CN101642811B - Preparation method of molybdenum product with heavy single weight - Google Patents
Preparation method of molybdenum product with heavy single weight Download PDFInfo
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- CN101642811B CN101642811B CN200910087584XA CN200910087584A CN101642811B CN 101642811 B CN101642811 B CN 101642811B CN 200910087584X A CN200910087584X A CN 200910087584XA CN 200910087584 A CN200910087584 A CN 200910087584A CN 101642811 B CN101642811 B CN 101642811B
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Abstract
The invention relates to a preparation method of a molybdenum product with heavy single weight, in particular to a method for preparing a rare metal product by a powder metallurgy method. The method is characterized by comprising the following steps: taking molybdenum dioxide as a raw material; carrying out high-temperature hydrogen reduction on the molybdenum dioxide to obtain a raw material molybdenum powder; pulverizing and sieving the initial raw material molybdenum powder, and then processing the molybdenum powder with a high-energy collision air-flow mill; and finally pressing the obtained molybdenum powder with large apparent density, high flow velocity and low impurity content into a molybdenum blank, and then sintering the molybdenum blank to obtain the molybdenum product. In themethod, the initial molybdenum powder with large apparent density, good fluidity and low impurity content is obtained by high-temperature hydrogen reduction on the molybdenum dioxide, and the apparent density of the molybdenum powder is further improved by high-energy collision air-flow mill processing to finally obtain the molybdenum product with the heavy single weight after forming and sintering. The method of the invention has low requirement on the raw material, easy controlled production process, and simple, safe and reliable operation, thus being applicable to batch production; and themolybdenum product with the heavy single weight which is 50% more than that of the common molybdenum power can be prepared in a mould with the same size.
Description
Technical field
A kind of preparation method of molybdenum product with heavy single weight relates to the method that a kind of powder metallurgy prepares the rare metal goods.
Background technology
Molybdenum product generally is by the powder metallurgy method preparation, comprises main technique steps such as powder process, shaping, sintering.Common molybdenum powder prepares big substance goods has some contradictions to be difficult to handle 1) common molybdenum powder apparent density is less at 1.0～2.0g/cm
3, prepare big substance goods and just must increase die size, along with the increase of mould, processes such as the shaping sintering very difficulty that becomes, even the product of some super large substance are as the molybdenum plate more than the 200kg, on existing equipment even can't finish.2) common molybdenum powder is mobile poor, and molybdenum powder is difficult for being filled into each corner of mould when preparing big substance product.3) during big substance product sintering, diffusion length is big, and impurity is got rid of difficulty.
Use plasma apparatus to after the molybdenum powder processing, can avoid above-mentioned contradiction.But plasma apparatus is relatively more expensive, output is little, and needs strict atmosphere protection.
Summary of the invention
Purpose of the present invention is exactly the deficiency that exists at above-mentioned prior art, provide a kind of low to ingredient requirement, production technology is easy to control, easy and simple to handle, cost is low, the preparation method of the molybdenum product with heavy single weight of easy realization of industrialization.
The present invention seeks to that following technical scheme realizes.
A kind of preparation method of molybdenum product with heavy single weight, it is characterized in that adopting molybdenum dioxide is raw material, the molybdenum dioxide high-temperature hydrogen reduction is obtained the raw material molybdenum powder, again with the pulverizing of initial feed molybdenum powder, screening after high energy collision type airflow milling is handled, will obtain big apparent density, high flow rate at last, hang down and contain that assorted molybdenum powder is pressed into the molybdenum base, sintering is made molybdenum product.
The preparation method of a kind of molybdenum product with heavy single weight of the present invention is characterized in that the reduction temperature of molybdenum dioxide high-temperature hydrogen reduction acquisition raw material molybdenum powder is 1100～1400 ℃, recovery time 2～6h.
The preparation method of a kind of molybdenum product with heavy single weight of the present invention is characterized in that described initial feed molybdenum powder is pulverized, screening process is carry out crushing and screening in vacuum breaking screening integral machine after, to cross 200 mesh standard sieves, gets sieve molybdenum powder down.
The preparation method of a kind of molybdenum product with heavy single weight of the present invention is characterized in that the processing time of described high energy collision type airflow milling processing procedure is 1～4h.
The preparation method of a kind of molybdenum product with heavy single weight of the present invention is characterized in that the described forming pressure that is pressed into the molybdenum base is 180～220MPa, dwell time 8～12min, secondary releasing pressure automatically.
