CN110614361B - Method for preparing block getter by microwave sintering - Google Patents
Method for preparing block getter by microwave sintering Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 34
- 238000009768 microwave sintering Methods 0.000 title claims abstract description 27
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 50
- 239000000956 alloy Substances 0.000 claims abstract description 50
- 238000005245 sintering Methods 0.000 claims abstract description 31
- 239000000843 powder Substances 0.000 claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000012298 atmosphere Substances 0.000 claims abstract description 8
- 238000000498 ball milling Methods 0.000 claims abstract description 8
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 8
- 230000001681 protective effect Effects 0.000 claims abstract description 8
- 238000010298 pulverizing process Methods 0.000 claims abstract description 6
- 238000003723 Smelting Methods 0.000 claims abstract description 5
- 229910052786 argon Inorganic materials 0.000 claims abstract description 4
- 229910000691 Re alloy Inorganic materials 0.000 claims description 27
- 239000000463 material Substances 0.000 claims description 22
- 229910001215 Te alloy Inorganic materials 0.000 claims description 21
- 230000007704 transition Effects 0.000 claims description 21
- 229910052721 tungsten Inorganic materials 0.000 claims description 21
- 229910052741 iridium Inorganic materials 0.000 claims description 18
- 229910052720 vanadium Inorganic materials 0.000 claims description 15
- 230000008569 process Effects 0.000 claims description 8
- 238000003825 pressing Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 238000000265 homogenisation Methods 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 238000002844 melting Methods 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- 229910000838 Al alloy Inorganic materials 0.000 claims description 3
- 229910001339 C alloy Inorganic materials 0.000 claims description 3
- 229910000531 Co alloy Inorganic materials 0.000 claims description 3
- 229910020706 Co—Re Inorganic materials 0.000 claims description 3
- 229910000640 Fe alloy Inorganic materials 0.000 claims description 3
- 229910011214 Ti—Mo Inorganic materials 0.000 claims description 3
- 229910007727 Zr V Inorganic materials 0.000 claims description 3
- 230000006698 induction Effects 0.000 claims description 3
- 229910052702 rhenium Inorganic materials 0.000 claims description 3
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims 3
- 239000000203 mixture Substances 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 238000004663 powder metallurgy Methods 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 230000008646 thermal stress Effects 0.000 description 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910052765 Lutetium Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000009770 conventional sintering Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000005324 grain boundary diffusion Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910001172 neodymium magnet Inorganic materials 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 238000005381 potential energy Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
Classifications
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
-
- 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
- B22F3/02—Compacting only
-
- 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
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C16/00—Alloys based on zirconium
-
- 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
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1054—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by microwave
-
- 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
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
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- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a method for preparing a block getter by microwave sintering, which comprises the following steps: preparing a getter alloy according to a certain formula, preparing an alloy ingot by a smelting method, carrying out heat treatment on the alloy ingot, and then crushing and ball-milling the alloy ingot in a protective atmosphere to obtain getter alloy powder of 300-80 meshes; putting the getter alloy powder into a die to be pressed to form a pressed compact; under a vacuum degree of 3 to 5 × 10 ‑3 Introducing high-purity argon in a protective atmosphere in a vacuum environment of Pa, and sintering a pressed blank by using a microwave oven; after microwave sintering is finished, the mixture is cooled to room temperature under the protection of nitrogen atmosphere and taken out of the furnace, and the block getter with strong anti-pulverization capability can be obtained. The invention has the advantages of low sintering temperature, high temperature rise speed, integral heating, uniform heating, fine and uniform alloy structure and the like, and the used time can be greatly shortened, thereby improving the preparation efficiency of the bulk getter.
Description
Technical Field
The invention relates to the field of powder metallurgy, in particular to a method for preparing a block getter by microwave sintering.
