CN116000310A - Preparation method of zirconium ferrovanadium getter based on 3D printing and zirconium ferrovanadium getter - Google Patents
Preparation method of zirconium ferrovanadium getter based on 3D printing and zirconium ferrovanadium getter Download PDFInfo
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- CN116000310A CN116000310A CN202310057595.3A CN202310057595A CN116000310A CN 116000310 A CN116000310 A CN 116000310A CN 202310057595 A CN202310057595 A CN 202310057595A CN 116000310 A CN116000310 A CN 116000310A
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- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 title claims abstract description 81
- 229910052726 zirconium Inorganic materials 0.000 title claims abstract description 81
- 229910000628 Ferrovanadium Inorganic materials 0.000 title claims abstract description 75
- PNXOJQQRXBVKEX-UHFFFAOYSA-N iron vanadium Chemical compound [V].[Fe] PNXOJQQRXBVKEX-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 238000010146 3D printing Methods 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 124
- 238000000034 method Methods 0.000 claims abstract description 36
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 29
- 239000000956 alloy Substances 0.000 claims abstract description 29
- 239000007921 spray Substances 0.000 claims abstract description 25
- 239000011230 binding agent Substances 0.000 claims abstract description 23
- 238000005245 sintering Methods 0.000 claims abstract description 23
- ZGTNJINJRMRGNV-UHFFFAOYSA-N [V].[Fe].[Zr] Chemical compound [V].[Fe].[Zr] ZGTNJINJRMRGNV-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 230000001681 protective effect Effects 0.000 claims abstract description 8
- 238000012545 processing Methods 0.000 claims abstract description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 12
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 7
- 229920001568 phenolic resin Polymers 0.000 claims description 7
- 239000005011 phenolic resin Substances 0.000 claims description 7
- 229910000640 Fe alloy Inorganic materials 0.000 claims description 6
- 229910052742 iron Inorganic materials 0.000 claims description 6
- 238000005507 spraying Methods 0.000 claims description 6
- 229910052720 vanadium Inorganic materials 0.000 claims description 6
- 239000004698 Polyethylene Substances 0.000 claims description 3
- 238000000889 atomisation Methods 0.000 claims description 3
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 3
- -1 polyethylene Polymers 0.000 claims description 3
- 229920000573 polyethylene Polymers 0.000 claims description 3
- 238000012216 screening Methods 0.000 claims description 2
- 230000006835 compression Effects 0.000 claims 1
- 238000007906 compression Methods 0.000 claims 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 17
- 239000000463 material Substances 0.000 abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 238000002156 mixing Methods 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 5
- 239000000654 additive Substances 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 4
- 238000003825 pressing Methods 0.000 description 4
- 238000012356 Product development Methods 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000009689 gas atomisation Methods 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 229910000986 non-evaporable getter Inorganic materials 0.000 description 3
- 238000007639 printing Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005247 gettering Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000003892 spreading Methods 0.000 description 2
- 230000007480 spreading Effects 0.000 description 2
- 230000003213 activating effect Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- YSZKOFNTXPLTCU-UHFFFAOYSA-N barium lithium Chemical compound [Li].[Ba] YSZKOFNTXPLTCU-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011960 computer-aided design Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000002274 desiccant Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
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Abstract
The invention provides a preparation method of a zirconium ferrovanadium getter based on 3D printing and the zirconium ferrovanadium getter, wherein the method comprises the following steps: providing spherical zirconium ferrovanadium alloy powder; establishing a three-dimensional model of the required powder product, layering and data processing the three-dimensional model to obtain a model file, and introducing the model file into powder 3DP forming equipment; paving spherical zirconium ferrovanadium alloy powder in a powder cylinder of powder 3DP forming equipment to form paving powder, combining an imported model file, adopting an array nozzle to selectively spray a binder in the paving powder for curing forming, and heating the formed body after multilayer superposition to prepare a presintered formed body with a preset shape; and (3) sintering the presintered formed body at a high temperature in a protective atmosphere to obtain the zirconium ferrovanadium getter corresponding to the structure of the three-dimensional model. The invention can obtain the shape-controllable high-strength zirconium vanadium iron getter material, realize die-free manufacture, and reduce the preparation cost while improving the product quality.
