CN102218535B - Sintering method for molybdenum product - Google Patents
Sintering method for molybdenum product Download PDFInfo
- Publication number
- CN102218535B CN102218535B CN201110197483.5A CN201110197483A CN102218535B CN 102218535 B CN102218535 B CN 102218535B CN 201110197483 A CN201110197483 A CN 201110197483A CN 102218535 B CN102218535 B CN 102218535B
- Authority
- CN
- China
- Prior art keywords
- sintering
- molybdenum
- temperature
- stove
- molybdenum product
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
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, molybdenum product sintering process adopts step sintering processing mostly, needs the insulating process of certain hour at each medium temperature point.The method sintering step is tediously long, conventional sintering step is 900 ℃, 1200 ℃, 1300 ℃, 1400 ℃, 1500 ℃, 1600 ℃, 1800 ℃ and 1960 ℃, sintering time is long, production efficiency is low, conventionally need sintering 18h～25h, the molybdenum product crystal grain that sintering obtains mostly is the large crystal grain goods of 2～3 grades, and product is unfavorable for following process.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned the deficiencies in the prior art, provides a kind of simple, efficient, workable, without the sintering method of the molybdenum product of sintering step.The method has improved the production efficiency of molybdenum product sintering greatly, has saved cost, and the molybdenum product crystal grain that adopts the method sintering to obtain is tiny, and 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, the method is: adopt the mode of isostatic cool pressing that molybdenum powder or molybdenum alloy powder are pressed into blank, then blank is placed in to Intermediate frequency sintering furnace or electrical resistance sintering stove, under hydrogen atmosphere protection, carry out sintering, obtain molybdenum product after cooling with stove; The technique of described sintering is: adopt thermocouple accurate temperature measurement and control temperature deviation in stove to be not more than ± 5 ℃, with the heating rate of 20 ℃/min, temperature in stove is risen to 500 ℃, then with the heating rate of 2 ℃/min, temperature in stove is risen to 1600 ℃～1900 ℃.
The sintering method of above-mentioned a kind of molybdenum product, the quality purity of described molybdenum powder is 99.96%.
The sintering method of above-mentioned a kind of molybdenum product, the weight of described blank is not more than 2.0 kilograms.
The sintering method of above-mentioned a kind of molybdenum product, described molybdenum alloy powder is molybdenum-lanthanum alloy powder.
The sintering method of above-mentioned a kind of molybdenum product, in described molybdenum-lanthanum alloy powder, the quality percentage composition of lanthanum is not more than 0.3%.
The sintering method of above-mentioned a kind of molybdenum product, the granularity of described molybdenum powder and molybdenum alloy powder is 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, efficient, workable.
2, compacting of the present invention adopts the mode of isostatic cool pressing, after compacting, is to rely on model moral supernatural power to be attached together between molybdenum powder or molybdenum alloy powder particle, and particle is not out of shape.
3, in sintering process of the present invention without sintering step, do not need the insulating process of medium temperature point, shortened sintering time, greatly improved production efficiency, 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 crystal grain rank reaches 4～9 grades, and 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.
Accompanying drawing explanation
Fig. 1 is the fracture surface sweeping electromicroscopic photograph of the blank after the embodiment of the present 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 present invention 1 compacting, and multiplication factor is 1000 times.
Fig. 3 is the fracture surface sweeping electromicroscopic photograph of the molybdenum product prepared of the embodiment of the present invention 1 sintering, and multiplication factor is 1000 times.
Fig. 4 is the metallographic structure figure of the molybdenum product prepared of the embodiment of the present invention 1 sintering.
Fig. 5 is the metallographic structure figure of the molybdenum alloy goods prepared of the embodiment of the present invention 2 sintering.
Fig. 6 is the fracture surface sweeping electromicroscopic photograph of the molybdenum product prepared of the embodiment of the present invention 3 sintering, and multiplication factor is 1000 times.
Fig. 7 is the metallographic structure figure of the molybdenum product prepared of the embodiment of the present invention 3 sintering.
Fig. 8 is the metallographic structure figure of the molybdenum alloy goods prepared of the embodiment of the present invention 4 sintering.
Fig. 9 is the fracture surface sweeping electromicroscopic photograph of the molybdenum product prepared of the embodiment of the present invention 5 sintering, and multiplication factor is 1000 times.
