CN112517914A - Preparation method of high-molybdenum-content ferromolybdenum powder for powder metallurgy - Google Patents
Preparation method of high-molybdenum-content ferromolybdenum powder for powder metallurgy Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 58
- 229910001309 Ferromolybdenum Inorganic materials 0.000 title claims abstract description 31
- 238000004663 powder metallurgy Methods 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title abstract description 13
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 35
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000000498 ball milling Methods 0.000 claims abstract description 23
- 239000011733 molybdenum Substances 0.000 claims abstract description 20
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 13
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 10
- 239000010959 steel Substances 0.000 claims abstract description 10
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 9
- 239000000956 alloy Substances 0.000 claims abstract description 9
- 239000011812 mixed powder Substances 0.000 claims abstract description 8
- 238000000137 annealing Methods 0.000 claims abstract description 5
- 230000009467 reduction Effects 0.000 claims abstract description 5
- 238000000227 grinding Methods 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 2
- 238000010923 batch production Methods 0.000 abstract description 2
- 229910052802 copper Inorganic materials 0.000 abstract description 2
- 239000010949 copper Substances 0.000 abstract description 2
- 239000012535 impurity Substances 0.000 abstract description 2
- 229910052760 oxygen Inorganic materials 0.000 abstract description 2
- 239000001301 oxygen Substances 0.000 abstract description 2
- 238000009865 steel metallurgy Methods 0.000 abstract description 2
- 229910000601 superalloy Inorganic materials 0.000 abstract description 2
- 239000010935 stainless steel Substances 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 108010038629 Molybdoferredoxin Proteins 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- HBELESVMOSDEOV-UHFFFAOYSA-N [Fe].[Mo] Chemical compound [Fe].[Mo] HBELESVMOSDEOV-UHFFFAOYSA-N 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000005725 8-Hydroxyquinoline Substances 0.000 description 1
- 241001279686 Allium moly Species 0.000 description 1
- 229910001018 Cast iron Inorganic materials 0.000 description 1
- 229910000640 Fe alloy Inorganic materials 0.000 description 1
- 229910000519 Ferrosilicon Inorganic materials 0.000 description 1
- 229910000997 High-speed steel Inorganic materials 0.000 description 1
- 229910001182 Mo alloy Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 229910001315 Tool steel Inorganic materials 0.000 description 1
- FRWKYVLNGPTUTE-UHFFFAOYSA-N [Fe].[Mo].[Mo] Chemical compound [Fe].[Mo].[Mo] FRWKYVLNGPTUTE-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001739 density measurement Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052961 molybdenite Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229960003540 oxyquinoline Drugs 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- MCJGNVYPOGVAJF-UHFFFAOYSA-N quinolin-8-ol Chemical compound C1=CN=C2C(O)=CC=CC2=C1 MCJGNVYPOGVAJF-UHFFFAOYSA-N 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000007655 standard test method Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000009628 steelmaking Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- B22F1/0003—
-
- 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
- B22F1/14—Treatment of metallic powder
- B22F1/142—Thermal or thermo-mechanical treatment
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/041—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. blending, milling
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
-
- 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
- B22F2201/00—Treatment under specific atmosphere
- B22F2201/01—Reducing atmosphere
- B22F2201/013—Hydrogen
-
- 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
- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/20—Refractory metals
-
- 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
- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/35—Iron
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- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention relates to a preparation method of high-molybdenum-content ferromolybdenum powder for powder metallurgy, which comprises the following steps: using reduced iron powder or atomized iron powder and molybdenum powder as raw material, ball-milling the mixed powder, and adding the obtained product in H2And carrying out reduction and annealing treatment in the atmosphere to obtain the ferromolybdenum alloy powder. According to the preparation method of the high-molybdenum-content ferromolybdenum powder for powder metallurgy, the selectable range of raw materials can be increased, the production cost is reduced, the production efficiency is improved, the preparation method is suitable for industrial batch production, and the powder quality is obviously improved; the method for preparing the high-molybdenum-content ferromolybdenum powder has the advantages of being high in yield, low in copper and other impurities, high in molybdenum content and low in oxygen content, and can be used for preparing high-performance alloy steel and powder metallurgy materials.
Description
Technical Field
The invention belongs to the technical field of powder material preparation, and particularly relates to a preparation method of molybdenum iron powder with high molybdenum content for powder metallurgy.
Background
The ferromolybdenum powder is mainly used as an additive of molybdenum element in steel making. The addition of molybdenum in the steel can make the steel have uniform fine grain structure, and can raise hardenability of the steel, and is favorable for eliminating temper brittleness. In high speed steel, molybdenum may replace a portion of tungsten. Molybdenum is widely used in combination with other alloying elements for the production of stainless steel, heat resistant steel, acid resistant steel and tool steel, as well as alloys with specific physical properties, and the addition of molybdenum to cast iron increases its strength and wear resistance. Ferromolybdenum is an alloy of molybdenum and iron, and is an important raw alloy powder for powder metallurgy products.
