CN103658652A - Method for sintering pure molybdenum metal sheet green pressing - Google Patents
Method for sintering pure molybdenum metal sheet green pressing Download PDFInfo
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- CN103658652A CN103658652A CN201210358966.3A CN201210358966A CN103658652A CN 103658652 A CN103658652 A CN 103658652A CN 201210358966 A CN201210358966 A CN 201210358966A CN 103658652 A CN103658652 A CN 103658652A
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Abstract
The invention relates to a method for sintering a pure molybdenum metal sheet green pressing in the technology of molybdenum metal processing. The method includes the steps that (1) the pure molybdenum metal sheet green pressing with the thickness of 0.4-1.5mm is placed into a hydrogen protection atmosphere furnace, and keeps the temperature of 1100-1300 DEG C for 1 to 3 hours; (2) after the step (1) is finished, the pure molybdenum metal sheet green pressing keeps the temperature of 1500-1700 DEG C for 0.5 to 3 hours. The method is simple in manufacturing process, short in production cycle, low in energy consumption, free of pollution, high in target product production efficiency, little in production equipment investment, small in occupied area, and suitable for industrial production.
Description
Technical field
The invention belongs to molybdenum processing technique field, particularly relate to a kind of sintering method of pure molybdenum light sheet green compact.
Background technology
Mo and Mo alloys is owing to having high-melting-point, high elastic modulus, good shock resistance and corrosion resistance, conduction, heat conductivility, fabulous heat-resistant anti-fatigue performance and the low excellent properties such as the coefficient of expansion, widely apply the fields such as medical treatment, metallurgy, electric light source, semiconductor devices, thermal structure part and nuclear industry, being most widely used with sheet material in the application of molybdenum materials.The processing of molybdenum board material mainly comprise following three processes: pressed compact moulding, sintering and rolling.Wherein sintering is that powder compact is heated under proper temperature, atmosphere, realizes the process connecting between particle by means of atomic migration, is that goods obtain the critical process with certain tissue and performance.The sintering of pure molybdenum belongs to unary system sintering, generally experiences low temperature presintering knot and two stages of high temperature sintering.The sintering temperature in low temperature presintering knot stage is generally 25% left and right of melting point metal temperature, and its Main Function is moisture and the volatile impurity of low melting point that metal volatilization is adsorbed.High temperature sintering phase temperature is generally about 50%~85% of melting point metal temperature, and Main Function is to make sintered body fine and close most possibly.
Existing pure molybdenum preparation is first by hydraulic press and mould mostly, and metal dust is pressed into square or rectangle slab green compact, then adopts step sintering processing, at each medium temperature point, needs the insulating process of certain hour.The method sintering step is tediously long, and conventional sintering step is 900 ℃, and 1200 ℃, 1300 ℃, 1400 ℃, 1500 ℃, 1600 ℃, 1800 ℃ and 1960 ℃, sintering time is long, production efficiency is low, conventionally needs sintering 18 ~ 25h, and the material structure that sintering obtains is thick, is unfavorable for post-production.And, because adopted blank is thicker, more than being mostly 20mm, during sintering, be difficult to obtain high density.The defects such as in addition, this sintering process also exists highly energy-consuming, production efficiency is low, the production cycle is long, process equipment investment is large.Visible, because blank is too thick and heavy, caused the complexity of follow-up sintering technique tediously long, the material density of acquisition and organize not good enoughly, and then has a strong impact on the combination property of material.Therefore, if reduce molybdenum plate green compact thickness, can greatly simplify its sintering process, and then improve material combination property.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of sintering method of pure molybdenum light sheet green compact, enhances productivity, and reduces and pollutes, and reduces costs.
The technical solution adopted for the present invention to solve the technical problems is: the sintering method that a kind of pure molybdenum light sheet green compact is provided:
(1), by thickness, being 0.4 to 1.5mm, pure molybdenum light sheet green compact was placed in hydrogen shield atmosphere furnace, the temperature insulations of 1100 to 1300 degrees Celsius 1 to 3 hour;
(2), after completing steps (1), 1500 to 1700 degrees Celsius of insulations 0.5 to 3 hour.
Described pure molybdenum light sheet green compact thickness is 0.4 millimeter, in step (1), 1100 degrees Celsius of insulations 1 hour, in step (2), at 1500 degrees Celsius, is incubated 1 hour.
