CN112355312A - Activation sintering preparation method of ultrafine-grained pure molybdenum metal material - Google Patents
Activation sintering preparation method of ultrafine-grained pure molybdenum metal material Download PDFInfo
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- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 238000005245 sintering Methods 0.000 title claims abstract description 64
- 239000007769 metal material Substances 0.000 title claims abstract description 19
- 230000004913 activation Effects 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000000498 ball milling Methods 0.000 claims abstract description 50
- 238000000034 method Methods 0.000 claims abstract description 22
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000001257 hydrogen Substances 0.000 claims abstract description 20
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 20
- 238000003825 pressing Methods 0.000 claims abstract description 19
- 239000012298 atmosphere Substances 0.000 claims abstract description 12
- 230000008569 process Effects 0.000 claims abstract description 10
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 9
- 239000011733 molybdenum Substances 0.000 claims abstract description 9
- 239000002245 particle Substances 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 6
- 238000000713 high-energy ball milling Methods 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims description 11
- 238000004321 preservation Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000012300 argon atmosphere Substances 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 5
- 238000009694 cold isostatic pressing Methods 0.000 claims description 3
- 238000009837 dry grinding Methods 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 238000009766 low-temperature sintering Methods 0.000 abstract description 3
- 238000005054 agglomeration Methods 0.000 abstract description 2
- 230000002776 aggregation Effects 0.000 abstract description 2
- 238000000465 moulding Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 229910052786 argon Inorganic materials 0.000 description 3
- 230000003247 decreasing effect Effects 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 229910001182 Mo alloy Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- -1 molybdenum metals Chemical class 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
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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
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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
- 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
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
-
- 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
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Abstract
本发明公开了一种超细晶纯钼金属材料的活化烧结制备方法，包括以下步骤：1)取适量钼粉，按一定球料比放入球磨罐，进行高能球磨活化，得到球磨后钼粉；2)将步骤1)中球磨后的粉末按照需求进行压制，得到坯料；3)将步骤2)中坯料放入烧结炉中；在氢气氛围下按照设定的参数进行烧结成型，得到纯钼金属。本发明采用高能球磨法活化钼粉，能够有效减少钼粉的团聚，使钼粉颗粒粒度均匀减小，并降低烧结活化能；球磨工艺也相对简单，能够规模化应用。本发明采用的是氢气氛烧结，设备要求不高，同时烧结温度为1400℃，与传统1900℃左右相比，能够有效节约能源；更为重要的是，低温烧结能实现钼烧结坯的超细晶粒，从而获得较高的力学性能。
The invention discloses a preparation method for activation and sintering of ultrafine-grained pure molybdenum metal material. 2) Pressing the powder after ball milling in step 1) as required to obtain a billet; 3) putting the billet in step 2) into a sintering furnace; sintering and molding according to the set parameters under a hydrogen atmosphere to obtain pure molybdenum Metal. The present invention adopts the high-energy ball milling method to activate the molybdenum powder, which can effectively reduce the agglomeration of the molybdenum powder, uniformly reduce the particle size of the molybdenum powder, and reduce the activation energy of sintering; the ball milling process is relatively simple and can be applied on a large scale. The invention adopts hydrogen atmosphere sintering, the equipment requirements are not high, and the sintering temperature is 1400 ° C, which can effectively save energy compared with the traditional 1900 ° C; more importantly, the low temperature sintering can realize the ultra-fine molybdenum sintered blank. grains to obtain higher mechanical properties.
Description
Technical Field
The invention belongs to the technical field of molybdenum metal materials, and particularly relates to an activation sintering preparation method of an ultrafine-grained pure molybdenum metal material.
Background
Molybdenum metal is a commonly used high-temperature material, has the advantages of high melting point, high strength, high creep deformation and corrosion resistance, low thermal expansion coefficient, excellent thermal conductivity and electronic conductivity and the like, and has very wide application in the fields of aerospace, electronic and electric products, machining, military, metallurgy and the like. With the rapid development of economy and industry, the application of molybdenum metal materials in aspects of high and new technology weaponry, advanced science and technology, nuclear energy development and the like is further expanded, and higher requirements are put forward on the mechanical properties of the molybdenum metal materials.
The sintering temperature of the molybdenum metal material is usually about 1900 ℃, and because the molybdenum metal powder is very sensitive to the sintering temperature and can grow rapidly when meeting high temperature in the sintering process, the grain size of the molybdenum metal material prepared by the traditional method is larger (more than 50 mu m), so that the molybdenum metal material has larger brittleness, and the improvement of yield strength and tensile strength is limited; at the same time, higher sintering temperatures also consume more energy.
