CN102218535A - Sintering method for molybdenum product - Google Patents
Sintering method for molybdenum product Download PDFInfo
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- CN102218535A CN102218535A CN 201110197483 CN201110197483A CN102218535A CN 102218535 A CN102218535 A CN 102218535A CN 201110197483 CN201110197483 CN 201110197483 CN 201110197483 A CN201110197483 A CN 201110197483A CN 102218535 A CN102218535 A CN 102218535A
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Abstract
The invention discloses a sintering method for a molybdenum product. The method comprises the following steps of: pressing molybdenum powder or molybdenum alloy powder into a blank in a cold isostatic pressing way; placing the blank into an intermediate frequency sintering furnace or a resistance sintering furnace; sintering under the protection of hydrogen atmosphere; cooling together with the furnace to obtain the molybdenum product. The sintering process comprises the following steps of: precisely measuring the temperature by using a thermocouple, controlling the deviation of temperature in the furnace to be within +/- 5 DEG C; raising the temperature in the furnace to the temperature of 500 DEG C in the temperature rising rate of 20 DEG C/min; and raising the temperature in the furnace to 1,600 and 1,900 DEG C in the temperature rising rate of 2 DEG C/min. The sintering method is simple and efficient, and easy to implement; sintering steps do not exist in the sintering process, namely a heat preservation process of a medium temperature point is not needed, so the sintering time is shortened, the production efficiency is greatly improved, and the cost is saved. By the sintering method, the grains of the sintered molybdenum product are small, and the metal densification degree is relatively high.
Description
Technical field
The invention belongs to molybdenum product sintering technology field, be specifically related to a kind of sintering method of molybdenum product.
Background technology
At present, the molybdenum product sintering process adopts the step sintering processing mostly, promptly all needs the insulating process of certain hour at each medium temperature point.This method sintering step is tediously long, sintering step commonly used is 900 ℃, 1200 ℃, 1300 ℃, 1400 ℃, 1500 ℃, 1600 ℃, 1800 ℃ and 1960 ℃, sintering time is long, production efficiency is low, usually need sintering 18h~25h, the molybdenum product crystal grain that sintering obtains mostly is 2~3 grades big crystal grain goods, and product is unfavorable for following process.
Summary of the invention
Technical problem to be solved by this invention is at above-mentioned the deficiencies in the prior art, provides a kind of simple, efficient, workable, the sintering method of the molybdenum product of no sintering step.This method has improved the production efficiency of molybdenum product sintering greatly, has saved cost, and the molybdenum product crystal grain that adopts this method sintering to obtain is tiny, and the metal compaction degree is higher.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of sintering method of molybdenum product, it is characterized in that, this method is: adopt the mode of isostatic cool pressing that molybdenum powder or molybdenum alloy powder are pressed into blank, then blank is placed intermediate frequency sintering furnace or electrical resistance sintering stove, under the hydrogen atmosphere protection, carry out sintering, with obtaining molybdenum product after the stove cooling; The technology of described sintering is: adopt the accurate thermometric of thermocouple and control that temperature deviation is not more than in the stove ± 5 ℃, with the heating rate of 20 ℃/min temperature in the stove is risen to 500 ℃, the heating rate with 2 ℃/min rises to 1600 ℃~1900 ℃ with temperature in the stove then.
The sintering method of above-mentioned a kind of molybdenum product, the quality purity of described molybdenum powder are 99.96%.
The sintering method of above-mentioned a kind of molybdenum product, the weight of described blank are not more than 2.0 kilograms.
The sintering method of above-mentioned a kind of molybdenum product, described molybdenum alloy powder are the molybdenum-lanthanum alloy powder.
The sintering method of above-mentioned a kind of molybdenum product, the quality percentage composition of lanthanum is not more than 0.3% in the described molybdenum-lanthanum alloy powder.
The sintering method of above-mentioned a kind of molybdenum product, the granularity of described molybdenum powder and molybdenum alloy powder are 2.5 μ m~4.0 μ m.
The sintering method of above-mentioned a kind of molybdenum product, the system of described compacting is: pressing pressure 150MPa~200MPa, dwell time 10min.
The sintering method of above-mentioned a kind of molybdenum product, the density of described molybdenum product reaches 94%~98% of solid density.