Background
Microwave sintering is a method for realizing densification by utilizing the special wave band of microwave to couple with the basic fine structure of a material to generate heat, and the dielectric loss of the material heats the whole material to a sintering temperature. The powder metallurgy material is applied to various powder metallurgy products, such as sintered NdFeB permanent magnet materials, iron, nickel, diamond, aluminum, copper, aluminum, tin and other metal powder, is subjected to a heating test, and is successfully manufactured into small gears and other annular and tubular mechanical parts. The microwave sintering device has the characteristics of instantaneity and no pollution, and heat conduction is not needed in the microwave heating process, so that the microwave sintering device has no thermal inertia, namely has instantaneity, which means that a heat source can be cut off instantaneously and heat in time, and the energy is saved (70% -90% of the energy is saved compared with the conventional sintering device) and is easy to control. Meanwhile, the microwave sintering heat source is pure, the sintered material is not polluted, and the sintering under vacuum and various atmospheres and pressures can be conveniently realized. For getter materials, because of their high surface activity, they require a non-polluting heat source and a clean sintering environment, whereas vacuum microwave sintering has these characteristics, such as the purity of the heat source, the absence of contamination of the sintered getter material, etc.
Disclosure of Invention
The invention aims to provide a method for preparing a bulk getter by microwave sintering, which has uniform heating and high efficiency.
The purpose of the invention is realized as follows: the method for preparing the bulk getter by microwave sintering comprises the following steps:
1) Preparing a getter alloy according to a certain formula, preparing an alloy ingot by a smelting method, carrying out heat treatment on the alloy ingot, and then crushing and ball-milling the alloy ingot in a protective atmosphere to obtain getter alloy powder of 300-80 meshes;
2) And filling the getter alloy powder into a die, and pressing to form a compact.
3) Introducing high-purity argon in protective atmosphere in a vacuum environment with the vacuum degree of 3-5 multiplied by 10 < -3 > Pa, and sintering the pressed compact by a microwave oven.
4) After microwave sintering is finished, the mixture is cooled to room temperature under the protection of nitrogen atmosphere and taken out of the furnace, and the block getter with strong anti-pulverization capability can be obtained.
Compared with the prior art, the invention has the advantages that: microwave heating is to convert microwave energy absorbed by a material into kinetic energy and potential energy of molecules in the material, heat is generated from the inside of the material instead of other heating bodies, and the thermodynamic gradient, heat conduction and other traditional heating generated by the internal body heating are different. In the heating process of the body, electromagnetic energy permeates into the inside of the getter material pressed compact in a wave form to cause dielectric loss and generate heat, so that the material is integrally and uniformly heated at the same time, the temperature gradient in the material is small or zero, the internal thermal stress of the material can be reduced to the minimum degree, the heat cannot be generated (500 to 600 ℃/min) even under the condition of very fast temperature rise, the defect that the getter material pressed compact is cracked due to the thermal stress caused by the fast temperature rise in the traditional sintering process is overcome, and the production efficiency is improved undoubtedly. Meanwhile, under the action of microwave electromagnetic energy, the kinetic energy of molecules or ions in the getter material is increased, and the sintering activation energy is reduced, so that the densification speed of the material is accelerated, the sintering time is shortened, and meanwhile, due to the improvement of the diffusion coefficient, the grain boundary diffusion of the material is enhanced, the density of the material is improved, so that the low-temperature rapid sintering of the material is realized, and the energy is saved.
In a preferred embodiment of the present invention, the getter alloy includes the following types:
a) Zr-Al alloy, zr-Al-RE alloy, zr-Al-TE-RE alloy, wherein TE comprises transition group elements of Ti, fe, co, ni, mn, pd, ru, pt, V, cr, nb, mo, tc, rh, hf, ta, W, re, os, ir;
b) Zr-C alloy, zr-C-RE alloy, zr-C-TE-RE alloy, wherein TE comprises transition group elements of Ti, fe, co, ni, mn, pd, ru, pt, V, cr, nb, mo, tc, rh, hf, ta, W, re, os and Ir;
c) Zr-V-Fe alloy, zr-V-Fe-RE alloy, zr-V-Fe-TE alloy, zr-V-Fe-RE-TE alloy, wherein TE comprises transition elements of Ti, co, ni, mn, pd, ru, pt, cr, nb, mo, tc, rh, hf, ta, W, re, os and Ir;
d) Zr-Co alloy, zr-Co-RE alloy, zr-Co-TE alloy, zr-Co-RE-TE alloy, wherein TE comprises transition group elements of Ti, fe, ni, mn, pd, ru, pt, V, cr, nb, mo, tc, rh, hf, ta, W, re, os and Ir;
e) Ti-Mo alloy, ti-Mo-RE alloy, ti-Mo-TE alloy, ti-Mo-RE-TE alloy, wherein TE comprises transition group elements of Zr, fe, co, ni, mn, pd, ru, pt, V, cr, nb, tc, rh, hf, ta, W, re, os and Ir;
f) Ti-Zr-V alloy, ti-Zr-V-RE alloy, ti-Zr-V-TE-RE alloy, wherein TE comprises transition group elements of Fe, co, ni, mn, pd, ru, pt, cr, nb, mo, tc, rh, hf, ta, W, re, os and Ir;
g) Zr-Co-Re (rhenium) alloy, zr-Co-Re-RE-TE alloy, wherein TE comprises transition elements of Ti, fe, co, ni, mn, pd, ru, pt, V, cr, nb, mo, tc, rh, hf, ta, W, os and Ir.