Disclosure of Invention
The invention aims to provide an activation sintering preparation method of an ultrafine-grained pure molybdenum metal material, which can effectively reduce the sintering temperature of the molybdenum metal material and achieve higher density so as to obtain an ultrafine-grained structure.
The activation sintering preparation method of the ultrafine-grained pure molybdenum metal material comprises the following steps:
1) preparing ball-milled molybdenum powder: taking a proper amount of molybdenum powder, putting the molybdenum powder into a ball milling tank according to a certain ball material ratio, and performing high-energy ball milling activation to obtain ball-milled molybdenum powder;
2) preparing a blank: pressing the powder subjected to ball milling in the step 1) as required to obtain a blank;
3) preparing a pure molybdenum sintered product: putting the blank in the step 2) into a sintering furnace; sintering and forming are carried out under the hydrogen atmosphere according to set parameters to obtain the pure molybdenum metal.
In the step 1), the molybdenum powder is industrial molybdenum powder, and the Fischer-Tropsch type particle size is 2-6 mu m; the ball milling process is dry milling under protective gas: the revolution speed of ball milling is 300-600 r/min; the ball-material ratio is (10-30) to 1; the total ball milling time is 12-96 h; introducing inert gas for protection during ball milling; after the ball milling is finished, the powder in the ball milling tank can be taken out after the ball milling tank is cooled to the room temperature.
Preferably, the inert atmosphere is argon atmosphere, the revolution speed of ball milling is 350r/min, the ball-material ratio is 10:1, and the total ball milling time is 24 h.
In the step 2), the pressing pressure is 200-400 MPa, the pressing mode is one-way pressing or cold isostatic pressing, and the pressure maintaining time is 60-120 s.
Preferably, the pressing pressure is 300MPa, the pressing mode is one-way pressing or cold isostatic pressing, and the dwell time is 120 s.
In the step 3), sintering treatment is carried out in the whole hydrogen atmosphere, wherein the sintering temperature is 1300-1600 ℃; when the temperature is lower than 1000 ℃, the heating rate is 8-12 ℃/min, the sintering temperature is 1000 ℃, and the heating rate is 4-6 ℃/min; the heat preservation time is 2-6 h, and the hydrogen flow is 0.8-2.0L/min.
Preferably, the sintering temperature is 1400 ℃, the heating rate is 10 ℃/min and 1000-1400 ℃ when the temperature is lower than 1000 ℃ in the sintering process, and the heating rate is 5 ℃/min; the heat preservation time is 2h, and the hydrogen flow is 0.8L/min.
The molybdenum metal sintered compact is prepared according to the method.
The principle of the invention is as follows: according to the invention, molybdenum powder is prepared by high-energy ball milling, molybdenum powder particles are refined, and sintering activation energy is reduced, so that higher density can be achieved at a lower sintering temperature during sintering, and finer granularity is ensured.
The invention has the beneficial effects that:
1) according to the invention, the molybdenum powder is activated by adopting a high-energy ball milling method, so that the agglomeration of the molybdenum powder can be effectively reduced, the particle size of the molybdenum powder is uniformly reduced, and the sintering activation energy is reduced; the ball milling process is relatively simple and can be applied in large scale.
2) The invention adopts hydrogen atmosphere sintering, the equipment requirement is not high, and meanwhile, the sintering temperature is 1400 ℃, compared with the traditional sintering temperature of about 1900 ℃, the energy can be effectively saved; more importantly, the ultra-fine crystal grains of the molybdenum sintering blank can be realized through low-temperature sintering, so that higher mechanical properties can be obtained.
3) The density of the molybdenum blank obtained by sintering at 1400 ℃ by adopting the method provided by the invention is more than 95%, the grain size is relatively uniform and is about 5-6 mu m, and the hardness is greatly improved to 438.3HV which is far higher than that of a sintered blank (100HV) of non-ball-milled industrial molybdenum powder.
Drawings
FIG. 1 is a scanning electron micrograph of the original commercial molybdenum powder of example 1;
FIG. 2 is a scanning electron microscope image of the molybdenum powder prepared in example 1 after ball milling at 350 r/min;
FIG. 3 is a scanning electron micrograph of a sintered molybdenum alloy billet prepared in example 1;
FIG. 4 is a scanning electron micrograph of a sintered molybdenum alloy billet prepared at 1800 ℃ according to comparative example 3.
Detailed Description
Example 1
Weighing 100g of industrial molybdenum powder, wherein the appearance of the industrial molybdenum powder is shown in figure 1, the average particle size of the industrial molybdenum powder is 3 mu m, putting the industrial molybdenum powder into a ball milling tank, the ball-material ratio is 10:1, and the ball milling revolution speed is 350 r/min; the total time of ball milling is 24 hours, and the machine is stopped for 8-10 min every 1 hour of ball milling; argon is introduced as protective gas during ball milling, the appearance after ball milling is shown in figure 2, and the comparison between figure 1 and figure 2 shows that the molybdenum powder after ball milling has better dispersibility and the particle size is obviously reduced.