Description
Technical Field
The invention relates to the technical field of preparation of electric vacuum suction elements, in particular to a preparation method of a zirconium ferrovanadium getter based on 3D printing and the zirconium ferrovanadium getter.
Background
Non-evaporable getters (Non-Evaporable Getter, NEG) have been widely used in scientific research and industrial production in electric vacuum devices, ultra-high vacuum production, atomic energy industry, and the like due to their low equilibrium gas pressure, large gettering capacity, high gettering rate, and the like. The ternary zirconium ferrovanadium getter has the advantages of low activation temperature and working at room temperature, so that the ternary zirconium ferrovanadium getter is widely applied in multiple fields, and is an excellent getter material with low price, convenient use and strong adsorption capacity.
The prior direct powder pressing method is a main preparation method of the zirconium ferrovanadium getter material, and the method is to press alloy powder with a certain size and diameter in a die, so that the directly pressed zirconium ferrovanadium getter has poor firmness and is easy to fall off particles when being used in strong impact vibration occasions. In addition, with the development of miniaturization and precision of vacuum electronic devices, the requirements on the shape and the size of the getter are diversified, which puts higher requirements on the precision and the shape of the getter mould, greatly increases the production cost, and the traditional powder pressing method is difficult to meet the existing getter preparation requirements.
The search finds that:
the invention of China patent publication No. CN114288982A discloses a composite getter and a preparation method thereof, wherein a barium-lithium getter and a non-evaporable getter are pressed and formed in a vacuum argon-filled glove box, are placed in a metal carrier, and are wrapped by a drying agent, and are pressed and formed again to obtain the composite getter; placing the formed composite getter into a vacuum heating furnace, and heating and activating under vacuum; the cooled compound getter is rapidly packaged in vacuum in a sealing way. But this patent still has the following problems: the patent is formed by adopting the traditional pressing technology, and cannot meet the personalized customization of the size and shape of the getter.
Chinese patent application publication No. CN114929920a discloses a printable FeCrAl powder material for additive manufacturing and an additive manufactured object and its use, wherein the additive manufacturing method uses a computer aided design of a 3D shaped object to be printed, by decomposing into 2D flakes using software, which also links the generated data to hardware. But this patent still has the following problems: the patent adopts a powder bed fusion additive manufacturing method, can realize personalized customization of the size and the shape of the getter, but has high production cost due to the adoption of a high-energy heat source.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a preparation method of a zirconium ferrovanadium getter based on 3D printing and the zirconium ferrovanadium getter.
According to one aspect of the invention, there is provided a method for preparing a 3D printing-based zirconium ferrovanadium getter, the method comprising:
providing spherical zirconium ferrovanadium alloy powder;
establishing a three-dimensional model of a required powder product, layering and data processing the three-dimensional model to obtain a model file, and introducing the model file into powder 3DP forming equipment;
paving the spherical zirconium ferrovanadium alloy powder in a powder cylinder of powder 3DP forming equipment to form paving powder, selectively spraying a binder in the paving powder by adopting an array nozzle to form by curing, and heating the formed body after multilayer superposition to prepare a presintered formed body with a preset shape;
and sintering the presintered formed body at a high temperature in a protective atmosphere to obtain the zirconium ferrovanadium getter corresponding to the structure of the three-dimensional model.
Further, the providing of spherical zirconium ferrovanadium alloy powder, wherein: spherical zirconium ferrovanadium alloy powder is formed by adopting an air atomization method or a plasma rotating electrode method.
Further, the spherical zirconium ferrovanadium alloy powder is provided, wherein the spherical zirconium ferrovanadium alloy powder comprises the following components in percentage by mass: 72-77% of zirconium, 15-20% of vanadium and 3-8% of iron.
Further, the method for providing spherical zirconium ferrovanadium alloy powder further comprises the following steps: and screening the spherical zirconium ferrovanadium powder to obtain the powder with the granularity range of 20-50 mu m.
Further, paving the spherical zirconium vanadium iron alloy powder into a powder cylinder of powder 3DP forming equipment to form paving powder, wherein the spherical zirconium vanadium iron alloy powder is paved by adopting a powder paving mode of a reverse roller.