The present invention compared with prior art has the following advantages:
1, the inventive method is simple, and is efficient, workable.
2, the mode of isostatic cool pressing is adopted in compacting of the present invention, after the compacting, is to rely on model moral supernatural power to be attached together between molybdenum powder or molybdenum alloy powder particle, and particle is distortion not.
3, no sintering step in the sintering process of the present invention does not promptly need the insulating process of medium temperature point, has shortened sintering time, has improved production efficiency greatly, has saved cost.
4, the molybdenum product crystal grain that adopts method sintering of the present invention to obtain is tiny, and crystallite dimension is less than 40 μ m, and the crystal grain rank reaches 4~9 grades, and the metal compaction degree is higher, and density reaches 94%~98% of solid density.
Below in conjunction with drawings and Examples, technical scheme of the present invention is described in further detail.
Description of drawings
Fig. 1 is the fracture surface sweeping electromicroscopic photograph of the blank after the embodiment of the invention 1 compacting, and multiplication factor is 5000 times.
Fig. 2 is the fracture surface sweeping electromicroscopic photograph of the blank after the embodiment of the invention 1 compacting, and multiplication factor is 1000 times.
Fig. 3 is the fracture surface sweeping electromicroscopic photograph of the molybdenum product of the embodiment of the invention 1 sintering preparation, and multiplication factor is 1000 times.
Fig. 4 is the metallographic structure figure of the molybdenum product of the embodiment of the invention 1 sintering preparation.
Fig. 5 is the metallographic structure figure of the molybdenum alloy goods of the embodiment of the invention 2 sintering preparation.
Fig. 6 is the fracture surface sweeping electromicroscopic photograph of the molybdenum product of the embodiment of the invention 3 sintering preparation, and multiplication factor is 1000 times.
Fig. 7 is the metallographic structure figure of the molybdenum product of the embodiment of the invention 3 sintering preparation.
Fig. 8 is the metallographic structure figure of the molybdenum alloy goods of the embodiment of the invention 4 sintering preparation.
Fig. 9 is the fracture surface sweeping electromicroscopic photograph of the molybdenum product of the embodiment of the invention 5 sintering preparation, and multiplication factor is 1000 times.
Figure 10 is the metallographic structure figure of the molybdenum product of the embodiment of the invention 5 sintering preparation.
Figure 11 is the metallographic structure figure of the molybdenum alloy goods of the embodiment of the invention 6 sintering preparation.
Figure 12 is the fracture surface sweeping electromicroscopic photograph of the molybdenum product of the embodiment of the invention 7 sintering preparation, and multiplication factor is 1000 times.
Figure 13 is the metallographic structure figure of the molybdenum product of the embodiment of the invention 7 sintering preparation.
Figure 14 is the metallographic structure figure of the molybdenum alloy goods of the embodiment of the invention 8 sintering preparation.
The specific embodiment
Embodiment 1
Adopting the mode of isostatic cool pressing is 3.7 μ m with granularity; quality purity is that 99.96% molybdenum powder is pressed into blank; pressing pressure 180MPa; dwell time 10min; billet weight is not more than 2.0 kilograms; then blank is placed the intermediate frequency sintering furnace; under the hydrogen atmosphere protection, carry out sintering; adopt the accurate thermometric of thermocouple in the sintering process and control the interior temperature deviation of stove to be not more than ± 5 ℃; heating rate with 20 ℃/min rises to 500 ℃ with temperature in the stove from room temperature (25 ℃) earlier; heating rate with 2 ℃/min rises to 1600 ℃ with temperature in the stove then, and accumulative total heating-up time 9.56h is with obtaining 94% the molybdenum product that density reaches solid density after the stove cooling.
Fig. 1 and Fig. 2 are the fracture surface sweeping electromicroscopic photographs (Fig. 1 multiplication factor is 5000 times, and Fig. 2 multiplication factor is 1000 times) of the blank that obtains after repressed of present embodiment molybdenum powder, from photo as can be seen, not distortion of molybdenum powder particle in the pressing process.
Fig. 3 is the fracture stereoscan photograph of the molybdenum product of present embodiment sintering preparation, and molybdenum product is organized densified substantially as can be seen from photo.Fig. 4 is the metallographic structure figure of the molybdenum product of present embodiment sintering preparation, and as can be seen from the figure, molybdenum product is densified substantially, and crystallite dimension is below the 20 μ m, and the crystal grain rank is 8 grades.
