CN114570939A - Hard alloy material system for 3D printing and 3D printing method - Google Patents
Hard alloy material system for 3D printing and 3D printing method Download PDFInfo
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- CN114570939A CN114570939A CN202210234753.3A CN202210234753A CN114570939A CN 114570939 A CN114570939 A CN 114570939A CN 202210234753 A CN202210234753 A CN 202210234753A CN 114570939 A CN114570939 A CN 114570939A
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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
- B22F10/14—Formation of a green body by jetting of binder onto a bed of metal powder
-
- 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
- B22F10/60—Treatment of workpieces or articles after build-up
- B22F10/64—Treatment of workpieces or articles after build-up by thermal means
-
- 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
- B22F3/1017—Multiple heating or additional steps
- B22F3/1021—Removal of binder or filler
-
- 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
- B33Y10/00—Processes of additive manufacturing
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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
- B33Y40/20—Post-treatment, e.g. curing, coating or polishing
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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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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
- C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
- C22C29/067—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds comprising a particular metallic binder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
- C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
- C22C29/08—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds based on tungsten carbide
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Abstract
The invention discloses a hard alloy material system for 3D printing and a 3D printing method, wherein the hard alloy material system comprises the following components in parts by mass: 0.5-3 parts of chromium carbide, and the balance of WC-Co/Ni/Fe hard alloy composite material powder, wherein the WC-Co/Ni/Fe hard alloy composite material powder is spherical or spheroidal or other-shaped particles, the granularity of the WC-Co/Ni/Fe hard alloy composite material powder is 5-150 mu m, and the granularity of the chromium carbide powder is 0.2-3 mu m. The density of the hard alloy sample piece obtained by the 3D printing method reaches 99% or more than 99%, WC crystal grains are obviously refined and uniformly distributed, and the WC crystal grains do not grow abnormally.
Description
Technical Field
The invention relates to the technical field of additive manufacturing, in particular to a hard alloy material system for 3D printing and a 3D printing method.
Background
The hard alloy is a composite material prepared by a powder metallurgy process from hard compounds (such as WC) of refractory metals and bonding metals (such as Fe, Co and Ni), has a series of excellent performances of high hardness, wear resistance, good strength and toughness, heat resistance, corrosion resistance and the like, and is widely applied to the fields of cutting tools, hardware molds, aerospace parts and the like. However, the traditional hard alloy preparation has long production period, hard alloy workpieces with complex shapes are difficult to prepare, the shapes are also limited by molds, a plurality of sets of molds are required to be prepared, and the cost is increased. Therefore, the traditional hard alloy preparation technology cannot meet the industrial requirement of high-speed development.
The Binder Jetting technology (Binder Jetting) is an advanced additive manufacturing technology capable of generating tiny liquid drops through a nozzle to be jetted to a tiled powder layer, and then circularly and repeatedly carrying out the processes of powder layering layer by layer and jet printing to obtain a printed piece. After the binder is sprayed and formed into a printing piece, the binder needs to be solidified at a certain temperature, and then the printing green body is degreased, sintered and the like. The technology has the advantages of low cost, high printing speed, high printing precision, capability of printing large-size samples and the like, and therefore, the technology becomes a preferred technology for hard alloy additive manufacturing.
However, when the binder spray forming technology is used to prepare the hard alloy material, abnormal growth of WC crystal grains is easily generated in the sintering process, and the mechanical properties of the hard alloy are seriously influenced.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a hard alloy material system for 3D printing, which mixes WC-Co/Ni/Fe hard alloy composite material powder with chromium carbide powder, so that the chromium carbide powder is distributed in a contact area between the WC-Co/Ni/Fe hard alloy composite material powder, and abnormal growth of WC grains can be effectively inhibited in the sintering process; the technical scheme is as follows:
a hard alloy material system for 3D printing comprises the following components in parts by mass: 0.5-3 parts of chromium carbide, and the balance of WC-Co/Ni/Fe hard alloy composite material powder, wherein the WC-Co/Ni/Fe hard alloy composite material powder is spherical or spheroidal or other-shaped particles, the granularity of the WC-Co/Ni/Fe hard alloy composite material powder is 5-150 mu m, and the granularity of the chromium carbide powder is 0.2-3 mu m. The mass part of the chromium carbide is preferably 0.5-1 part.