Further, the method adopts an array nozzle to selectively spray a binder in the powder paving powder for curing and forming, wherein: the binder is any one of polyethylene, butyral resin and phenolic resin; the viscosity of the binder is 7-10 mPa.S.
Further, the method adopts an array nozzle to selectively spray a binder in the powder paving powder for curing and forming, wherein: the array type spray head is a piezoelectric spray head, the diameter of the spray head is 30-50 mu m, and the spraying speed is 2-5 m/s.
Further, the multi-layered post-stack thermoformed shaped body produces a pre-sintered shaped body of a predetermined shape, wherein: heating to 180-200 ℃ and keeping for 10-30 min, wherein the relative density of the presintered formed body is 50-80%.
Further, the presintered shaped body is subjected to high temperature sintering under a protective atmosphere, wherein: the sintering temperature is 1200-1500 ℃, the sintering time is 1-3 h, and the vacuum degree is less than 3.0X10 -3 Pa。
According to another aspect of the invention, a zirconium ferrovanadium getter is provided, the zirconium ferrovanadium getter is prepared by the method, and the compressive strength of the zirconium ferrovanadium getter is 18.5-24.3 MPa.
Compared with the prior art, the invention has at least one of the following beneficial effects:
1. the invention adopts the powder 3DP method to form, and the high-strength zirconium vanadium iron getter material with controllable shape is obtained by sintering the formed body at high temperature, thereby realizing the die-free manufacture, improving the product quality and reducing the preparation cost.
2. The invention is based on the powder 3DP technology forming process, can realize the rapid manufacture of the high-strength getter material with a complex structure, simultaneously satisfies the customized manufacture of users, and can greatly shorten the product development period.
Drawings
Other features, objects and advantages of the present invention will become more apparent upon reading of the detailed description of non-limiting embodiments, given with reference to the accompanying drawings in which:
fig. 1 is a schematic flow chart of a preparation method of a 3D printing-based zirconium ferrovanadium getter in an embodiment of the invention.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the present invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications could be made by those skilled in the art without departing from the inventive concept. These are all within the scope of the present invention.
Powder 3D printing (3 DP) technology is a 3D printing method using droplet ejection, powder bonding. Under the control of a computer, the spray head selectively sprays a binder on a layer of powder material paved in advance according to the information of the current layering section to enable part of powder to be bonded to form a layer of section thin layer; after one layer is formed, the workbench is lowered by one layer thickness, powder is paved on the next layer, then the adhesive is sprayed on selected areas, and the formed thin layer is adhered to the formed part into a whole; the process is continuously circulated until the parts are completed; the process enables single piece and small lot rapid manufacturing of complex structural parts.
The powder 3DP technology is used for forming and processing the zirconium ferrovanadium material, so that the product development period can be greatly shortened, the cost is reduced, the device manufacturing with a high-strength complex structure is realized, the customized production can be carried out according to the requirements of users, the complex modeling and forming are realized, and the method has important significance for realizing wider application of the zirconium ferrovanadium getter material in the electric vacuum field.
For this reason, the embodiment of the invention provides a preparation method of a zirconium ferrovanadium getter based on 3D printing, which comprises the following steps:
s1, providing spherical zirconium ferrovanadium alloy powder, wherein the spherical powder has good fluidity and is easy to form;
s2, establishing a three-dimensional model of the required powder product in a computer, layering and data processing the three-dimensional model to obtain a model file, namely, slicing the three-dimensional model into a model file in an STL format by adopting slicing software, and guiding the model file into powder 3DP forming equipment (3 DP printing equipment);
s3, paving spherical zirconium ferrovanadium alloy powder in a powder cylinder of powder 3DP forming equipment to form paving powder, combining an imported model file, adopting an array nozzle to selectively spray a binder in the paving powder to solidify and form, and heating the formed body after multilayer superposition to prepare a presintered formed body with a preset shape;
and S4, sintering the presintered formed body at a high temperature in a protective atmosphere, wherein the protective atmosphere can prevent oxidation, and the zirconium ferrovanadium getter corresponding to the structure of the three-dimensional model is obtained.