The traditional ferromolybdenum powder production raw material is mainly molybdenite (MoS)2) Before smelting, the molybdenum concentrate is usually roasted by oxidation in a multi-hearth furnace to obtain roasted molybdenum ore with sulfur content less than 0.07%. The ferromolybdenum smelting is generally carried out by using ferrosilicon containing 75% silicon and a small amount of aluminum particles as reducing agent, cooling the obtained ferromolybdenum ingot, and crushing to obtain ferromolybdenum powder (particles). The ferromolybdenum powder prepared by the method generally contains 50-60% of molybdenum, the grades of the ferromolybdenum powder are mainly FeMo55, FeMo60, FeMo70 and the like, and the production of the ferromolybdenum powder with the Mo content of more than 70% still has great technical problems.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a preparation method of ferromolybdenum powder with high molybdenum content for powder metallurgy. The gist of the invention is as follows:
the invention relates to a preparation method of high-molybdenum-content ferromolybdenum powder for powder metallurgy, which comprises the following steps:
a. taking iron powder and molybdenum powder as raw materials, wherein the content of molybdenum is more than 70 wt%;
b. placing the mechanically mixed powder into a ball milling tank, wherein grinding balls are proportioned according to the mass of the added powder, and the mass of the grinding balls is not more than 20 times of the mass of the powder;
c. placing the ball milling tank on a ball mill, controlling the ball milling rotation speed within the range of 300-500r/min, and ball milling time to be 1-2 h;
d. the alloy powder is subjected to H at the temperature of 500-600 DEG C2And carrying out reduction and annealing treatment in the atmosphere.
According to an exemplary embodiment of the present invention, the purity of the reduced iron powder or the atomized iron powder in the raw material of step a is greater than 98%, the particle size is minus 100 mesh, the particle size of the molybdenum powder is less than or equal to 100 μm, and the purity is greater than or equal to 99%.
According to an exemplary embodiment of the present invention, the content of molybdenum in the moly iron powder is greater than 70 wt%.
According to an exemplary embodiment of the present invention, step a is performed as follows: the reduced iron powder or the atomized iron powder and the superfine molybdenum powder are used as raw materials and are mechanically mixed in a V-shaped mixer, a double-cone mixer or a roller mixer.
According to an exemplary embodiment of the present invention, step b is performed as follows: putting mixed powder of molybdenum powder and iron powder into a ball milling tank, and putting steel balls with the diameters of 10mm, 5mm and 3mm as grinding balls, wherein the mass ratio of the grinding balls to the powder is not more than 20: 1; and sealing the ball milling tank.
According to an exemplary embodiment of the present invention, the time of the reduction and annealing treatment of step d is 1.5-2 h.
Compared with the prior art, the method for preparing the ferromolybdenum powder with high molybdenum content has the following substantive characteristics and remarkable progress: 1) the optional range of raw materials is increased, and most of iron powder and molybdenum powder in the market can be used as raw materials; 2) the production cost is reduced, the production efficiency is improved, the technical scheme of the application has simple process flow and lower requirements on production equipment, and is suitable for industrial batch production; 3) the preparation method has the advantages that the powder quality is obviously improved, the yield of the high-molybdenum-content molybdenum iron powder prepared by the technical scheme is high, the content of copper and other impurities is low, the characteristics of high molybdenum content and low oxygen content are realized, and the preparation method can be used for preparing high-performance alloy steel and powder metallurgy materials.
Drawings
Fig. 1 is an SEM photograph of the ferromolybdenum powder prepared according to example 1 of the present invention.
Fig. 2 is an SEM photograph of the ferromolybdenum powder prepared according to example 2 of the present invention.
Detailed Description
In order to make the technical solution and advantages of the present invention more apparent, the present invention is further described in detail by the following specific examples. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Example 1:
this example prepares the ferromolybdenum powder as follows:
reduced iron powder with minus 100 meshes and molybdenum powder with minus 400 meshes are used as raw materials, and the mass ratio of Fe to Mo is 29: 71; mixing for 60min on a V-shaped mixer; placing 500g of mixed powder and grinding balls in a ball milling tank, wherein the mass of the grinding balls is 15 times that of the powder; controlling the ball milling speed in a ball mill within the range of 400r/min, wherein the ball milling time is 2 h; subjecting the alloy powder to H at 550 ℃2And treating for 90min in the atmosphere to obtain ferromolybdenum powder.
Example 2:
this example prepares the ferromolybdenum powder as follows:
using minus 100-mesh atomized iron powder and minus 400-mesh molybdenum powder as raw materials, wherein the mass ratio of Fe to Mo is 29: 71; mixing for 90min on a V-shaped mixer; placing 500g of mixed powder and grinding balls in a ball milling tank, wherein the mass of the grinding balls is 10 times that of the powder; controlling the ball milling speed in a ball mill within the range of 450r/min, wherein the ball milling time is 90 min; subjecting the alloy powder to H at 600 deg.C2And treating for 60min in the atmosphere to obtain ferromolybdenum powder.