And taking the molybdenum powder subjected to ball milling out in a glove box under the argon atmosphere, putting the molybdenum powder into a prepared die, and performing unidirectional pressing at the pressing pressure of 300MPa for 120s to obtain a blank.
Putting the pressed blank into a hydrogen sintering furnace, ensuring the hydrogen sintering atmosphere, checking the purity and igniting, and increasing and decreasing the temperature speed: when the temperature is reduced to 700 ℃, the temperature can be naturally cooled along with the furnace; the sintering temperature is 1400 ℃, the heat preservation time is 2h, the hydrogen flow is 0.8L/min, and when the temperature is reduced to be below 80 ℃, a sample is taken out. The obtained molybdenum metal sintered blank has a density of 95% and a hardness of 438.3 HV.
Comparative example 1
The sintering raw material is unprocessed industrial molybdenum powder, the process parameters in all other preparation processes are basically consistent with those in the embodiment 1, and the sintering temperature is 1400 ℃. As can be seen from the data in Table 1, the density of the sample of comparative example 2 is only 85.54%, and the hardness is less than 90HV, which is a great difference from that of example 1.
Comparative example 2
Only the ball milling rotation speed is changed to be 100r/min, the process parameters in all other preparation processes are basically consistent with those in the embodiment 1, and the sintering temperature is 1400 ℃. As can be seen from the data in Table 1, the density and hardness of the sample of comparative example 1 are greatly reduced compared with those of example 1, which shows that a molybdenum sintered compact with high density and high hardness can be obtained at a lower sintering temperature only when the ball milling rotation speed reaches a higher value.
TABLE 1 comparison of properties of molybdenum metals prepared under different conditions
| Material sample | Relative density/% | hardness/HV |
| Example 1 | 95.37 | 438.3 |
| Comparative example 1 | 85.54 | 87.2 |
| Comparative example 2 | 91.39 | 149.9 |
Comparative example 3
The sintering raw material is unprocessed industrial molybdenum powder, the process parameters in all other preparation processes are basically consistent with those in the embodiment 1, and the sintering temperature is 1800 ℃. The micro-topography is shown in fig. 4.
As can be seen from a comparison of FIGS. 3 and 4, the grain size of the sample in example 1 is about 10 μm, while the grain size of the comparative sample is about 50 μm, indicating that the low-temperature sintering method is effective in controlling the grains of the sintered molybdenum compact.
Example 2
Weighing 100g of industrial molybdenum powder, wherein the appearance of the industrial molybdenum powder is shown in figure 1, the average particle size is 3 mu m, putting the industrial molybdenum powder into a ball milling tank, the ball-material ratio is 20:1, and the ball milling revolution speed is 450 r/min; the total time of ball milling is 36h, and the machine is stopped for 8-10 min every 1h of ball milling; argon is introduced as protective gas during ball milling to obtain the molybdenum powder after ball milling.
And taking the molybdenum powder subjected to ball milling out in a glove box under the argon atmosphere, putting the molybdenum powder into a prepared die, and performing unidirectional pressing at the pressing pressure of 200MPa for 80s to obtain a blank.
Putting the pressed blank into a hydrogen sintering furnace, ensuring the hydrogen sintering atmosphere, checking the purity and igniting, and increasing and decreasing the temperature speed: when the temperature is reduced to 700 ℃, the temperature can be naturally cooled along with the furnace; the sintering temperature is 1300 ℃, the heat preservation time is 6h, the hydrogen flow is 1.5L/min, and when the temperature is reduced to be below 80 ℃, a sample is taken out. Obtaining a molybdenum metal sintering blank, wherein the density of the molybdenum metal sintering blank reaches 95.1%; the hardness is up to 422 HV.
Example 3
Weighing 100g of industrial molybdenum powder, wherein the appearance of the industrial molybdenum powder is shown in figure 1, the average particle size is 3 mu m, putting the industrial molybdenum powder into a ball milling tank, the ball-material ratio is 25:1, and the ball milling revolution speed is 550 r/min; the total time of ball milling is 12 hours, and the machine is stopped for 8-10 min every 1 hour of ball milling; argon is introduced as protective gas during ball milling to obtain the molybdenum powder after ball milling.
And taking the molybdenum powder subjected to ball milling out in a glove box under the argon atmosphere, putting the molybdenum powder into a prepared die, and performing unidirectional pressing at the pressing pressure of 400MPa for 60s to obtain a blank.