In some embodiments, a spherical zirconium ferrovanadium alloy powder is provided, wherein: the spherical zirconium ferrovanadium alloy powder is formed by adopting an air atomization method or a plasma rotating electrode method, and has good fluidity, thereby being beneficial to powder laying in the printing process.
In some embodiments, a spherical zirconium ferrovanadium powder is provided, wherein the spherical zirconium ferrovanadium powder comprises, in mass percent: 72-77% of zirconium, 15-20% of vanadium and 3-8% of iron.
In some embodiments, there is provided a spherical zirconium ferrovanadium alloy powder, further comprising: the spherical zirconium ferrovanadium powder is screened to obtain powder with the granularity range of 20-50 mu m, so as to meet the requirement of the subsequent printing process on the particle size of the powder.
In some embodiments, the spherical zirconium vanadium iron alloy powder is laid in a powder cylinder of a powder 3DP forming device to form laid powder, wherein the spherical zirconium vanadium iron alloy powder is laid in a reverse roll powder laying manner, comprising: the spherical zirconium ferrovanadium alloy powder is conveyed to a powder bed through a feeding piston, a rotating guide roller is utilized to uniformly advance on the powder bed to scrape the powder layer, the rotating linear speed direction of the guide roller is opposite to the advancing direction, the powder spreading speed is 7-25 s/layer, and the layer thickness is 50-350 mu m, so that a good powder spreading effect is realized.
In some embodiments, the binder is selectively sprayed in the spread powder to cure the powder using an array spray head, wherein: the binder is any one of polyethylene, butyral resin and phenolic resin, preferably, the binder is mixed liquid of 65-55% of phenolic resin and 35-45% of ethanol by volume fraction, and the binder of the components has a good flowing effect; considering that too much binder can cause blockage of the spray head, too much thin powder has poor binding effect, and the viscosity of the binder is 7-10 mPa.S.
In some embodiments, the binder is selectively sprayed in the spread powder to cure the powder using an array spray head, wherein: the array type spray head is a piezoelectric spray head, the piezoelectric spray head can realize high-frequency spray, the spray efficiency is high, the diameter of the spray head is 30-50 mu m, and the spray speed is 2-5 m/s.
In step S3, the higher the heating temperature is, the higher the atomic diffusion energy, the formation and growth rate of the sintered body are, the more metallurgical bonding surfaces between the particles are, and the pores tend to be reduced and spheroidized. The strength of the sintered body is ensured by the bonding surfaces between the particles, and if all the particles in the sintered body are sintered together without any voids, the strength of the sintered part can reach the strength of a dense material, preferably a multi-layered stacked and heat-formed shaped body, to produce a pre-sintered shaped body of a predetermined shape, wherein: heating to 180-200 ℃ in an oven and keeping for 10-30 min, wherein the relative density of the presintered formed body is 50-80%.
In some embodiments, the pre-sintered shaped body is subjected to high temperature sintering under a protective atmosphere, wherein: the sintering temperature is 1200-1500 ℃, the sintering time is 1-3 h, and the vacuum degree is less than 3.0X10 -3 Pa。
According to the zirconium ferrovanadium getter, the zirconium ferrovanadium getter is prepared by the method, and the compressive strength of the zirconium ferrovanadium getter is 18.5-24.3 MPa according to different sintering temperatures.
The embodiment adopts the powder 3DP method to form, and the high-strength zirconium vanadium iron getter material with controllable shape is obtained by sintering the formed body at high temperature, so that the die-free manufacturing can be realized, the product quality is improved, and the preparation cost is reduced. In addition, the forming process based on the powder 3DP technology can realize the rapid manufacture of the high-strength getter material with a complex structure, simultaneously meet the customized manufacture of users, and can greatly shorten the product development period.
In the above embodiment, the sintering temperature is a key factor affecting the compressive strength, and the higher the sintering temperature, the greater the compressive strength; compared with the existing preparation method of the zirconium ferrovanadium getter, such as a powder pressing method and the like, the embodiment of the invention has the advantages of low cost, no mould, personalized forming and the like.
Specific examples are provided below to further illustrate the method of making the 3D printing-based zirconium vanadium iron getter of the present application.