Example 3:
this example prepares the ferromolybdenum powder as follows:
reduced iron powder with minus 100 meshes and molybdenum powder with minus 400 meshes are used as raw materials, and the mass ratio of Fe to Mo is 20: 80; mixing for 60min on a V-shaped mixer; placing 500g of mixed powder and grinding balls in a ball milling tank, wherein the mass of the grinding balls is 20 times that of the powder; controlling the ball milling speed in a ball mill within the range of 400r/min, wherein the ball milling time is 2 h; the alloy powder is processed at 550 DEG CIn H2And treating for 90min in the atmosphere to obtain ferromolybdenum powder.
Example 4:
the powders obtained in examples 1 to 3 were used for the preparation of samples which were observed using a scanning electron microscope model zeiss EVO18 under vacuum at room temperature of 25 ℃ and at an ambient humidity of 30%. As can be seen from fig. 1 and 2, the iron particles substantially maintain the particle size and morphology of the raw material iron powder, while the molybdenum particles after ball milling are bonded to the surface of the iron particles to form a strong metallurgical bond while maintaining a small particle size of the raw material molybdenum powder.
Example 5:
the ferromolybdenum material was prepared from the powders prepared in examples 1 to 3, and was pressed into a green compact under a pressing pressure of 500MPa, and was sintered to obtain a sintered body material, wherein the sintering temperature was 1400 ℃, the atmosphere was an ammonia decomposition atmosphere, and the sintering time was 90 min. The material numbers are M1, M2, and M3, respectively. Measuring the density of the material according to GB/T3850-2015 Density measurement method for dense sintered metal material and hard alloy; the mechanical properties of the material are measured according to JB/T6646-2007 physical property detection Specification for sintered metal products. And (3) measuring the molybdenum content according to GB/T5059.1-2014 'weight method for measuring molybdenum-iron-molybdenum content, ammonium metavanadate titration method and 8-hydroxyquinoline weight method'. The results are shown in Table 1.
Table 1 performance parameters of the samples after powder sampling prepared in examples 1 to 3
Example 6:
the ferromolybdenum powders prepared in examples 1 to 3 were used to prepare 316L stainless steel material, and 316L stainless steel material commonly used on the market as a comparative example, in which the molybdenum content was 2.5 wt%. The mechanical properties of the material were measured according to the ASTM A370-2017 Standard test method and definition of mechanical Properties test for Steel products, and the test results are shown in Table 2.
TABLE 2 Performance parameters of the powders prepared in examples 1 to 3 as starting materials for 316L stainless steel preparation
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (6)
1. A method for preparing a high molybdenum content ferromolybdenum powder for powder metallurgy, which is characterized by comprising the following steps:
a. taking reduced iron powder or atomized iron powder and superfine molybdenum powder as raw materials, and mechanically mixing according to the proportion that the content of molybdenum is more than 70 wt%;
b. placing the mixed powder and grinding balls in a ball milling tank, wherein the grinding balls are proportioned according to the mass of the added powder, and the mass of the grinding balls is not more than 20 times of the mass of the powder;
c. placing the ball milling tank on a ball mill, controlling the ball milling rotation speed within the range of 300-500r/min, and ball milling time to be 1-2 h;
d. the alloy powder is subjected to H at the temperature of 700-800 DEG C2And carrying out reduction and annealing treatment in the atmosphere to obtain the ferromolybdenum powder.
2. The method according to claim 1, wherein the purity of the reduced iron powder or atomized iron powder in the raw material of step a is greater than or equal to 99%, the particle size is minus 100 mesh, the particle size of molybdenum powder is less than or equal to 100 μm, and the purity is greater than or equal to 99%.
3. A method according to claim 1 or 2, characterized in that the molybdenum content of the said ferro-molybdenum powder is more than 70 wt%, up to 90 wt%.
4. The method of claim 1 or 2, wherein step a is performed as follows: the reduced iron powder or the atomized iron powder and the superfine molybdenum powder are used as raw materials and are mechanically mixed in a V-shaped mixer, a double-cone mixer or a roller mixer.
5. The method of claim 1, wherein step b is performed as follows: putting mixed powder of molybdenum powder and iron powder into a ball milling tank, and putting steel balls with the diameters of 10mm, 5mm and 3mm as grinding balls, wherein the mass ratio of the grinding balls to the powder is not more than 20: 1; and sealing the ball milling tank.
6. The method according to claim 1, wherein the time for the reduction and annealing treatment in step d is 1.5-2 h.
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CN108796255A (en) * | 2018-06-14 | 2018-11-13 | 马林生 | A kind of high-purity ferro-molybdenum preparation process |
CN110976888A (en) * | 2019-12-24 | 2020-04-10 | 郑州大学 | Complete solid solution molybdenum-niobium alloy powder and preparation method and application thereof |
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