In a further preferred embodiment of the present invention, RE is a rare earth element Y, sc, la, ce, pr, nd, pm, sm, eu, gd, tb, dy, ho, er, tm, yb, lu.
In a further preferred embodiment of the present invention, the getter alloy powder is charged into a mold and pressed to obtain a molding pressure of 1 to 8t/cm2, while maintaining the pressure for 1 to 30 seconds.
In a more preferred embodiment of the present invention, the green compact has a relative density of 30 to 60%.
In a further preferred embodiment of the present invention, the microwave power used for sintering in the microwave oven is 2Kw, and the microwave frequency is 2.45 GHz.
In a further preferable embodiment of the invention, the sintering process of the microwave oven sintering is performed by keeping the temperature at 850 to 1000 ℃ for 50 to 150 seconds.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The method for preparing the bulk getter by microwave sintering comprises the following steps:
1) Preparing a getter alloy according to a certain formula, preparing an alloy ingot by a smelting method, carrying out heat treatment on the alloy ingot, and then crushing and ball-milling the alloy ingot in a protective atmosphere to obtain getter alloy powder of 300-80 meshes;
2) And putting the getter alloy powder into a die, and pressing to form a green compact.
3) Introducing high-purity argon gas in protective atmosphere at the same time under the vacuum condition with the vacuum degree of 3-5 multiplied by 10 < -3 > Pa, and sintering the pressed compact by adopting a microwave oven.
4) After the microwave sintering is finished, the mixture is cooled to room temperature under the protection of nitrogen atmosphere and taken out of the furnace, and the block getter with strong pulverization resistance can be obtained.
The above getter alloys include the following:
a) Zr-Al alloy, zr-Al-RE alloy, zr-Al-TE-RE alloy, wherein TE comprises transition group elements of Ti, fe, co, ni, mn, pd, ru, pt, V, cr, nb, mo, tc, rh, hf, ta, W, re, os and Ir;
b) Zr-C alloy, zr-C-RE alloy, zr-C-TE-RE alloy, wherein TE comprises transition group elements of Ti, fe, co, ni, mn, pd, ru, pt, V, cr, nb, mo, tc, rh, hf, ta, W, re, os and Ir;
c) Zr-V-Fe alloy, zr-V-Fe-RE alloy, zr-V-Fe-TE alloy, zr-V-Fe-RE-TE alloy, wherein TE comprises transition elements of Ti, co, ni, mn, pd, ru, pt, cr, nb, mo, tc, rh, hf, ta, W, re, os and Ir;
d) Zr-Co alloy, zr-Co-RE alloy, zr-Co-TE alloy, zr-Co-RE-TE alloy, wherein TE comprises transition group elements of Ti, fe, ni, mn, pd, ru, pt, V, cr, nb, mo, tc, rh, hf, ta, W, re, os and Ir;
e) Ti-Mo alloy, ti-Mo-RE alloy, ti-Mo-TE alloy, ti-Mo-RE-TE alloy, wherein TE comprises transition group elements of Zr, fe, co, ni, mn, pd, ru, pt, V, cr, nb, tc, rh, hf, ta, W, re, os and Ir;
f) Ti-Zr-V alloy, ti-Zr-V-RE alloy, ti-Zr-V-TE-RE alloy, wherein TE comprises transition group elements Fe, co, ni, mn, pd, ru, pt, cr, nb, mo, tc, rh, hf, ta, W, re, os, ir;
g) Zr-Co-Re (rhenium) alloy, zr-Co-Re-RE-TE alloy, wherein TE comprises transition elements of Ti, fe, co, ni, mn, pd, ru, pt, V, cr, nb, mo, tc, rh, hf, ta, W, os and Ir.