Example 1
The embodiment provides a preparation method of a zirconium ferrovanadium getter based on 3D printing, which comprises the following steps:
(1) The total weight of the zirconium ferrovanadium alloy powder prepared by the inert gas atomization method with the grain size ranging from 20 μm to 50 μm is 500g, and the alloy comprises the following components in percentage by mass: 75% of zirconium, 19.5% of vanadium and 5.5% of iron.
(2) The molded body model is established by CAD software, the diameter of the model is 330mm, the thickness of the model is 6.35mm, the CAD model is cut into slices and then stored into an STL file containing CAD model data information, and the STL file is imported into powder 3DP molding equipment.
(3) Mixing phenolic resin and ethanol according to the mass percentage ratio of 55:45, uniformly mixing by adopting an electric stirrer, stirring for 4min at the rotating speed of 225rad/min, and obtaining the adhesive with the viscosity of 8.mPa.S.
(4) The binder was injected into a piezo-electric spray head and selectively sprayed at a rate of 4m/s into the zirconium ferrovanadium powder laid in the powder bed at a powder laying rate of 10 s/layer and a layer thickness of 100 μm.
(5) The shaped bodies were placed in an oven, heated to 185℃in the oven and incubated for 25min.
(6) Placing the dried presintered formed body into a vacuum sintering furnace for sintering at 1300 ℃ for 2h with the vacuum degree of 1.0x10 -3 Pa. The compressive strength of the tested sample was 18.5MPa.
Example 2
The embodiment provides a preparation method of a zirconium ferrovanadium getter based on 3D printing, which comprises the following steps:
(1) The total weight of the zirconium ferrovanadium alloy powder prepared by the inert gas atomization method with the grain size ranging from 20 μm to 50 μm is 500g, and the alloy comprises the following components in percentage by mass: 75% of zirconium, 19.5% of vanadium and 5.5% of iron.
(2) The molded body model is established by CAD software, the diameter of the model is 330mm, the thickness of the model is 6.35mm, the CAD model is cut into slices and then stored into an STL file containing CAD model data information, and the STL file is imported into powder 3DP molding equipment.
(3) Mixing phenolic resin and ethanol according to the mass percentage ratio of 55:45, uniformly mixing by adopting an electric stirrer, stirring for 4min at the rotating speed of 225rad/min, and obtaining the adhesive with the viscosity of 8.mPa.S.
(4) The binder was injected into a piezo-electric spray head and selectively sprayed at a rate of 4m/s into the zirconium ferrovanadium powder laid in the powder bed at a powder laying rate of 10 s/layer and a layer thickness of 100 μm.
(5) The shaped bodies were placed in an oven, heated to 185℃in the oven and incubated for 25min.
(6) Placing the dried presintered formed body into a vacuum sintering furnace for sintering at 1350 ℃ for 2h with the vacuum degree of 1.0x10 -3 Pa. The compressive strength of the tested sample was 23.8MPa.
Example 3
The embodiment provides a preparation method of a zirconium ferrovanadium getter based on 3D printing, which comprises the following steps:
(1) The total weight of the zirconium ferrovanadium alloy powder prepared by the inert gas atomization method with the grain size ranging from 20 μm to 50 μm is 500g, and the alloy comprises the following components in percentage by mass: 75% of zirconium, 19.5% of vanadium and 5.5% of iron.
(2) The molded body model is established by CAD software, the diameter of the model is 330mm, the thickness of the model is 6.35mm, the CAD model is cut into slices and then stored into an STL file containing CAD model data information, and the STL file is imported into powder 3DP molding equipment.
(3) Mixing phenolic resin and ethanol according to the mass percentage ratio of 55:45, uniformly mixing by adopting an electric stirrer, stirring for 4min at the rotating speed of 225rad/min, and obtaining the adhesive with the viscosity of 8.mPa.S.
(4) The binder was injected into a piezo-electric spray head and selectively sprayed at a rate of 4m/s into the zirconium ferrovanadium powder laid in the powder bed at a powder laying rate of 10 s/layer and a layer thickness of 100 μm.