No sintering step in the sintering process of present embodiment does not promptly need the insulating process of medium temperature point, has shortened sintering time, improved production efficiency greatly, saved cost, the molybdenum product of sintering preparation carries out density measurement through drainage, the density 9.57g/cm of molybdenum product
2
Embodiment 2
The sintering method of present embodiment is identical with embodiment 1, and wherein difference is: raw materials usedly be not more than 0.3% molybdenum-lanthanum alloy powder for lanthanum quality percentage composition.
Fig. 5 is the metallographic structure figure of the molybdenum alloy goods of present embodiment sintering preparation, and as can be seen from the figure, the molybdenum alloy goods are densified substantially, and crystallite dimension is below the 20 μ m, and the crystal grain rank is 9 grades.
No sintering step in the sintering process of present embodiment does not promptly need the insulating process of medium temperature point, has shortened sintering time, has improved production efficiency greatly, has saved cost.
Embodiment 3
Adopting the mode of isostatic cool pressing is 2.5 μ m with granularity; quality purity is that 99.96% molybdenum powder is pressed into blank; pressing pressure 200MPa; dwell time 10min; billet weight is not more than 2.0 kilograms; then blank is placed the electrical resistance sintering stove; under the hydrogen atmosphere protection, carry out sintering; adopt the accurate thermometric of thermocouple in the sintering process and control the interior temperature deviation of stove to be not more than ± 5 ℃; heating rate with 20 ℃/min rises to 500 ℃ with temperature in the stove from room temperature (25 ℃) earlier; heating rate with 2 ℃/min rises to 1700 ℃ with temperature in the stove then, and accumulative total heating-up time 10.39h is with obtaining 95.5% the molybdenum product that density reaches solid density after the stove cooling.
Fig. 6 is the fracture stereoscan photograph of the molybdenum product of present embodiment sintering preparation, and as can be seen, sintering structure crystal grain is tiny from photo.Fig. 7 is the metallographic structure figure of the molybdenum product of present embodiment sintering preparation, and as can be seen from the figure, molybdenum product is densified substantially, and crystallite dimension is below the 20 μ m, and the crystal grain rank is 9 grades.
No sintering step in the sintering process of present embodiment does not promptly need the insulating process of medium temperature point, has shortened sintering time, improved production efficiency greatly, saved cost, the molybdenum product of sintering preparation carries out density measurement through drainage, the density 9.72g/cm of molybdenum product
2
Embodiment 4
The sintering method of present embodiment is identical with embodiment 3, and wherein difference is: raw materials usedly be not more than 0.3% molybdenum-lanthanum alloy powder for lanthanum quality percentage composition.
Fig. 8 is the metallographic structure figure of the molybdenum alloy goods of present embodiment sintering preparation, and as can be seen from the figure, the molybdenum alloy goods are densified substantially, and crystallite dimension is below the 20 μ m, and the crystal grain rank is 9 grades.
No sintering step in the sintering process of present embodiment does not promptly need the insulating process of medium temperature point, has shortened sintering time, has improved production efficiency greatly, has saved cost.
Embodiment 5
Adopting the mode of isostatic cool pressing is 4.0 μ m with granularity; quality purity is that 99.96% molybdenum powder is pressed into blank; pressing pressure 150MPa; dwell time 10min; billet weight is not more than 2.0 kilograms; then blank is placed the intermediate frequency sintering furnace; under the hydrogen atmosphere protection, carry out sintering; adopt the accurate thermometric of thermocouple in the sintering process and control the interior temperature deviation of stove to be not more than ± 5 ℃; heating rate with 20 ℃/min rises to 500 ℃ with temperature in the stove from room temperature (25 ℃) earlier; heating rate with 2 ℃/min rises to 1800 ℃ with temperature in the stove then, and accumulative total heating-up time 11.22h is with obtaining 97% the molybdenum product that density reaches solid density after the stove cooling.
Fig. 9 is the fracture stereoscan photograph of the molybdenum product of present embodiment sintering preparation, and as can be seen, the metal compaction degree improves very fast from photo.Figure 10 is the metallographic structure figure of the molybdenum product of present embodiment sintering preparation, and as can be seen from the figure, crystallite dimension is 20 μ m~30 μ m, and the crystal grain rank is 6 grades.