Figure 10 is the metallographic structure figure of the molybdenum product prepared of the embodiment of the present invention 5 sintering.
Figure 11 is the metallographic structure figure of the molybdenum alloy goods prepared of the embodiment of the present invention 6 sintering.
Figure 12 is the fracture surface sweeping electromicroscopic photograph of the molybdenum product prepared of the embodiment of the present invention 7 sintering, and multiplication factor is 1000 times.
Figure 13 is the metallographic structure figure of the molybdenum product prepared of the embodiment of the present invention 7 sintering.
Figure 14 is the metallographic structure figure of the molybdenum alloy goods prepared of the embodiment of the present invention 8 sintering.
The specific embodiment
Embodiment 1
Adopting the mode of isostatic cool pressing is 3.7 μ m by 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 in to Intermediate frequency sintering furnace, under hydrogen atmosphere protection, carry out sintering, in sintering process, adopt thermocouple accurate temperature measurement and control temperature deviation in stove to be not more than ± 5 ℃, first with the heating rate of 20 ℃/min, temperature in stove is risen to 500 ℃ from room temperature (25 ℃), then with the heating rate of 2 ℃/min, temperature in stove is risen to 1600 ℃, accumulative total heating-up time 9.56h, after cooling with stove, obtain 94% the molybdenum product that density reaches solid density.
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 the present embodiment molybdenum powder, from photo, can find out, in pressing process, molybdenum powder particle is not out of shape.
Fig. 3 is the fracture stereoscan photograph of the molybdenum product prepared of the present embodiment sintering, can find out that molybdenum product organizes substantially densified from photo.Fig. 4 is the metallographic structure figure of the molybdenum product prepared of the present embodiment sintering, and as can be seen from the figure, molybdenum product is substantially densified, and crystallite dimension is below 20 μ m, and crystal grain rank is 8 grades.
In the sintering process of the present embodiment, without sintering step, do not need the insulating process of medium temperature point, shortened sintering time, greatly improve production efficiency, saved cost, molybdenum product prepared by sintering carries out density measurement through drainage, the density 9.57g/cm of molybdenum product
2.
Embodiment 2
The sintering method of the present embodiment is identical with embodiment 1, and wherein difference is: be raw materials usedly 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 prepared of the present embodiment sintering, and as can be seen from the figure, molybdenum alloy goods are substantially densified, and crystallite dimension is below 20 μ m, and crystal grain rank is 9 grades.
In the sintering process of the present embodiment, without sintering step, do not need the insulating process of medium temperature point, shortened sintering time, greatly improved production efficiency, saved cost.
Embodiment 3
Adopting the mode of isostatic cool pressing is 2.5 μ m by 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 in to electrical resistance sintering stove, under hydrogen atmosphere protection, carry out sintering, in sintering process, adopt thermocouple accurate temperature measurement and control temperature deviation in stove to be not more than ± 5 ℃, first with the heating rate of 20 ℃/min, temperature in stove is risen to 500 ℃ from room temperature (25 ℃), then with the heating rate of 2 ℃/min, temperature in stove is risen to 1700 ℃, accumulative total heating-up time 10.39h, after cooling with stove, obtain 95.5% the molybdenum product that density reaches solid density.
Fig. 6 is the fracture stereoscan photograph of the molybdenum product prepared of the present embodiment sintering, from photo, can find out, sintering structure crystal grain is tiny.Fig. 7 is the metallographic structure figure of the molybdenum product prepared of the present embodiment sintering, and as can be seen from the figure, molybdenum product is substantially densified, and crystallite dimension is below 20 μ m, and crystal grain rank is 9 grades.
In the sintering process of the present embodiment, without sintering step, do not need the insulating process of medium temperature point, shortened sintering time, greatly improve production efficiency, saved cost, molybdenum product prepared by sintering carries out density measurement through drainage, the density 9.72g/cm of molybdenum product
2.
Embodiment 4
The sintering method of the present embodiment is identical with embodiment 3, and wherein difference is: be raw materials usedly 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 prepared of the present embodiment sintering, and as can be seen from the figure, molybdenum alloy goods are substantially densified, and crystallite dimension is below 20 μ m, and crystal grain rank is 9 grades.