The WC-Co/Ni/Fe hard alloy composite material powder is mixed with the chromium carbide powder, so that chromium carbide is distributed in a mutual contact area between the WC-Co/Ni/Fe hard alloy composite material powder, and then printing and sintering are carried out, so that the abnormal growth of WC grains can be inhibited. However, if the chromium carbide is uniformly distributed in the WC-Co/Ni/Fe hard alloy composite material powder rather than outside, the WC crystal grains are abnormally grown after printing and sintering.
Preferably, the WC-Co/Ni/Fe hard alloy composite material powder comprises: 80-94 parts of tungsten carbide and 6-20 parts of Co/Ni/Fe.
Preferably, the WC-Co/Ni/Fe hard alloy composite material powder has a WC grain size of 0.1-3 μm.
Preferably, the chromium carbide can be replaced by one or at least two of vanadium carbide, molybdenum carbide, niobium carbide, tantalum carbide and titanium carbide; the chromium carbide can also be replaced by a mixture of chromium carbide and at least one of vanadium carbide, molybdenum carbide, niobium carbide, tantalum carbide and titanium carbide.
The invention also provides a 3D printing method, which comprises the following steps:
s1, providing raw materials according to the hard alloy material system for 3D printing, uniformly mixing to obtain a premix, and placing the premix in a printing bin;
s2, slicing the three-dimensional structure of the printed piece layer by layer according to the set layer thickness, defining printing parameters and printing strategies; obtaining slice information of each layer of the three-dimensional structure of the printed piece from bottom to top;
s3 spreading the premix in the printing stock bin to a workbench according to a certain powder spreading layer thickness to obtain the current layer;
s4, adopting a binder spray forming process, and spraying, permeating and drying the binder according to the current layer structure information of the printed matter; the printing environment is normal-pressure atmosphere;
s5, repeating the steps S3-S4 to obtain a green printing part;
s6, carrying out curing treatment on the green printing part obtained in the step S5 and removing unformed powder;
and S7, degreasing the green printing part solidified in the step S6, then carrying out vacuum sintering or air pressure sintering, and cooling along with a furnace to obtain the required hard alloy sample.
Preferably, the binder in step S4 is a water-based or organic solvent adhesive, and the saturation degree of the binder is 60% to 100%.
Preferably, the penetration time of the binder in the step S4 is 2-10S; the drying time of the binder is 10-20 s.
Preferably, the thickness of the powder layer in the step s3 is 20-400 μm.
Preferably, in the step S6, the curing temperature is 180-200 ℃, and the heat preservation time is 6-8 h; in the step S7, the degreasing sintering temperature is 300-1000 ℃, and the heat preservation time is 45-180 min.
Preferably, in the step S7, the vacuum sintering temperature is 1350-1500 ℃, the heat preservation time is 30-180 min, and the vacuum degree is 0.01-100 Pa. Most preferably, in the step S7, the vacuum sintering temperature is 1430 ℃, the heat preservation time is 90min, and the vacuum degree is 1-2 Pa.
Preferably, in the step S7, the sintering temperature of the gas is 1350-1500 ℃, the heat preservation time is 30-180 min, the gas is pure argon, and the pressure is i-10 MPa. Most preferably, in the step S7, the sintering temperature is 1430-1490 ℃, the heat preservation time is 90-180 min, the gas is pure argon, and the pressure is 2-4 MPa.
According to the hard alloy material system, chromium carbide is distributed in a void area formed between overlapped powder particles of the WC-Co/Ni/Fe hard alloy composite material, when the hard alloy material system is used for binder jet printing, abnormal growth of WC grains can be effectively prevented in a sintering process, and the hardness of the prepared hard alloy is obviously enhanced compared with that of a material without the chromium carbide; and when the mass part of the chromium carbide is 0.5-1, the density of the hard alloy prepared by the WC-Co/Ni/Fe hard alloy composite material system added with the chromium carbide is higher than that of a product without the chromium carbide.
Drawings
FIG. 1 is an electron micrograph of a cemented carbide sample prepared in example 2;
fig. 2 is an electron micrograph of a cemented carbide sample prepared in comparative example 2.