No sintering step in the sintering process of present embodiment does not promptly need the insulating process of medium temperature point, has shortened sintering time, improved production efficiency greatly, saved cost, the molybdenum product of sintering preparation carries out density measurement through drainage, the density 9.87g/cm of molybdenum product
2
Embodiment 6
The sintering method of present embodiment is identical with embodiment 5, and wherein difference is: raw materials usedly be not more than 0.3% molybdenum-lanthanum alloy powder for lanthanum quality percentage composition.
Figure 11 is the metallographic structure figure of the molybdenum alloy goods of present embodiment sintering preparation, and as can be seen from the figure, the metal compaction degree improves very fast, and crystallite dimension is 20 μ m~30 μ m, and the crystal grain rank is 6 grades.
No sintering step in the sintering process of present embodiment does not promptly need the insulating process of medium temperature point, has shortened sintering time, has improved production efficiency greatly, has saved cost.
Embodiment 7
Adopting the mode of isostatic cool pressing is 3.7 μ m with granularity; quality purity is that 99.96% molybdenum powder is pressed into blank; pressing pressure 200MPa; dwell time 10min; billet weight is not more than 2.0 kilograms; then blank is placed the electrical resistance sintering stove; under the hydrogen atmosphere protection, carry out sintering; adopt the accurate thermometric of thermocouple in the sintering process and control the interior temperature deviation of stove to be not more than ± 5 ℃; heating rate with 20 ℃/min rises to 500 ℃ with temperature in the stove from room temperature (25 ℃) earlier; heating rate with 2 ℃/min rises to 1900 ℃ with temperature in the stove then, and accumulative total heating-up time 12.06h is with obtaining 98% the molybdenum product that density reaches solid density after the stove cooling.
Figure 12 is the fracture stereoscan photograph of the molybdenum product of present embodiment sintering preparation, and as can be seen, grain structure is densified from photo.Figure 13 is the metallographic structure figure of the molybdenum product of present embodiment sintering preparation, and as can be seen from the figure, crystallite dimension is 30 μ m~40 μ m, and the crystal grain rank is 4 grades.
No sintering step in the sintering process of present embodiment does not promptly need the insulating process of medium temperature point, has shortened sintering time, improved production efficiency greatly, saved cost, the molybdenum product of sintering preparation carries out density measurement through drainage, the density 9.98g/cm of molybdenum product
2
Embodiment 8
The sintering method of present embodiment is identical with embodiment 7, and wherein difference is: raw materials usedly be not more than 0.3% molybdenum-lanthanum alloy powder for lanthanum quality percentage composition.
Figure 14 is the metallographic structure figure of the molybdenum alloy goods of present embodiment sintering preparation, and as can be seen from the figure, grain structure is densified, and crystallite dimension is 20 μ m~30 μ m, and the crystal grain rank is 6 grades.
No sintering step in the sintering process of present embodiment does not promptly need the insulating process of medium temperature point, has shortened sintering time, has improved production efficiency greatly, has saved cost.
The above; it only is preferred embodiment of the present invention; be not that the present invention is done any restriction, everyly any simple modification that above embodiment did, change and equivalent structure changed, all still belong in the protection domain of technical solution of the present invention according to the invention technical spirit.
Claims (8)
1. the sintering method of a molybdenum product, it is characterized in that this method is: adopt the mode of isostatic cool pressing that molybdenum powder or molybdenum alloy powder are pressed into blank, then blank is placed intermediate frequency sintering furnace or electrical resistance sintering stove, under the hydrogen atmosphere protection, carry out sintering, with obtaining molybdenum product after the stove cooling; The technology of described sintering is: adopt the accurate thermometric of thermocouple and control that temperature deviation is not more than in the stove ± 5 ℃, with the heating rate of 20 ℃/min temperature in the stove is risen 500 ℃, the heating rate with 2 ℃/min rises to 1600 ℃~1900 ℃ with temperature in the stove then.
2. the sintering method of a kind of molybdenum product according to claim 1 is characterized in that, the quality purity of described molybdenum powder is 99.96%.
3. the sintering method of a kind of molybdenum product according to claim 1 is characterized in that, the weight of described blank is not more than 2.0 kilograms.