Described pure molybdenum light sheet green compact thickness is 0.5 millimeter, in step (1), 1150 degrees Celsius of insulations 1 hour, in step (2), at 1550 degrees Celsius, is incubated 1 hour.
Described pure molybdenum light sheet green compact thickness is 0.6 millimeter, in step (1), 1150 degrees Celsius of insulations 1 hour, in step (2), at 1550 degrees Celsius, is incubated 1.5 hours.
Described pure molybdenum light sheet green compact thickness is 0.7 millimeter, in step (1), 1180 degrees Celsius of insulations 1 hour, in step (2), at 1600 degrees Celsius, is incubated 1 hour.
Described pure molybdenum light sheet green compact thickness is 0.8 millimeter, in step (1), 1200 degrees Celsius of insulations 1 hour, in step (2), at 1600 degrees Celsius, is incubated 1.5 hours.
Described pure molybdenum light sheet green compact thickness is 0.9 millimeter, in step (1), 1200 degrees Celsius of insulations 1.5 hours, in step (2), at 1650 degrees Celsius, is incubated 1 hour.
Described pure molybdenum light sheet green compact thickness is 1.3 millimeters, in step (1), 1250 degrees Celsius of insulations 3 hours, in step (2), at 1700 degrees Celsius, is incubated 2 hours.
Described pure molybdenum light sheet green compact thickness is 1.4 millimeters, in step (1), 1300 degrees Celsius of insulations 2 hours, in step (2), at 1700 degrees Celsius, is incubated 2 hours.
Described pure molybdenum light sheet green compact thickness is 1.5 millimeters, in step (1), 1300 degrees Celsius of insulations 2.5 hours, in step (2), at 1700 degrees Celsius, is incubated 2.5 hours.
The common thickness of pure molybdenum light sheet green compact adopting in the present invention is 0.4 ~ 1.5mm, the easier sintering of slab of this thickness.
Pre-sintering temperature described in the present invention is 1100 ~ 1300 ℃, and temperature retention time is 1 ~ 3 hour, and the moisture under this condition in blank and volatile impurity are able to abundant volatilization, and residualinternal stress is able to abundant elimination; Between powder particle, adhesive surface forms and expands, and part crystal particle crystal boundary forms, and the intensity of sintered body is improved.
The temperature of high temperature sintering described in the present invention is 1500 ~ 1700 ℃, temperature retention time is 0.5 ~ 3 hour, under this condition, atom and crystal boundary fully spread and flow, closed pore dwindles and nodularization, the size of hole and quantity reduce, and it is large that crystal grain diameter becomes, and number of die tails off, sintered body is further densified, and approaches theoretical value.
Beneficial effect
Preparation technology of the present invention is simple, with short production cycle, energy consumption is low, pollution-free, and target product production efficiency is high, investment of production equipment is little, occupied ground is little, is applicable to suitability for industrialized production.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.In addition should be understood that those skilled in the art can make various changes or modifications the present invention after having read the content of the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
A sintering method for pure molybdenum light sheet green compact, comprises the following steps:
(1), by thickness, being 0.4 to 1.5mm, pure molybdenum light sheet green compact was placed in hydrogen shield atmosphere furnace, the temperature insulations of 1100 to 1300 degrees Celsius 1 to 3 hour;
(2), after completing steps (1), 1500 to 1700 degrees Celsius of insulations 0.5 to 3 hour.
Embodiment 1
In hydrogen shield atmosphere furnace, the pure molybdenum light sheet green compact of 0.4mm thickness is carried out respectively to presintering and high temperature sintering; Wherein, the sintering temperature of described presintering is 1100 ℃, and temperature retention time is 1 hour; The sintering temperature of high temperature sintering is 1500 ℃, and temperature retention time is 1 hour.
Embodiment 2
In hydrogen shield atmosphere furnace, the pure molybdenum light sheet green compact of 0.5mm thickness is carried out respectively to presintering and high temperature sintering; Wherein, the sintering temperature of described presintering is 1150 ℃, and temperature retention time is 1 hour; The sintering temperature of high temperature sintering is 1550 ℃, and temperature retention time is 1 hour.
Embodiment 3
In hydrogen shield atmosphere furnace, the pure molybdenum light sheet green compact of 0.6mm thickness is carried out respectively to presintering and high temperature sintering; Wherein, the sintering temperature of described presintering is 1150 ℃, and temperature retention time is 1 hour; The sintering temperature of high temperature sintering is 1550 ℃, and temperature retention time is 1.5 hours.