Detailed Description
The present invention is explained in detail below using specific examples, which are not intended to limit the present invention in any way, and any modifications within the spirit and scope of the present invention are within the scope of the present invention.
Example 1
The embodiment comprises the following steps:
(A) providing a material: according to the mass percentage, 0.5 part of chromium carbide (the grain size of FSSS powder is 0.2 micron), and the balance of spherical or nearly spherical WC-6Co hard alloy material grains with the grain size of 5-30 microns, wherein the size of WC grains in the grains is 1 micron;
(B) mixing materials: adding alcohol and hard alloy balls into the raw materials according to the proportion, mixing, wherein the volume ratio of the alcohol to the raw material powder is 1: 1, the mass of the hard alloy balls is 1-2 times of the total mass of the raw material powder, the ball milling time is 30 minutes, the ball milling speed is 200 revolutions per minute, obtaining dry mixed powder through a rotary evaporator, and finally drying in an oven at 70 ℃ for 6-12 hours to obtain a uniformly dried mixture;
(C) placing the mixed powder material into a bin of a binder jet printing machine, and spreading material particles to a workbench through a powder spreading device to obtain a current layer, wherein the powder spreading thickness is 20 microns;
(D) the saturation degree of the adopted binder is 60%, the current section of the hard alloy printing piece is subjected to jet printing, the permeation time of the binder is 2 seconds, the drying temperature is 180 ℃, and the drying time is 5 seconds;
(E) c, paving material particles on the section layer again, and repeating the steps C-D to obtain a green blank of the printing part;
(F) and (3) curing: curing the green body of the printed part at the curing temperature of 180 ℃ for 8 hours, and sweeping the unformed powder after the curing is finished to obtain a cured part;
(G) and (3) sintering: and introducing argon gas for degreasing and sintering, wherein the degreasing temperature is 300 ℃, keeping the temperature for 180 minutes, then sintering, the highest temperature is 1490 ℃, keeping the temperature for 30 minutes, introducing 2MPa argon gas for atmospheric pressure sintering, keeping the temperature for 180 minutes, and finally cooling along with a furnace to obtain the required hard alloy sintered piece.
Example 2
The embodiment comprises the following steps:
(A) providing a material: according to the mass percentage, 1 part of chromium carbide (the grain size of FSSS powder is 0.5 micron), and the balance of spherical or nearly spherical WC-15Co hard alloy material particles with the grain size of 15-50 microns, wherein the size of WC grains in the particles is 1 micron;
(B) mixing materials: adding alcohol and hard alloy balls into the raw materials according to the proportion, mixing, wherein the volume ratio of the alcohol to the raw material powder is 1: 1, the mass of the hard alloy balls is 1-2 times of the total mass of the raw material powder, the ball milling time is 30 minutes, the ball milling speed is 200 revolutions per minute, obtaining dry mixed powder through a rotary evaporator, and finally drying in an oven at 70 ℃ for 6-12 hours to obtain a uniformly dried mixture;
(C) placing the mixed powder material into a bin of a binder jet printing machine, and spreading material particles to a workbench through a powder spreading device to obtain a current layer, wherein the powder spreading thickness is 45 microns;
(D) the saturation degree of the adopted binder is 80%, the current section of the hard alloy printing piece is subjected to jet printing, the permeation time of the binder is 5 seconds, the drying temperature is 180 ℃, and the drying time is 10 seconds;
(E) c, paving material particles on the section layer again, and repeating the steps C-D to obtain a green blank of the printing part;
(F) and (3) curing: curing the green body of the printed part at the curing temperature of 200 ℃ for 6 hours, and sweeping the unformed powder after the curing is finished to obtain a cured part;
(G) and (3) sintering: and introducing argon gas for degreasing and sintering, wherein the degreasing temperature is 300 ℃, preserving heat for 180 minutes, then sintering, the maximum temperature is 1430 ℃, preserving heat for 90 minutes, introducing argon gas with the pressure of 4MPa for air pressure sintering, preserving heat for 90 minutes, and finally cooling along with a furnace to obtain the required hard alloy sintered part.