In the sintering process of the present embodiment, without sintering step, do not need the insulating process of medium temperature point, shortened sintering time, greatly improved production efficiency, saved cost.
Embodiment 5
Adopting the mode of isostatic cool pressing is 4.0 μ m by 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 in to Intermediate frequency sintering furnace, under hydrogen atmosphere protection, carry out sintering, in sintering process, adopt thermocouple accurate temperature measurement and control temperature deviation in stove to be not more than ± 5 ℃, first with the heating rate of 20 ℃/min, temperature in stove is risen to 500 ℃ from room temperature (25 ℃), then with the heating rate of 2 ℃/min, temperature in stove is risen to 1800 ℃, accumulative total heating-up time 11.22h, after cooling with stove, obtain 97% the molybdenum product that density reaches solid density.
Fig. 9 is the fracture stereoscan photograph of the molybdenum product prepared of the present embodiment sintering, from photo, can find out, metal compaction degree improves very fast.Figure 10 is the metallographic structure figure of the molybdenum product prepared of the present embodiment sintering, and as can be seen from the figure, crystallite dimension is 20 μ m～30 μ m, and crystal grain rank is 6 grades.
In the sintering process of the present embodiment, without sintering step, do not need the insulating process of medium temperature point, shortened sintering time, greatly improve production efficiency, saved cost, molybdenum product prepared by sintering carries out density measurement through drainage, the density 9.87g/cm of molybdenum product
2.
Embodiment 6
The sintering method of the present embodiment is identical with embodiment 5, and wherein difference is: be raw materials usedly 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 prepared of the present embodiment sintering, and as can be seen from the figure, metal compaction degree improves very fast, and crystallite dimension is 20 μ m～30 μ m, and crystal grain rank is 6 grades.
In the sintering process of the present embodiment, without sintering step, do not need the insulating process of medium temperature point, shortened sintering time, greatly improved production efficiency, saved cost.
Embodiment 7
Adopting the mode of isostatic cool pressing is 3.7 μ m by 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 in to electrical resistance sintering stove, under hydrogen atmosphere protection, carry out sintering, in sintering process, adopt thermocouple accurate temperature measurement and control temperature deviation in stove to be not more than ± 5 ℃, first with the heating rate of 20 ℃/min, temperature in stove is risen to 500 ℃ from room temperature (25 ℃), then with the heating rate of 2 ℃/min, temperature in stove is risen to 1900 ℃, accumulative total heating-up time 12.06h, after cooling with stove, obtain 98% the molybdenum product that density reaches solid density.
Figure 12 is the fracture stereoscan photograph of the molybdenum product prepared of the present embodiment sintering, from photo, can find out, grain structure is densified.Figure 13 is the metallographic structure figure of the molybdenum product prepared of the present embodiment sintering, and as can be seen from the figure, crystallite dimension is 30 μ m～40 μ m, and crystal grain rank is 4 grades.
In the sintering process of the present embodiment, without sintering step, do not need the insulating process of medium temperature point, shortened sintering time, greatly improve production efficiency, saved cost, molybdenum product prepared by sintering carries out density measurement through drainage, the density 9.98g/cm of molybdenum product
2.
Embodiment 8
The sintering method of the present embodiment is identical with embodiment 7, and wherein difference is: be raw materials usedly 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 prepared of the present embodiment sintering, and as can be seen from the figure, grain structure is densified, and crystallite dimension is 20 μ m～30 μ m, and crystal grain rank is 6 grades.
In the sintering process of the present embodiment, without sintering step, do not need the insulating process of medium temperature point, shortened sintering time, greatly improved production efficiency, saved cost.
The above; it is only preferred embodiment of the present invention; not the present invention is done to any restriction, every any simple modification of above embodiment being done according to invention technical spirit, change and equivalent structure change, and all still belong in the protection domain of technical solution of the present invention.
