnace, and filling pure argon into the furnace at the cooling stage, wherein the argon flow is 50L/min, so as to finish vacuum sintering, and removing the support piece to obtain the metal 3D printing part.
Example 4
The present embodiment provides an insulating material, a metal 3D printing part and a method for manufacturing the same, which are different from embodiment 1 in that:
the isolating material comprises the following components in percentage by volume: 58% of ceramic powder, 25% of polymer binder and 17% of paraffin wax;
wherein the specific composition of the ceramic powder is shown in the following table 1, based on 100% of the volume of the ceramic powder; the mass of the polymer binder is 100%, and the specific composition of the polymer binder is shown in the following table 2;
the preparation method of the isolation material comprises the following steps:
(1) Placing ceramic powder, polymer binder and paraffin wax into a high-speed stirrer, and mixing at 155 ℃ for 150min to obtain a mixture;
(2) Adding the mixture obtained in the step (1) into a screw extruder, extruding wires through a die, winding wires through a disc device, and collecting the wires into coiled wires to obtain the isolation material, wherein the temperature of a feeding section of the screw extruder is 20 ℃, the temperature of a compression section is 100 ℃, the temperature of a homogenizing section is 120 ℃, the temperature of a machine head is 155 ℃, the temperature of the die section is 155 ℃, and the diameter of the wires is 1.6mm;
other conditions were the same as in example 1.
Example 5
The present embodiment provides an insulating material, a metal 3D printing part and a method for manufacturing the same, which are different from embodiment 1 in that:
the isolating material comprises the following components in percentage by volume: 65% of ceramic powder, 25% of polymer binder and 10% of paraffin;
wherein the specific composition of the ceramic powder is shown in the following table 1, based on 100% of the volume of the ceramic powder; the mass of the polymer binder is 100%, and the specific composition of the polymer binder is shown in the following table 2;
the preparation method of the isolation material comprises the following steps:
(1) Placing ceramic powder, a polymer binder and paraffin wax into a high-speed stirrer, and mixing for 110min at 185 ℃ to obtain a mixture;
(2) Adding the mixture obtained in the step (1) into a screw extruder, extruding wires through a mouth die, winding wires through a disc device, and collecting the wires into coiled wires to obtain the isolation material, wherein the temperature of a feeding section of the screw extruder is 40 ℃, the temperature of a compression section is 120 ℃, the temperature of a homogenizing section is 160 ℃, the temperature of a machine head is 185 ℃, the temperature of the mouth die section is 185 ℃, and the diameter of the wires is 2.4mm;
other conditions were the same as in example 1.
Example 6
The present embodiment provides an insulating material, a metal 3D printing part and a method for manufacturing the same, which are different from embodiment 1 in that:
the isolating material comprises the following components in percentage by volume: 58% of ceramic powder, 18% of polymer binder and 24% of paraffin wax;
wherein the specific composition of the ceramic powder is shown in the following table 1, based on 100% of the volume of the ceramic powder; the mass of the polymer binder is 100%, and the specific composition of the polymer binder is shown in the following table 2;
other conditions were the same as in example 1.
Examples 7 to 11
Examples 7-11 provide a release material, a metal 3D printed part, and a method of making the same, differing from example 1 in the composition and content of the polymeric binder, as described in table 2, with the other conditions being the same as example 1.
Example 12
The present embodiment provides an insulating material, a metal 3D printed part and a method for manufacturing the same, which are different from embodiment 1 in that the method for manufacturing the metal 3D printed part does not include step (B), and other conditions are the same as embodiment 1.
Example 13
The present embodiment provides an insulating material, a metal 3D printed part and a method for manufacturing the same, which are different from embodiment 1 in that the method for manufacturing the metal 3D printed part does not include step (C), and other conditions are the same as embodiment 1.
Comparative example 1
This comparative example provides a metal 3D printing part and a method of manufacturing the same, differing from example 1 in that the support and the metal 3D printing part are not provided with a spacer layer, and the other conditions are the same as example 1.
TABLE 1
A1 2 O 3 /(%) | ZrO 2 /(%) | SiO 2 /(%) | |
Example 1 | 48 | 30 | 22 |
Example 2 | 55 | 29 | 16 |
Example 3 | 57 | 28 | 15 |
Example 4 | 46 | 24 | 30 |
Example 5 | 50 | 32 | 28 |
Example 6 | 57 | 32 | 11 |
Example 7 | 48 | 30 | 22 |
Example 8 | 48 | 30 | 22 |
Example 9 | 48 | 30 | 22 |
Example 10 | 48 | 30 | 22 |
Example 11 | 48 | 30 | 22 |
Example 12 | 48 | 30 | 22 |
Example 13 | 48 | 30 | 22 |
Comparative example 1 | / | / | / |
TABLE 2
The performance of the metallic 3D printed parts provided in the above examples and comparative examples was tested as follows:
difficulty level of removal of support: comparing the difficulty level of removing the support during the preparation of the metal 3D printed part of the above examples and comparative examples, wherein:
easy to: the printing part can be separated from the support piece without using auxiliary tools manually;
it is difficult to: manually using auxiliary tools (such as pliers) to separate the printing element from the support;
difficult: the printing element is separated from the support by machining.
Appearance: and observing whether the support piece material remains on the surface of the prepared metal 3D printing part.