Putting the pressed blank into a hydrogen sintering furnace, ensuring the hydrogen sintering atmosphere, checking the purity and igniting, and increasing and decreasing the temperature speed: when the temperature is reduced to 700 ℃, the temperature can be naturally cooled along with the furnace when the temperature is reduced to 1000 ℃, 12 ℃/min, 1000-1500 ℃, 6 ℃/min; the sintering temperature is 1500 ℃, the heat preservation time is 3.5h, the hydrogen flow is 2.0L/min, and when the temperature is reduced to be below 80 ℃, a sample is taken out. Obtaining a molybdenum metal sintering blank, wherein the density of the molybdenum metal sintering blank reaches 96.3%; the hardness is up to 445 HV.
Claims (8)
1. An activation sintering preparation method of an ultra-fine grain pure molybdenum metal material comprises the following steps:
1) preparing ball-milled molybdenum powder: taking a proper amount of molybdenum powder, putting the molybdenum powder into a ball milling tank according to a certain ball material ratio, and performing high-energy ball milling activation to obtain ball-milled molybdenum powder;
2) preparing a blank: pressing the powder subjected to ball milling in the step 1) as required to obtain a blank;
3) preparing a pure molybdenum sintered product: putting the blank in the step 2) into a sintering furnace; sintering and forming are carried out under the hydrogen atmosphere according to set parameters to obtain the pure molybdenum metal.
2. The method for preparing ultra-fine grain pure molybdenum metal material by activation sintering according to claim 1, wherein in the step 1), the molybdenum powder is industrial grade molybdenum powder with a particle size of 2-6 μm; the ball milling process is dry milling under protective gas: the revolution speed of ball milling is 300-600 r/min; the ball-material ratio is (10-30) to 1; the total ball milling time is 12-96 h; introducing inert gas for protection during ball milling; after the ball milling is finished, the powder in the ball milling tank can be taken out after the ball milling tank is cooled to the room temperature.
3. The method for preparing ultra-fine grain pure molybdenum metal material by activation sintering according to claim 2, wherein the inert atmosphere is argon atmosphere, the revolution speed of ball milling is 350r/min, the ball-to-material ratio is 10:1, and the total time of ball milling is 24 hours.
4. The method for preparing an ultra-fine grain pure molybdenum metal material through activation sintering according to claim 1, wherein in the step 2), the pressing pressure is 200-400 MPa, the pressing mode is unidirectional pressing or cold isostatic pressing, and the pressure holding time is 60-120 s.
5. The method of claim 4, wherein the pressing pressure is 300MPa and the dwell time is 120 s.
6. The method for preparing an ultra-fine grain pure molybdenum metal material by activation sintering according to claim 1, wherein in the step 3), sintering treatment is performed in a whole hydrogen atmosphere, and the sintering temperature is 1300-1600 ℃; when the temperature is lower than 1000 ℃, the heating rate is 8-12 ℃/min, the sintering temperature is 1000 ℃, and the heating rate is 4-6 ℃/min; the heat preservation time is 2-6 h, and the hydrogen flow is 0.8-2.0L/min.
7. The method for preparing ultra-fine grain pure molybdenum metal material by activation sintering according to claim 6, wherein the sintering temperature is 1400 ℃, the temperature rise rate is 10 ℃/min and 1000-1400 ℃ when the temperature is lower than 1000 ℃ in the sintering process, and the temperature rise rate is 5 ℃/min; the heat preservation time is 2h, and the hydrogen flow is 0.8L/min.
8. The preparation method according to any one of claims 1 to 7, wherein the molybdenum sintered compact is prepared.
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| CN113088847A (en) * | 2021-04-16 | 2021-07-09 | 中南大学 | Preparation method of high-density high-toughness ultrafine-grained molybdenum |
| CN114850473A (en) * | 2022-04-13 | 2022-08-05 | 金堆城钼业股份有限公司 | Molybdenum and molybdenum alloy material sintering method and application thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113088847A (en) * | 2021-04-16 | 2021-07-09 | 中南大学 | Preparation method of high-density high-toughness ultrafine-grained molybdenum |
| CN113088847B (en) * | 2021-04-16 | 2022-04-15 | 中南大学 | A kind of preparation method of high-density high-strength and tough ultrafine-grained molybdenum |
| CN114850473A (en) * | 2022-04-13 | 2022-08-05 | 金堆城钼业股份有限公司 | Molybdenum and molybdenum alloy material sintering method and application thereof |
| CN114850473B (en) * | 2022-04-13 | 2024-02-02 | 金堆城钼业股份有限公司 | Sintering method and application of molybdenum and molybdenum alloy material |
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