Example 3
The embodiment comprises the following steps:
(A) providing a material: according to the mass percentage, 1 part of chromium carbide (the grain size of FSSS powder is 0.5 micron), and the balance of spherical or nearly spherical WC-20Co hard alloy material particles with the grain size of 30-70 microns, wherein the size of WC grains in the particles is 1 micron;
(B) mixing materials: adding alcohol and hard alloy balls into the raw materials according to the proportion, mixing, wherein the volume ratio of the alcohol to the raw material powder is 1: 1, the mass of the hard alloy balls is 1-2 times of the total mass of the raw material powder, the ball milling time is 30 minutes, the ball milling speed is 200 revolutions per minute, obtaining dry mixed powder through a rotary evaporator, and finally drying in an oven at 70 ℃ for 6-12 hours to obtain a uniformly dried mixture;
(C) placing the mixed powder material into a bin of a binder jet printing machine, and flatly paving material particles to a workbench through a powder paving device to obtain a current layer, wherein the powder paving thickness is 65 micrometers;
(D) the saturation degree of the adopted binder is 100%, the current section of the hard alloy printing piece is subjected to jet printing, the permeation time of the binder is 10 seconds, the drying temperature is 180 ℃, and the drying time is 15 seconds;
(E) c, paving material particles on the section layer again, and repeating the steps C-D to obtain a green blank of the printing part;
(F) and (3) curing: curing the green body of the printed part at the curing temperature of 200 ℃ for 6 hours, and sweeping the unformed powder after the curing is finished to obtain a cured part;
(G) and (3) sintering: and introducing argon gas for degreasing and sintering, wherein the degreasing temperature is 300 ℃, preserving the temperature for 180 minutes, then sintering, the highest temperature is 1350 ℃, preserving the temperature for 180 minutes, introducing 6MPa argon gas for air pressure sintering, preserving the temperature for 60 minutes, and finally cooling along with the furnace to obtain the required hard alloy sintered piece.
Example 4
The embodiment comprises the following steps:
(A) providing a material: according to the mass percentage, 0.5 part of chromium carbide (the grain size of FSSS powder is 0.2 micron), and the balance of spherical or nearly spherical WC-6Ni hard alloy material particles with the grain size of 50-100 microns, wherein the size of WC crystal grains in the particles is 1 micron;
(B) mixing materials: adding alcohol and hard alloy balls into the raw materials according to the proportion, mixing, wherein the volume ratio of the alcohol to the raw material powder is 1: 1, the mass of the hard alloy balls is 1-2 times of the total mass of the raw material powder, the ball milling time is 30 minutes, the ball milling speed is 200 revolutions per minute, obtaining dry mixed powder through a rotary evaporator, and finally drying in an oven at 70 ℃ for 6-12 hours to obtain a uniformly dried mixture;
(C) placing the mixed powder material into a bin of a binder jet printing machine, and spreading material particles to a workbench through a powder spreading device to obtain a current layer, wherein the powder spreading thickness is 100 microns;
(D) the saturation degree of the adopted binder is 100%, the current section of the hard alloy printing piece is subjected to jet printing, the permeation time of the binder is 15 seconds, the drying temperature is 180 ℃, and the drying time is 20 seconds;
(E) c, paving material particles on the section layer again, and repeating the steps C-D to obtain a green blank of the printing part;
(F) and (3) curing: curing the green body of the printed part at the curing temperature of 180 ℃ for 8 hours, and sweeping the unformed powder after the curing is finished to obtain a cured part;
(G) and (3) sintering: and introducing argon gas for degreasing and sintering, wherein the degreasing temperature is 500 ℃, keeping the temperature for 90 minutes, then sintering, the highest temperature is 1490 ℃, keeping the temperature for 30 minutes, introducing argon gas with the pressure of 8MPa for pressure sintering, keeping the temperature for 45 minutes, and finally cooling along with a furnace to obtain the required hard alloy sintered piece.