The performance test results of the metal 3D printed parts provided in the above examples and comparative examples are shown in table 3:
TABLE 3 Table 3
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From the contents of table 3, through the design of the components of the isolation material, the design of the components of the polymer binder is further adopted, the prepared isolation material is suitable for the preparation of metal 3D printing parts, and can be further used for preparing an isolation layer between a support piece and the metal 3D printing parts, so that the support piece and the metal 3D printing parts can be quickly separated, the support piece cannot remain on the metal 3D printing parts, and meanwhile, the situation that the metal 3D printing parts collapse in the process of removing the support piece can be guaranteed.
Compared with example 1, if the polymer binder for preparing the release material does not contain polystyrene, high-density polyethylene, ethylene-vinyl acetate copolymer, polyethylene glycol or stearic acid (examples 7-11), the prepared release material is not suitable for being used as a release material for metal 3D printing parts, and thus the prepared metal 3D printing parts can cause adhesion between the 3D printing body and the support, and require manual removal by using auxiliary tool pliers or other auxiliary tools.
In contrast to example 1, if no degreasing soak or vacuum sintering is performed during the preparation of the metal 3D printed part (examples 12-13), the final target metal 3D printed part cannot be obtained.
Compared with example 1, if no isolation layer is provided in the process of preparing the metal 3D printing part (comparative example 1), the support needs to be removed by means of machining, and the prepared metal 3D printing part has a support material residue on the surface.
The applicant states that the detailed process flow of the present invention is illustrated by the above examples, but the present invention is not limited to the above detailed process flow, i.e. it does not mean that the present invention must be implemented depending on the above detailed process flow. It should be apparent to those skilled in the art that any modification of the present invention, equivalent substitution of raw materials for the product of the present invention, addition of auxiliary components, selection of specific modes, etc., falls within the scope of the present invention and the scope of disclosure.
Claims (20)
1. An insulation material, characterized in that the insulation material comprises the following components in percentage by volume:
58-65% of ceramic powder, 18-25% of polymer binder and 10-24% of paraffin;
wherein, based on the mass of the polymer binder being 100%, the polymer binder comprises the following components in percentage by mass: 58-65% of polystyrene, 6-10% of high-density polyethylene, 7-12% of ethylene-vinyl acetate copolymer, 8-26% of polyethylene glycol and 3-5% of stearic acid.
2. The insulation material of claim 1, wherein the ceramic powder is selected from A1 2 O 3 、ZrO 2 Or SiO 2 Any one or a combination of at least two of these.
3. The insulation material of claim 2, wherein the ceramic powder comprises A1 2 O 3 、ZrO 2 And SiO 2 Is a group of (2)And (b) adding A1 to the ceramic powder in an amount of 100% by volume of the ceramic powder 2 O 3 46-57% by volume of ZrO in the ceramic powder 2 24-32% by volume of SiO in the ceramic powder 2 The volume percentage of (2) is 11-30%.
4. The insulation material of claim 1, wherein D of the ceramic powder 50 The grain diameter is 3-5 mu m.
5. A method of producing the insulation material according to any one of claims 1 to 4, comprising the steps of:
(1) Placing ceramic powder, a polymer binder and paraffin into a high-speed stirrer for mixing to obtain a mixture;
(2) And (3) adding the mixture obtained in the step (1) into a screw extruder, extruding the wire through a die, and winding the wire into a coiled wire through a disc device to obtain the isolation material.
6. The method according to claim 5, wherein the temperature of the mixing is 155 to 185 ℃.
7. The method according to claim 5, wherein the mixing time is 110 to 150 minutes.
8. The method of claim 5, wherein the post-mixing further comprises a post-treatment step.
9. The method of claim 8, wherein the post-treatment is cooling to room temperature.
10. The preparation method according to claim 5, wherein the temperature of the feeding section of the screw extruder is 25-50 ℃, the temperature of the compression section is 100-130 ℃, the temperature of the homogenizing section is 120-160 ℃, the temperature of the head is 155-185 ℃, and the temperature of the die section is 155-185 ℃.
11. The method according to claim 5, wherein the extruded wire has a wire diameter of 1.6 to 2.4mm.
12. The preparation method of the metal 3D printing part is characterized by comprising the following steps of:
(A) Adopting a 3D printer with two 3D printing nozzles, firstly using a first nozzle, printing a printing material on a lower support piece according to a digital model of a metal 3D printing part, then heating and melting an isolation material through a second nozzle of the printer under control of a computer, printing a layer of isolation layer on the lower support piece, printing the metal part above the isolation layer by adopting the printing material, and continuing to repeat the above process when encountering a part needing to be supported until the printing according to the digital model of the metal 3D printing part is completed, so as to obtain a green mould;
(B) Soaking and degreasing the green mould obtained in the step (A), and drying to obtain a brown mould;
(C) Vacuum sintering the palm die obtained in the step (B) to remove the supporting piece, thereby obtaining the metal 3D printing part;
wherein the insulation material comprises the insulation material of any one of claims 1-4.
13. The method of claim 12, wherein the 3D printer is configured to print the separator at a nozzle temperature of 200-240 ℃ and a hot bed temperature of 85-110 ℃.
14. The method of claim 12, wherein the spacer layer has a thickness of 0.050 to 0.150mm.
15. The method of claim 12, wherein the dip degreasing solvent is tetrachloroethylene and/or trans-1, 2-dichloroethylene.
16. The method of claim 12, wherein the soaking degreasing temperature is 80-120 ℃.
17. The method of claim 12, wherein the soaking degreasing time is 12-24 hours.
18. The method of claim 12, wherein the drying temperature is 60-70 ℃.
19. The method of claim 12, wherein the drying time is from 6 to 12 hours.
20. A metal 3D printed part made by the method of any one of claims 12-19.
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