Embodiment 4
In hydrogen shield atmosphere furnace, the pure molybdenum light sheet green compact of 0.7mm thickness is carried out respectively to presintering and high temperature sintering; Wherein, the sintering temperature of described presintering is 1180 ℃, and temperature retention time is 1 hour; The sintering temperature of high temperature sintering is 1600 ℃, and temperature retention time is 1 hour.
Embodiment 5
In hydrogen shield atmosphere furnace, the pure molybdenum light sheet green compact of 0.8mm thickness is carried out respectively to presintering and high temperature sintering; Wherein, the sintering temperature of described presintering is 1200 ℃, and temperature retention time is 1 hour; The sintering temperature of high temperature sintering is 1600 ℃, and temperature retention time is 1.5 hours.
Embodiment 6
In hydrogen shield atmosphere furnace, the pure molybdenum light sheet green compact of 0.9mm thickness is carried out respectively to presintering and high temperature sintering; Wherein, the sintering temperature of described presintering is 1200 ℃, and temperature retention time is 1.5 hours; The sintering temperature of high temperature sintering is 1650 ℃, and temperature retention time is 1 hour.
Embodiment 7
In hydrogen shield atmosphere furnace, the pure molybdenum light sheet green compact of 1mm thickness is carried out respectively to presintering and high temperature sintering; Wherein, the sintering temperature of described presintering is 1250 ℃, and temperature retention time is 1.5 hours; The sintering temperature of high temperature sintering is 1650 ℃, and temperature retention time is 1.5 hours.
Embodiment 8
In hydrogen shield atmosphere furnace, the pure molybdenum light sheet green compact of 1.1mm thickness is carried out respectively to presintering and high temperature sintering; Wherein, the sintering temperature of described presintering is 1250 ℃, and temperature retention time is 2 hours; The sintering temperature of high temperature sintering is 1700 ℃, and temperature retention time is 1.5 hours.
Embodiment 9
In hydrogen shield atmosphere furnace, the pure molybdenum light sheet green compact of 1.2mm thickness is carried out respectively to presintering and high temperature sintering; Wherein, the sintering temperature of described presintering is 1250 ℃, and temperature retention time is 2.5 hours; The sintering temperature of high temperature sintering is 1700 ℃, and temperature retention time is 2 hours.
Embodiment 10
In hydrogen shield atmosphere furnace, the pure molybdenum light sheet green compact of 1.3mm thickness is carried out respectively to presintering and high temperature sintering; Wherein, the sintering temperature of described presintering is 1250 ℃, and temperature retention time is 3 hours; The sintering temperature of high temperature sintering is 1700 ℃, and temperature retention time is 2 hours.
Embodiment 11
In hydrogen shield atmosphere furnace, the pure molybdenum light sheet green compact of 1.4mm thickness is carried out respectively to presintering and high temperature sintering; Wherein, the sintering temperature of described presintering is 1300 ℃, and temperature retention time is 2 hours; The sintering temperature of high temperature sintering is 1700 ℃, and temperature retention time is 2 hours.
Embodiment 12
In hydrogen shield atmosphere furnace, the pure molybdenum light sheet green compact of 1.5mm thickness is carried out respectively to presintering and high temperature sintering; Wherein, the sintering temperature of described presintering is 1300 ℃, and temperature retention time is 2.5 hours; The sintering temperature of high temperature sintering is 1700 ℃, and temperature retention time is 2.5 hours.
Claims (10)
1. a sintering method for pure molybdenum light sheet green compact, is characterized in that:
(1), by thickness, being 0.4 to 1.5mm, pure molybdenum light sheet green compact was placed in hydrogen shield atmosphere furnace, the temperature insulations of 1100 to 1300 degrees Celsius 1 to 3 hour;
(2), after completing steps (1), 1500 to 1700 degrees Celsius of insulations 0.5 to 3 hour.
2. the sintering method of a kind of pure molybdenum light sheet green compact according to claim 1, it is characterized in that, the thickness of described pure molybdenum light sheet green compact is 0.4 millimeter, in step (1), 1100 degrees Celsius of insulations 1 hour, in step (2), at 1500 degrees Celsius, is incubated 1 hour.
3. the sintering method of a kind of pure molybdenum light sheet green compact according to claim 1, it is characterized in that, described pure molybdenum light sheet green compact thickness is 0.5 millimeter, in step (1), 1150 degrees Celsius of insulations 1 hour, in step (2), at 1550 degrees Celsius, is incubated 1 hour.