Example 5
The embodiment comprises the following steps:
(A) providing a material: according to the mass percentage, 1 part of chromium carbide (the grain size of FSSS powder is 0.2 micron), and the balance of spherical or nearly spherical WC-15Ni hard alloy material particles with the grain size of 70-150 microns, wherein the size of WC crystal grains in the particles is 1 micron;
(B) mixing materials: adding alcohol and hard alloy balls into the raw materials according to the proportion, mixing, wherein the volume ratio of the alcohol to the raw material powder is 1: 1, the mass of the hard alloy balls is 1-2 times of the total mass of the raw material powder, the ball milling time is 30 minutes, the ball milling speed is 200 revolutions per minute, obtaining dry mixed powder through a rotary evaporator, and finally drying in an oven at 70 ℃ for 6-12 hours to obtain a uniformly-dried mixture;
(C) placing the mixed powder material into a bin of a binder jet printing machine, and spreading material particles to a workbench through a powder spreading device to obtain a current layer, wherein the powder spreading thickness is 150 microns;
(D) the saturation degree of the adopted binder is 100%, the current section of the hard alloy printing piece is subjected to jet printing, the permeation time of the binder is 15 seconds, the drying temperature is 180 ℃, and the drying time is 15 seconds;
(E) c, paving material particles on the section layer again, and repeating the steps C-D to obtain a green blank of the printing part;
(F) and (3) curing: curing the green body of the printed part at 200 ℃ for 6 hours, and then removing the unformed powder to obtain a cured part;
(G) and (3) sintering: and introducing argon gas for degreasing and sintering, wherein the degreasing temperature is 1000 ℃, keeping the temperature for 45 minutes, then sintering, the highest temperature is 1430 ℃, keeping the temperature for 90 minutes, introducing argon gas with the pressure of 4MPa for atmospheric sintering, keeping the temperature for 90 minutes, and finally cooling along with a furnace to obtain the required hard alloy sintered piece.
Example 6
The embodiment comprises the following steps:
(A) providing a material: according to the mass percentage, 1 part of chromium carbide (the grain size of FSSS powder is 0.2 micron), and the balance of spherical or nearly spherical WC-15Fe hard alloy material particles with the grain size of 15-50 microns, wherein the size of WC crystal grains in the particles is 1 micron;
(B) mixing materials: adding alcohol and hard alloy balls into the raw materials according to the proportion, mixing, wherein the volume ratio of the alcohol to the raw material powder is 1: 1, the mass of the hard alloy balls is 1-2 times of the total mass of the raw material powder, the ball milling time is 30 minutes, the ball milling speed is 200 revolutions per minute, obtaining dry mixed powder through a rotary evaporator, and finally drying in an oven at 70 ℃ for 6-12 hours to obtain a uniformly dried mixture;
(C) placing the mixed powder material into a bin of a binder jet printing machine, and spreading material particles to a workbench through a powder spreading device to obtain a current layer, wherein the powder spreading thickness is 50 microns;
(D) the saturation degree of the adopted binder is 60%, the current section of the hard alloy printing piece is subjected to jet printing, the permeation time of the binder is 2 seconds, the drying temperature is 180 ℃, and the drying time is 10 seconds;
(E) c, paving material particles on the section layer again, and repeating the steps C-D to obtain a green blank of the printing part;
(F) and (3) curing: curing the green body of the printed part at 200 ℃ for 6 hours, and then removing the unformed powder to obtain a cured part;
(G) and (3) sintering: and introducing argon gas for degreasing and sintering, wherein the degreasing temperature is 300 ℃, keeping the temperature for 90 minutes, then sintering, the highest temperature is 1430 ℃, keeping the temperature for 90 minutes, introducing 6MPa argon gas for air pressure sintering, keeping the temperature for 60 minutes, and finally cooling along with a furnace to obtain the required hard alloy sintered piece.