The RE is rare earth elements Y, sc, la, ce, pr, nd, pm, sm, eu, gd, tb, dy, ho, er, tm, yb and Lu.
And filling the getter alloy powder into a die, pressing to obtain the forming pressure of 1 to 8t/cm < 2 >, and keeping the pressure for 1 to 30 s.
The relative density of the green compact is 30 to 60 percent.
The microwave power used for sintering in the microwave oven is 2Kw, and the microwave frequency is 2.45 GHz.
The sintering process of the microwave oven sintering is to keep the temperature at 850 to 1000 ℃ for 50 to 150 s.
Example 1
Based on a stoichiometric formula of Zr51.44V40.46Fe8.10 (weight ratio), an alloy ingot is prepared by a vacuum induction melting method, the alloy ingot is subjected to homogenization heat treatment at 1050 ℃ for 5 h, then is rapidly cooled to room temperature, the cooled ingot is crushed and ball-milled to powder of 325 meshes to 200 meshes, the powder is filled into a rigid mold, and the powder is subjected to 1.5 t/cm 2 Pressing under the pressure of (1) to obtain a green compact, sintering the green compact in a vacuum microwave oven at a vacuum degreeIs 4 x 10 -3 Pa, microwave power 1.6 Kw, microwave frequency 2.45 GHz. The sintering process comprises the following steps: at 900 ℃ for 70s. After microwave sintering is finished, the mixture is cooled to room temperature under the protection of nitrogen atmosphere and taken out of the furnace, and the bulk getter with strong anti-pulverization capability can be obtained. After the getter is activated for 15 min at 480 ℃, the total hydrogen absorption amount is as follows: 230 cm of 3 ·Pa/g。
Example 2
Based on a Ti92Mo8 (weight ratio) stoichiometric formula, preparing an alloy ingot by a vacuum induction melting method, carrying out homogenization heat treatment on the alloy ingot at 1150 ℃ for 6 h, then carrying out quick cooling to room temperature, crushing and ball-milling the cooled ingot to 325-200 mesh powder, putting the powder into a rigid mold, and carrying out ball milling at 5 t/cm 2 Pressing under a pressure of (3) to obtain a green compact, sintering the green compact in a vacuum microwave oven at a vacuum degree of 3X 10 -3 Pa, microwave power of 1.5Kw, and microwave frequency of 2.45 GHz. The sintering process comprises the following steps: at 950 ℃ for 50s. After microwave sintering is finished, the mixture is cooled to room temperature under the protection of nitrogen atmosphere and taken out of the furnace, and the bulk getter with strong anti-pulverization capability can be obtained. After the getter is activated for 20 min at 300 ℃, the total hydrogen absorption amount is as follows: 163 cm 3 ·Pa/g。
The present invention is not limited to the above-mentioned embodiments, and based on the technical solutions disclosed in the present invention, those skilled in the art can make some substitutions and modifications to some technical features without creative efforts according to the disclosed technical contents, and these substitutions and modifications are all within the protection scope of the present invention.
Claims (6)
1. The method for preparing the bulk getter by microwave sintering is characterized in that the method for preparing the bulk getter material by the microwave sintering method comprises the following steps:
1) Preparing a getter alloy according to a certain formula, preparing an alloy ingot by a smelting method, carrying out heat treatment on the alloy ingot, and then crushing and ball-milling the alloy ingot in a protective atmosphere to obtain getter alloy powder of 80-300 meshes;
2) Putting the getter alloy powder into a die to be pressed to form a pressed blank;
3) Under the vacuum degree of 3-5 × 10 -3 Introducing high-purity argon in a protective atmosphere in a vacuum environment of Pa, and sintering a pressed blank by using a microwave oven;
4) After microwave sintering is finished, protecting and cooling to room temperature in a nitrogen atmosphere, and discharging to obtain a block getter with strong anti-pulverization capability;
the sintering process of the microwave oven sintering is that the temperature is kept for 50 to 150 seconds at 850 to 1000 ℃.