4. the sintering method of a kind of molybdenum product according to claim 1 is characterized in that, described molybdenum alloy powder is the molybdenum-lanthanum alloy powder.
5. the sintering method of a kind of molybdenum product according to claim 4 is characterized in that, the quality percentage composition of lanthanum is not more than 0.3% in the described molybdenum-lanthanum alloy powder.
6. the sintering method of a kind of molybdenum product according to claim 1 is characterized in that, the granularity of described molybdenum powder and molybdenum alloy powder is 2.5 μ m~4.0 μ m.
7. the sintering method of a kind of molybdenum product according to claim 1 is characterized in that, the system of described compacting is: pressing pressure 150MPa~200MPa, dwell time 10min.
8. the sintering method of a kind of molybdenum product according to claim 1 is characterized in that, the density of described molybdenum product reaches 94%~98% of solid density.
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CN102626845A (en) * | 2012-03-27 | 2012-08-08 | 苏州先端稀有金属有限公司 | Molybdenum lanthanum alloy tray processing method |
CN103132033A (en) * | 2013-03-26 | 2013-06-05 | 金堆城钼业股份有限公司 | Method for preparing molybdenum target |
CN103433490A (en) * | 2013-08-26 | 2013-12-11 | 四川省有色冶金研究院有限公司 | Method for preparing molybdenum semi-finished products |
CN103658653A (en) * | 2012-09-24 | 2014-03-26 | 上海六晶金属科技有限公司 | One-time sintering method of pure molybdenum metal sheet green pressing |
CN104525948A (en) * | 2014-12-23 | 2015-04-22 | 金堆城钼业股份有限公司 | Preparation method for molybdenum alloy electrode |
CN108543947A (en) * | 2018-05-11 | 2018-09-18 | 成都联虹钼业有限公司 | A kind of preparation method of molybdenum base |
CN110983090A (en) * | 2019-12-31 | 2020-04-10 | 金堆城钼业股份有限公司 | Sintering method of carbon-containing molybdenum alloy |
CN113399662A (en) * | 2021-06-21 | 2021-09-17 | 中南大学 | Preparation method of molybdenum-lanthanum alloy sintered blank and product thereof |
CN113600815A (en) * | 2021-06-24 | 2021-11-05 | 厦门虹鹭钨钼工业有限公司 | Preparation method of dry-type doped molybdenum alloy |
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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CN102626845A (en) * | 2012-03-27 | 2012-08-08 | 苏州先端稀有金属有限公司 | Molybdenum lanthanum alloy tray processing method |
CN103658653A (en) * | 2012-09-24 | 2014-03-26 | 上海六晶金属科技有限公司 | One-time sintering method of pure molybdenum metal sheet green pressing |
CN103132033A (en) * | 2013-03-26 | 2013-06-05 | 金堆城钼业股份有限公司 | Method for preparing molybdenum target |
CN103132033B (en) * | 2013-03-26 | 2016-03-16 | 金堆城钼业股份有限公司 | A kind of method preparing molybdenum target |
CN103433490A (en) * | 2013-08-26 | 2013-12-11 | 四川省有色冶金研究院有限公司 | Method for preparing molybdenum semi-finished products |
CN104525948A (en) * | 2014-12-23 | 2015-04-22 | 金堆城钼业股份有限公司 | Preparation method for molybdenum alloy electrode |
CN108543947A (en) * | 2018-05-11 | 2018-09-18 | 成都联虹钼业有限公司 | A kind of preparation method of molybdenum base |
CN110983090A (en) * | 2019-12-31 | 2020-04-10 | 金堆城钼业股份有限公司 | Sintering method of carbon-containing molybdenum alloy |
CN110983090B (en) * | 2019-12-31 | 2021-07-13 | 金堆城钼业股份有限公司 | Sintering method of carbon-containing molybdenum alloy |
CN113399662A (en) * | 2021-06-21 | 2021-09-17 | 中南大学 | Preparation method of molybdenum-lanthanum alloy sintered blank and product thereof |
CN113399662B (en) * | 2021-06-21 | 2022-03-18 | 中南大学 | Preparation method of molybdenum-lanthanum alloy sintered blank and product thereof |
CN113600815A (en) * | 2021-06-24 | 2021-11-05 | 厦门虹鹭钨钼工业有限公司 | Preparation method of dry-type doped molybdenum alloy |
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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