Example 7
The embodiment comprises the following steps:
(A) providing a material: according to the mass percentage, 1 part of chromium carbide (the grain size of FSSS powder is 0.2 micron), and the balance of spherical or nearly spherical WC-20Fe hard alloy material particles with the grain size of 30-70 microns, wherein the size of WC crystal grains in the particles is 1 micron;
(B) mixing materials: adding alcohol and hard alloy balls into the raw materials according to the proportion, mixing, wherein the volume ratio of the alcohol to the raw material powder is 1: 1, the mass of the hard alloy balls is 1-2 times of the total mass of the raw material powder, the ball milling time is 30 minutes, the ball milling speed is 200 revolutions per minute, obtaining dry mixed powder through a rotary evaporator, and finally drying in an oven at 70 ℃ for 6-12 hours to obtain a uniformly dried mixture;
(C) placing the mixed powder material into a bin of a binder jet printing machine, and spreading material particles to a workbench through a powder spreading device to obtain a current layer, wherein the powder spreading thickness is 100 microns;
(D) the saturation degree of the adopted binder is 150%, the current section of the hard alloy printing piece is subjected to jet printing, the permeation time of the binder is 5 seconds, the drying temperature is 180 ℃, and the drying time is 15 seconds;
(E) c, paving material particles on the section layer again, and repeating the steps C-D to obtain a green blank of the printing part;
(F) and (3) curing: curing the green body of the printed part at the curing temperature of 180 ℃ for 8 hours, and sweeping the unformed powder after the curing is finished to obtain a cured part;
(G) and (3) sintering: and introducing argon gas for degreasing and sintering, wherein the degreasing temperature is 500 ℃, preserving the temperature for 90 minutes, then sintering, the maximum temperature is 1350 ℃, preserving the temperature for 180 minutes, introducing 10MPa argon gas for air pressure sintering, preserving the temperature for 30 minutes, and finally cooling along with the furnace to obtain the required hard alloy sintered piece.
Example 8
The embodiment comprises the following steps:
(A) providing a material: according to the mass percentage, 3 parts of chromium carbide (the grain size of FSSS powder is 0.2 micron), and the balance of spherical or nearly spherical WC-20Ni hard alloy material particles with the grain size of 15-50 microns, wherein the size of WC crystal grains in the particles is 1 micron;
(B) mixing materials: adding alcohol and hard alloy balls into the raw materials according to the proportion, mixing, wherein the volume ratio of the alcohol to the raw material powder is 1: 1, the mass of the hard alloy balls is 1-2 times of the total mass of the raw material powder, the ball milling time is 30 minutes, the ball milling speed is 200 revolutions per minute, obtaining dry mixed powder through a rotary evaporator, and finally drying in an oven at 70 ℃ for 6-12 hours to obtain a uniformly dried mixture;
(C) placing the mixed powder material into a bin of a binder jet printing machine, and spreading material particles to a workbench through a powder spreading device to obtain a current layer, wherein the powder spreading thickness is 400 microns;
(D) the saturation degree of the adopted binder is 100%, the current section of the hard alloy printing piece is subjected to jet printing, the permeation time of the binder is 10 seconds, the drying temperature is 180 ℃, and the drying time is 10 seconds;
(E) c, paving material particles on the section layer again, and repeating the steps C-D to obtain a green blank of the printing part;
(F) and (3) curing: curing the green body of the printed part at the curing temperature of 180 ℃ for 8 hours, and sweeping the unformed powder after the curing is finished to obtain a cured part;
(G) and (3) sintering: and introducing argon gas for degreasing and sintering, wherein the degreasing temperature is 1000 ℃, preserving the heat for 90 minutes, then carrying out vacuum sintering, the maximum temperature is 1430 ℃, preserving the heat for 90 minutes, the vacuum degree is 1-2 Pa, and finally cooling along with the furnace to obtain the required hard alloy sintered piece.
Comparative example 1
The material is a spherical or nearly spherical WC-6Co hard alloy material particle with the particle size of 5-30 microns, the size of WC crystal grains in the particle is 1 micron, and the printing method and the degreasing sintering method are the same as those in the embodiment 1.
Comparative example 2
The material is a spherical or nearly spherical WC-15Co hard alloy material particle with the particle size of 15-50 microns, the WC grain size in the particle is 1 micron, and the printing method and the degreasing sintering method are consistent with those in the embodiment 2.
Comparative example 3
The material is spherical or nearly spherical WC-20Co hard alloy material particles with the particle size of 30-70 microns, the size of WC crystal grains in the particles is 1 micron, and the printing method and the degreasing sintering method are the same as those in the embodiment 3.
Comparative example 4
The material is spherical or nearly spherical WC-6Ni hard alloy material particles with the particle size of 50-100 microns, the size of WC crystal grains in the particles is 1 micron, and the printing method and the degreasing sintering method are the same as those in the embodiment 2.