4. the sintering method of a kind of pure molybdenum light sheet green compact according to claim 1, it is characterized in that, described pure molybdenum light sheet green compact thickness is 0.6 millimeter, in step (1), 1150 degrees Celsius of insulations 1 hour, in step (2), at 1550 degrees Celsius, is incubated 1.5 hours.
5. the sintering method of a kind of pure molybdenum light sheet green compact according to claim 1, it is characterized in that, described pure molybdenum light sheet green compact thickness is 0.7 millimeter, in step (1), 1180 degrees Celsius of insulations 1 hour, in step (2), at 1600 degrees Celsius, is incubated 1 hour.
6. the sintering method of a kind of pure molybdenum light sheet green compact according to claim 1, it is characterized in that, described pure molybdenum light sheet green compact thickness is 0.8 millimeter, in step (1), 1200 degrees Celsius of insulations 1 hour, in step (2), at 1600 degrees Celsius, is incubated 1.5 hours.
7. the sintering method of a kind of pure molybdenum light sheet green compact according to claim 1, it is characterized in that, described pure molybdenum light sheet green compact thickness is 0.9 millimeter, in step (1), 1200 degrees Celsius of insulations 1.5 hours, in step (2), at 1650 degrees Celsius, is incubated 1 hour.
8. the sintering method of a kind of pure molybdenum light sheet green compact according to claim 1, it is characterized in that, described pure molybdenum light sheet green compact thickness is 1.3 millimeters, in step (1), 1250 degrees Celsius of insulations 3 hours, in step (2), at 1700 degrees Celsius, is incubated 2 hours.
9. the sintering method of a kind of pure molybdenum light sheet green compact according to claim 1, it is characterized in that, described pure molybdenum light sheet green compact thickness is 1.4 millimeters, in step (1), 1300 degrees Celsius of insulations 2 hours, in step (2), at 1700 degrees Celsius, is incubated 2 hours.
10. the sintering method of a kind of pure molybdenum light sheet green compact according to claim 1, it is characterized in that, described pure molybdenum light sheet green compact thickness is 1.5 millimeters, in step (1), 1300 degrees Celsius of insulations 2.5 hours, in step (2), at 1700 degrees Celsius, is incubated 2.5 hours.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN105458266A (en) * | 2015-12-08 | 2016-04-06 | 西安瑞福莱钨钼有限公司 | Method for manufacturing molybdenum plate blank through sintering |
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CN1038230A (en) * | 1988-06-09 | 1989-12-27 | 天津大学冶金分校 | Low-temperature sintering high pure and ultra-fine crystal grain molybdenum base technology |
US5476632A (en) * | 1992-09-09 | 1995-12-19 | Stackpole Limited | Powder metal alloy process |
CN101254537A (en) * | 2008-04-11 | 2008-09-03 | 中南大学 | Method for preparing molybdenum and molybdenum alloys effuser by powder injection forming |
CN101956159A (en) * | 2010-09-30 | 2011-01-26 | 金堆城钼业股份有限公司 | Method for preparing high-purity molybdenum titanium sputtering target |
CN101966585A (en) * | 2010-11-01 | 2011-02-09 | 金堆城钼业股份有限公司 | Molybdenum blank preparing method |
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2012
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Patent Citations (5)
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CN1038230A (en) * | 1988-06-09 | 1989-12-27 | 天津大学冶金分校 | Low-temperature sintering high pure and ultra-fine crystal grain molybdenum base technology |
US5476632A (en) * | 1992-09-09 | 1995-12-19 | Stackpole Limited | Powder metal alloy process |
CN101254537A (en) * | 2008-04-11 | 2008-09-03 | 中南大学 | Method for preparing molybdenum and molybdenum alloys effuser by powder injection forming |
CN101956159A (en) * | 2010-09-30 | 2011-01-26 | 金堆城钼业股份有限公司 | Method for preparing high-purity molybdenum titanium sputtering target |
CN101966585A (en) * | 2010-11-01 | 2011-02-09 | 金堆城钼业股份有限公司 | Molybdenum blank preparing method |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN105458266A (en) * | 2015-12-08 | 2016-04-06 | 西安瑞福莱钨钼有限公司 | Method for manufacturing molybdenum plate blank through sintering |
CN105458266B (en) * | 2015-12-08 | 2018-03-02 | 西安瑞福莱钨钼有限公司 | It is a kind of to sinter the method for preparing molybdenum plate blank |
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Application publication date: 20140326 |