(5) The shaped bodies were placed in an oven, heated to 185℃in the oven and incubated for 25min.
(6) Placing the dried presintered formed body into a vacuum sintering furnace for sintering at 1400 ℃ for 2h with the vacuum degree of 1.0x10 -3 Pa. The compressive strength of the tested sample was 24.3MPa.
The foregoing describes specific embodiments of the present invention. It is to be understood that the invention is not limited to the particular embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the claims without affecting the spirit of the invention. The above-described preferred features may be used in any combination without collision.
Claims (10)
1. The preparation method of the zirconium ferrovanadium getter based on 3D printing is characterized by comprising the following steps of:
providing spherical zirconium ferrovanadium alloy powder;
establishing a three-dimensional model of a required powder product, layering and data processing the three-dimensional model to obtain a model file, and introducing the model file into powder 3DP forming equipment;
paving the spherical zirconium ferrovanadium alloy powder in a powder cylinder of powder 3DP forming equipment to form paving powder, selectively spraying a binder in the paving powder by adopting an array nozzle to form by curing, and heating the formed body after multilayer superposition to prepare a presintered formed body with a preset shape;
and sintering the presintered formed body at a high temperature in a protective atmosphere to obtain the zirconium ferrovanadium getter corresponding to the structure of the three-dimensional model.
2. The method of preparing a 3D printing based zirconium ferrovanadium getter according to claim 1, wherein the providing of spherical zirconium ferrovanadium alloy powder, wherein: spherical zirconium ferrovanadium alloy powder is formed by adopting an air atomization method or a plasma rotating electrode method.
3. The method for preparing a 3D printing-based zirconium ferrovanadium getter according to claim 1, wherein the spherical zirconium ferrovanadium alloy powder is provided, wherein the spherical zirconium ferrovanadium alloy powder comprises, in mass percent: 72-77% of zirconium, 15-20% of vanadium and 3-8% of iron.
4. The method for preparing a 3D printing-based zirconium ferrovanadium getter according to claim 1, wherein the providing of spherical zirconium ferrovanadium alloy powder further comprises: and screening the spherical zirconium ferrovanadium powder to obtain the powder with the granularity range of 20-50 mu m.
5. The method for preparing the 3D printing-based zirconium vanadium iron getter according to claim 1, wherein the spherical zirconium vanadium iron alloy powder is laid in a powder cylinder of a powder 3DP forming device to form a laid powder, wherein the spherical zirconium vanadium iron alloy powder is laid in a reverse roll powder laying mode.
6. The method for preparing a 3D printing-based zirconium ferrovanadium getter according to claim 1, wherein the selective spraying of binder in the powder paving powder is performed by an array nozzle, and the method comprises the steps of: the binder is any one of polyethylene, butyral resin and phenolic resin; the viscosity of the binder is 7-10 mPa.S.
7. The method for preparing a 3D printing-based zirconium ferrovanadium getter according to claim 1, wherein the selective spraying of binder in the powder paving powder is performed by an array nozzle, and the method comprises the steps of: the array type spray head is a piezoelectric spray head, the diameter of the spray head is 30-50 mu m, and the spraying speed is 2-5 m/s.
8. The method for preparing a 3D printing-based zirconium ferrovanadium getter according to claim 1, wherein the multi-layered post-stack thermoformed shaped body is prepared as a pre-sintered shaped body of a predetermined shape, wherein: heating to 180-200 ℃ and keeping for 10-30 min, wherein the relative density of the presintered formed body is 50-80%.
9. The method for preparing a 3D printing-based zirconium ferrovanadium getter according to claim 1, wherein the pre-sintered shaped body is sintered at high temperature in a protective atmosphere, wherein: the sintering temperature is 1200-1500 ℃, the sintering time is 1-3 h, and the vacuum degree is less than 3.0X10 -3 Pa。
10. A zirconium ferrovanadium getter, characterized in that it is obtained by a method according to any one of claims 1 to 9, having a compression strength of 18.5 to 24.3MPa.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310057595.3A CN116000310A (en) | 2023-01-18 | 2023-01-18 | Preparation method of zirconium ferrovanadium getter based on 3D printing and zirconium ferrovanadium getter |
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