2. The method for preparing the bulk getter by microwave sintering according to claim 1, wherein: the getter alloys are of the following classes:
a) Zr-Al alloy, zr-Al-RE alloy, zr-Al-TE-RE alloy, wherein TE comprises transition group elements of Ti, fe, co, ni, mn, pd, ru, pt, V, cr, nb, mo, rh, hf, ta, W, re, os, ir;
b) Zr-C alloy, zr-C-RE alloy, zr-C-TE-RE alloy, wherein TE comprises transition group elements of Ti, fe, co, ni, mn, pd, ru, pt, V, cr, nb, mo, rh, hf, ta, W, re, os and Ir;
c) Zr-V-Fe alloy, zr-V-Fe-RE alloy, zr-V-Fe-TE alloy, zr-V-Fe-RE-TE alloy, wherein TE comprises transition elements of Ti, co, ni, mn, pd, ru, pt, cr, nb, mo, rh, hf, ta, W, re, os and Ir;
d) Zr-Co alloy, zr-Co-RE alloy, zr-Co-TE alloy, zr-Co-RE-TE alloy, wherein TE comprises transition group elements of Ti, fe, ni, mn, pd, ru, pt, V, cr, nb, mo, rh, hf, ta, W, re, os and Ir;
e) Ti-Mo alloy, ti-Mo-RE alloy, ti-Mo-TE alloy, ti-Mo-RE-TE alloy, wherein TE comprises transition group elements of Zr, fe, co, ni, mn, pd, ru, pt, V, cr, nb, rh, hf, ta, W, re, os and Ir;
f) Ti-Zr-V alloy, ti-Zr-V-RE alloy, ti-Zr-V-TE-RE alloy, wherein TE comprises transition group elements of Fe, co, ni, mn, pd, ru, pt, cr, nb, mo, rh, hf, ta, W, re, os and Ir;
g) Zr-Co-Re (rhenium) alloy, zr-Co-Re-RE-TE alloy, wherein TE comprises transition elements of Ti, fe, co, ni, mn, pd, ru, pt, V, cr, nb, mo, rh, hf, ta, W, os and Ir.
3. The method for preparing the bulk getter by microwave sintering according to claim 1, wherein: the air suction alloy powder is filled into a die and pressed to obtain the forming pressure of 1 to 8t/cm 2 And keeping the pressure for 1 to 30 seconds.
4. The method for preparing the bulk getter by microwave sintering according to claim 1, wherein: the relative density of the green compact is 30 to 60 percent.
5. The method for preparing the bulk getter by microwave sintering according to claim 1, wherein: the microwave power adopted by the microwave oven for sintering is 2Kw, and the microwave frequency is 2.45 GHz.
6. The method for preparing the bulk getter by microwave sintering according to claim 1, wherein: the getter alloy is Zr 51.44 V 40.46 Fe 8.10 The method comprises the following steps:
preparing an alloy ingot by a vacuum induction melting method, carrying out homogenization heat treatment on the alloy ingot at 1050 ℃ for 5 hours, then quickly cooling to room temperature, crushing and ball-milling the cooled ingot to 200-325 meshes of powder, filling the powder into a rigid mold, and carrying out vacuum melting at 1.5 t/cm 2 Pressing under the pressure of (2) to obtain a green compact, sintering the green compact in a vacuum microwave oven at a vacuum degree of 4X 10 -3 Pa, microwave power of 1.6 Kw and microwave frequency of 2.45 GHz; the sintering process comprises the following steps: sintering at 900 ℃ for 70s; after the microwave sintering is finished, cooling to room temperature under the protection of nitrogen atmosphere, and discharging; or
The getter alloy is Ti 92 Mo 8 The method comprises the following steps:
by vacuum inductionPreparing an alloy ingot by a smelting method, carrying out homogenization heat treatment on the alloy ingot at 1150 ℃ for 6 hours, then quickly cooling to room temperature, crushing the cooled ingot, carrying out ball milling to obtain 200-325 mesh powder, putting the powder into a rigid mold, and carrying out homogenization heat treatment at 5 t/cm 2 Pressing under the pressure of (2) to obtain a green compact, sintering the green compact in a vacuum microwave oven at a vacuum degree of 3X 10 -3 Pa, microwave power of 1.5Kw and microwave frequency of 2.45 GHz; the sintering process comprises the following steps: sintering at 950 ℃ for 50s; and after the microwave sintering is finished, cooling to room temperature under the protection of nitrogen atmosphere, and discharging.
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Denomination of invention: A Method for Preparing Block Absorbent by Microwave Sintering Granted publication date: 20221014 Pledgee: The Bank of Shanghai branch Caohejing Limited by Share Ltd. Pledgor: Shanghai Jingwei Material Technology Co.,Ltd. Registration number: Y2024980012755 |
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