The preparation method of a kind of molybdenum product with heavy single weight of the present invention is characterized in that it is 1850～1950 ℃ that described sintering is made the sintering temperature of molybdenum product, temperature retention time 4～6h.
Method of the present invention, utilize the molybdenum dioxide high-temperature hydrogen reduction to obtain big apparent density, good fluidity, initial molybdenum powder that impurity content is low, handle the apparent density that further improves molybdenum powder through high energy collision type airflow milling again, after be shaped, sintering obtains the large piece weight molybdenum product.Method of the present invention, low to ingredient requirement, the molybdenum dioxide in the normal productive process all can be used as raw material of the present invention.Production technology is easy to control, and is easy and simple to handle, safe, reliable, is suitable for producing in batches, can prepare in onesize mould than the big molybdenum product more than 50% of common molybdenum powder substance.
Description of drawings
Fig. 1 is the process chart of method of the present invention.
The specific embodiment
A kind of preparation method of molybdenum product with heavy single weight adopts the molybdenum dioxide high-temperature hydrogen reduction to obtain the initial feed molybdenum powder, this initial feed molybdenum powder is handled through high energy collision type airflow milling obtained big apparent density, high flow rate, lowly contains assorted molybdenum powder.This molybdenum powder is made the large piece weight molybdenum product of indication of the present invention through shaping, sintering; Its step of preparation process comprises:
(1) with the molybdenum dioxide is raw material;
(2) with the molybdenum dioxide high-temperature hydrogen reduction, 1100～1400 ℃ of reduction temperatures exceed 200～500 ℃ of common molybdenum powder reduction temperature, recovery time 2～6h, and hydrogen flowing quantity is decided according to thickness of feed layer, boat charge and type of furnace size;
(3) this molybdenum powder is carried out crushing and screening in vacuum breaking screening integral machine, the vacuum of vacuum breaking screening integral machine is-800Pa that 200 mesh standard sieves are got undersize;
(4) with the molybdenum powder of high energy collision type airflow milling processing through high-temperature hydrogen reduction, processing time 1～4h;
(5) the molybdenum powder batch mixing in the bipyramid batch mixer after airflow milling is handled closes batch, closes batch time 1～6;
(6) this molybdenum powder is formed according to product requirement; Forming pressure is 180～220MPa, dwell time 8～12min, secondary releasing pressure automatically;
(7) shaping molybdenum base is carried out sintering in intermediate frequency furnace or resistance furnace; Sintering temperature is 1850～1950 ℃, temperature retention time 4～6h;
(8) detect the packing warehouse-in and obtain product of the present invention.
Embodiment 1
Get molybdenum dioxide 500kg, in single district Muffle furnace, carry out hydrogen reduction.The reducing process parameter is: 1300 ℃ of temperature, temperature retention time 4h, boat charge 3.0kg/ boat, hydrogen flowing quantity 0.7m
3/ h.
Molybdenum powder after above-mentioned technology reduction has caking, is placed in the vacuum breaking screening integral machine to handle, and vacuum is-800Pa to cross 200 mesh standard sieves.
After above-mentioned PROCESS FOR TREATMENT, receive molybdenum powder 371.50kg, apparent density reaches 3.06g/cm
3, Hall flow velocity 26s/50g, O content reaches below the 300ppm.This molybdenum powder is handled processing time 4h in QLM-240B type high energy collision type airflow milling.
Molybdenum powder after the above-mentioned high energy collision type airflow milling PROCESS FOR TREATMENT crossed 200 mesh standard sieves and in the bipyramid batch mixer, carry out batch mixing and close batch.The molybdenum powder apparent density of closing after testing after criticizing reaches 3.48g/cm
3, Hall flow velocity 29s/50g below the O content 900ppm, is suitable as the raw material of large piece weight molybdenum product.
Get the above-mentioned molybdenum powder 180kg rubber mold of packing into, die size is 1300 * 340 * 100mm, the common molybdenum powder 110～120kg that can only pack into, and molybdenum plate base substance improves more than 50%.Use hydrostatic pressing, forming technology is pressure 190MPa, dwell time 12min, secondary releasing pressure automatically.
Above-mentioned molybdenum pressed compact is placed the intermediate frequency furnace sintering, and sintering process sees the following form.