Comparative example 5
The material is spherical or nearly spherical WC-15Ni hard alloy material particles with the particle size of 70-150 microns, the size of WC crystal grains in the particles is 1 micron, and the printing method and the degreasing sintering method are the same as those in the embodiment 5.
Comparative example 6
The material is spherical or nearly spherical WC-15Fe hard alloy material particles with the particle size of 15-50 microns, the size of WC crystal grains in the particles is 1 micron, and the printing method and the degreasing sintering method are the same as those in the embodiment 6.
Comparative example 7
The material is spherical or nearly spherical WC-20Fe hard alloy material particles with the particle size of 30-70 microns, the size of WC crystal grains in the particles is 1 micron, and the printing method and the degreasing sintering method are the same as those in the embodiment 7.
Comparative example 8
The material is spherical or nearly spherical WC-20Ni hard alloy material particles with the particle size of 15-50 microns, the size of WC crystal grains in the particles is 1 micron, and the printing method and the degreasing sintering method are the same as those in the embodiment 8.
Performance testing
The density and hardness of the cemented carbide sintered pieces prepared in examples 1 to 8 and comparative examples 1 to 8 of the present invention and the abnormal growth of WC grains were measured, and the specific results are shown in table 1, and the specific test method is as follows:
the density method comprises the following steps: and carrying out water bath treatment on the sintered part, wherein the water bath temperature is 80-100 ℃, the water bath time is 0.5-2.5 h, and then carrying out density measurement on the sintered part by using an Archimedes drainage method.
Vickers hardness test method: cutting the sample piece by using a cutting machine, polishing the cut section by using a metallographic polishing machine, wiping the polished surface, placing on a Vickers hardness tester, and testing by adopting the national standard GB/T4340.1-2009.
The abnormal growth of WC crystal grains is observed by cutting and polishing the sintered piece and placing the sintered piece in a scanning electron microscope for observation.
Wherein, the electron microscope image of the hard alloy sample prepared in the example 2 is shown in fig. 1; an electron micrograph of the cemented carbide sample prepared in comparative example 2 is shown in fig. 2. The comparison of the electron micrographs of other examples and corresponding comparative examples also shows the effect of comparing example 2 and comparative example 2.
As can be seen from Table 1, the density of the hard alloy sample prepared in the embodiments 1-8 of the present invention reaches about 99%, the density is nearly fully dense, WC grains are obviously refined and uniformly distributed (as shown in FIG. 1), and no WC grains grow abnormally. In comparative examples 1 to 8 in which Cr3C2 was not added, WC grains grew abnormally and severely (as shown in fig. 2), and the hardness of the prepared cemented carbide was significantly lower than that of the examples. Therefore, the Cr3C2 is added on the basis of WC-Co/Ni/Fe in the design of the hard alloy material, so that the abnormal growth of WC crystal grains can be effectively inhibited, and the mechanical property of the hard alloy manufactured by additive manufacturing is obviously improved. And when the mass part of the added chromium carbide is 0.5-1, the density of the hard alloy prepared by the WC-Co/Ni/Fe hard alloy mixed powder added with the chromium carbide is higher than that of a product without the chromium carbide.
Table 1 hard alloy performance parameters prepared by the examples of the invention and their comparative parameters
| Scheme(s) | Material | Density (%) | Hardness (HV30) | Whether WC crystal grains grow abnormally or not |
| Example 1 | WC-6Co-0.5Cr3C2 | 99.65 | 1810 | Whether or not |
| Example 2 | WC-15Co-1.0Cr3C2 | 99.54 | 1288 | Whether or not |
| Example 3 | WC-20Co-3.0Cr3C2 | 99.88 | 1122 | Whether or not |
| Example 4 | WC-6Ni-0.5Cr3C2 | 99.81 | 1753 | Whether or not |
| Example 5 | WC-15Ni-1.0Cr3C2 | 99.63 | 1194 | Whether or not |
| Example 6 | WC-15Fe-3.0Cr3C2 | 99.34 | 1058 | Whether or not |
| Example 7 | WC-20Fe-1.0Cr3C2 | 99.57 | 986 | Whether or not |
| Example 8 | WC-20Ni-3.0Cr3C2 | 98.63 | 1023 | Whether or not |
| Comparative example 1 | WC-6Co | 99.57 | 1552 | Abnormal growth and severity of the disease |
| Comparative example 2 | WC-15Co | 99.42 | 1123 | Abnormal growth and severity |
| Comparative example 3 | WC-20Co | 99.89 | 1068 | Abnormal growth and severity |
| Comparative example 4 | WC-6Ni | 99.76 | 1436 | Abnormal growth and severity |
| Comparative example 5 | WC-15Ni | 99.19 | 1009 | Abnormal growth and severity |
| Comparative example 6 | WC-15Fe | 99.38 | 976 | Abnormal growth and severity |
| Comparative example 7 | WC-20Fe | 99.51 | 915 | Abnormal growth and severity |
| Comparative example 8 | WC-20Ni | 98.68 | 998 | Abnormal growth and severity |
Claims (10)
1. A cemented carbide material system for 3D printing, characterized by: the adhesive comprises the following components in parts by mass: 0.5-3 parts of chromium carbide, and the balance of WC-Co/Ni/Fe hard alloy composite material powder, wherein the WC-Co/Ni/Fe hard alloy composite material powder is spherical or spheroidal particles or powder with other shapes, the granularity of the WC-Co/Ni/Fe hard alloy composite material powder is 5-150 mu m, and the granularity of the chromium carbide powder is 0.2-3 mu m.
2. The cemented carbide material system for 3D printing according to claim 1, characterized in that: the WC-Co/Ni/Fe hard alloy composite material powder comprises: 80-94 parts of tungsten carbide and 6-20 parts of Co/Ni/Fe.
3. The cemented carbide material system for 3D printing according to claim 2, characterized in that: the chromium carbide may be replaced with vanadium carbide, molybdenum carbide, niobium carbide, tantalum carbide, or titanium carbide.
4. The cemented carbide material system for 3D printing according to claim 2, characterized in that: the WC-Co/Ni/Fe hard alloy composite material powder has WC grain size of 0.1-3 μm.
5. A3D printing method is characterized in that: the method comprises the following steps:
s1, providing raw materials according to the hard alloy material system for 3D printing as claimed in any one of claims 1-4, uniformly mixing to obtain a premix, and placing the premix in a printing bin;
s2, slicing the three-dimensional structure of the printed piece layer by layer according to the set layer thickness, defining printing parameters and printing strategies; obtaining slice information of each layer of the three-dimensional structure of the printed piece from bottom to top;
s3, spreading the premix in the printing bin to a workbench according to a certain powder spreading layer thickness to obtain a current layer;
s4, adopting a binder spray forming process, and spraying, permeating and drying the binder according to the current layer structure information of the printed matter; the printing environment is normal-pressure atmosphere;
s5, repeating the steps S3-S4 to obtain a green printing part;
s6, carrying out curing treatment on the green printing part obtained in the step S5 and removing unformed powder;
and S7, degreasing the green printing part solidified in the step S6, then carrying out vacuum sintering or air pressure sintering, and cooling along with a furnace to obtain the required hard alloy sample.
6. The 3D printing method according to claim 5, characterized in that: the binder in the step S4 is a water-based or organic solvent adhesive, and the saturation of the binder is 60-100%; the penetration time of the binder is 2-10 s; the drying time of the binder is 10-20 s.
7. The 3D printing method according to claim 5, characterized in that: the thickness of the powder spreading layer in the step S3 is 20-400 μm.
8. The 3D printing method according to claim 5, characterized in that: in the step S6, the curing temperature is 1g 0-200 ℃, and the heat preservation time is 6-8 h; in the step S7, the degreasing temperature is 300-1000 ℃, and the heat preservation time is 45-180 min.
9. The 3D printing method according to claim 5, characterized in that: in the step S7, the vacuum sintering temperature is 1350-1500 ℃, the heat preservation time is 30-180 min, and the vacuum degree is 0.01-100 Pa.
10. The 3D printing method according to claim 5, characterized in that: in the step S7, the gas pressure sintering temperature is 1350-1500 ℃, the heat preservation time is 30-180 min, the gas is pure argon, and the pressure intensity is 1-10 MPa.
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