This patent large common-substance molybdenum plate sintering process
Molybdenum plate substance through this technology sintering is 178kg, and appearance and size is 875 * 265 * 77mm, and actual density is 9.98g/cm
3
Embodiment 2
Raw material molybdenum powder preparation process is identical with example one, takes by weighing the 22kg rubber mold of packing into, and die size is Φ 80 * 1000mm, and common molybdenum powder can only be packed into about 13kg, and molybdenum bar base substance improves more than 60%.Use hydrostatic pressing, forming technology is pressure 190MPa, dwell time 12min, secondary releasing pressure automatically.
Behind sintering, the substance of molybdenum bar is 12.07kg, and appearance and size is Φ 60 * 750mm, and actual density is 9.81g/cm
3
Use the inventive method, in the mould of substance 13kg, prepared the sintering molybdenum bar of substance above 20kg.
Claims (3)
1. the preparation method of a molybdenum product with heavy single weight, it is characterized in that adopting molybdenum dioxide is raw material, the molybdenum dioxide high-temperature hydrogen reduction is obtained the raw material molybdenum powder, again with the pulverizing of initial feed molybdenum powder, screening after high energy collision type airflow milling is handled, will obtain big apparent density, high flow rate at last, hang down and contain that assorted molybdenum powder is pressed into the molybdenum base, sintering is made molybdenum product; The reduction temperature that its molybdenum dioxide high-temperature hydrogen reduction obtains the raw material molybdenum powder is 1100～1400 ℃, recovery time 2～6h; Described initial feed molybdenum powder is pulverized, screening process is carry out crushing and screening in vacuum breaking screening integral machine after, to cross 200 mesh standard sieves, gets sieve molybdenum powder down; The processing time of described high energy collision type airflow milling processing procedure is 1～4h.
2. the preparation method of a kind of molybdenum product with heavy single weight according to claim 1 is characterized in that the described forming pressure that is pressed into the molybdenum base is 180～220MPa, dwell time 8～12min, secondary releasing pressure automatically.
3. the preparation method of a kind of molybdenum product with heavy single weight according to claim 1 is characterized in that it is 1850～1950 ℃ that described sintering is made the sintering temperature of molybdenum product, temperature retention time 4～6h.
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| CN105195743A (en) * | 2014-06-13 | 2015-12-30 | 北京矿冶研究总院 | Preparation method of large single-weight tungsten plate blank or molybdenum plate blank |
| CN109014198A (en) * | 2018-08-16 | 2018-12-18 | 北京科技大学 | A method of preparing the pure molybdenum part of high-performance |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4045216A (en) * | 1975-11-03 | 1977-08-30 | Amax Inc. | Direct reduction of molybdenum oxide to substantially metallic molybdenum |
| US5173108A (en) * | 1989-03-21 | 1992-12-22 | Gte Products Corporation | Method for controlling the oxygen content in agglomerated molybdenum powders |
| CN2423027Y (en) * | 2000-03-17 | 2001-03-14 | 俞斌 | Colliding type fluid-bed jet mill |
| CN101259584A (en) * | 2008-04-25 | 2008-09-10 | 胡延槽 | Method for preparing high-density molybdenum tube |
| CN101352759A (en) * | 2008-09-02 | 2009-01-28 | 金堆城钼业股份有限公司 | Method for preparing special type molybdenum powder |
-
2009
- 2009-06-29 CN CN200910087584XA patent/CN101642811B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4045216A (en) * | 1975-11-03 | 1977-08-30 | Amax Inc. | Direct reduction of molybdenum oxide to substantially metallic molybdenum |
| US5173108A (en) * | 1989-03-21 | 1992-12-22 | Gte Products Corporation | Method for controlling the oxygen content in agglomerated molybdenum powders |
| CN2423027Y (en) * | 2000-03-17 | 2001-03-14 | 俞斌 | Colliding type fluid-bed jet mill |
| CN101259584A (en) * | 2008-04-25 | 2008-09-10 | 胡延槽 | Method for preparing high-density molybdenum tube |
| CN101352759A (en) * | 2008-09-02 | 2009-01-28 | 金堆城钼业股份有限公司 | Method for preparing special type molybdenum powder |
Non-Patent Citations (2)
| Title |
|---|
| Hiroshi Endo等.制备高纯钼粉或钨粉及高纯氧化钼或氧化钨粉的方法.《钼业经济技术》.1991,(第2期),第35页-第46页. * |
| JP昭63-42302A 1988.02.23 |
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