Claims (5)
1. the sintering method of a molybdenum product, it is characterized in that, the method is: adopt the mode of isostatic cool pressing that molybdenum powder or molybdenum alloy powder are pressed into blank, then blank is placed in to Intermediate frequency sintering furnace or electrical resistance sintering stove, under hydrogen atmosphere protection, carry out sintering, obtain molybdenum product after cooling with stove; The technique of described sintering is: adopt thermocouple accurate temperature measurement and control temperature deviation in stove to be not more than ± 5 ℃, with the heating rate of 20 ℃/min, temperature in stove is risen to 500 ℃, then with the heating rate of 2 ℃/min, temperature in stove is risen to 1600 ℃～1900 ℃; The density of described molybdenum product reaches 94%～98% of solid density; The granularity of described molybdenum powder and molybdenum alloy powder is 2.5 μ m～4.0 μ m; The system of described compacting is: pressing pressure 150MPa～200MPa, dwell time 10min.
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 molybdenum-lanthanum alloy powder.
5. the sintering method of a kind of molybdenum product according to claim 4, is characterized in that, in described molybdenum-lanthanum alloy powder, the quality percentage composition of lanthanum is not more than 0.3%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110197483.5A CN102218535B (en) | 2011-07-14 | 2011-07-14 | Sintering method for molybdenum product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110197483.5A CN102218535B (en) | 2011-07-14 | 2011-07-14 | Sintering method for molybdenum product |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102218535A CN102218535A (en) | 2011-10-19 |
| CN102218535B true CN102218535B (en) | 2014-05-14 |
Family
ID=44775376
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110197483.5A Active CN102218535B (en) | 2011-07-14 | 2011-07-14 | Sintering method for molybdenum product |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102218535B (en) |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102626845B (en) * | 2012-03-27 | 2015-06-03 | 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 |
| 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 |
| CN104525948B (en) * | 2014-12-23 | 2017-03-15 | 金堆城钼业股份有限公司 | A kind of preparation method of molybdenum alloy electrode |
| CN108543947B (en) * | 2018-05-11 | 2020-11-24 | 成都联虹钼业有限公司 | Preparation method of molybdenum blank |
| 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 |
| 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 |
| 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 |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6103392A (en) * | 1994-12-22 | 2000-08-15 | Osram Sylvania Inc. | Tungsten-copper composite powder |
| CN1296503C (en) * | 2005-05-15 | 2007-01-24 | 王治国 | Molybdenum-base alloy and its preparing method |
| AU2007217054A1 (en) * | 2006-02-17 | 2007-08-30 | Monsanto Technology Llc | Transition metal-containing catalysts and processes for their preparation and use as fuel cell catalysts |
| CN101423911B (en) * | 2007-10-29 | 2011-09-07 | 四平市北威钼业有限公司 | Manufacturing technology of molybdenum-based rare-earth alloy slab and equipment thereof |
| CN101722308B (en) * | 2008-10-11 | 2012-01-25 | 四平市北威钼业有限公司 | Molybdenum-base rare earth powder metallurgy forming plug and manufacturing method thereof |
| CN101934372B (en) * | 2010-07-30 | 2012-07-25 | 西北有色金属研究院 | Method for preparing large powder metallurgy TZM blank with uniform carbon and oxygen distribution |
-
2011
- 2011-07-14 CN CN201110197483.5A patent/CN102218535B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN102218535A (en) | 2011-10-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102218535B (en) | Sintering method for molybdenum product | |
| CN103045925B (en) | Preparation process of sputtered rotary molybdenum-sodium-alloy tubular target | |
| CN100489131C (en) | Method for manufacturing difficult-to-form pure rhenium sheet | |
| CN103071793B (en) | Molybdenum sputtering target material hot isostatic pressure production method | |
| CN103774020B (en) | The preparation method of Mo Re alloys foil | |
| CN103805952B (en) | A kind of large scale high purity tungsten target and production method thereof | |
| CN101948299A (en) | Preparation method of compact magnesia ceramics by sintering | |
| CN107586987B (en) | Titanium carbide-titanium diboride two-phase enhancing Cu-base composites and preparation method thereof | |
| CN112813397B (en) | Preparation method of molybdenum-sodium alloy plate-shaped target | |
| CN104073771B (en) | A kind of molybdenum mixes the preparation method of sodium sputtering target material | |
| CN105585317B (en) | A kind of cadmium stannate target and preparation method thereof | |
| CN103820691B (en) | A kind of normal pressure-sintered preparation method of FeAl/TiC matrix material | |
| CN101775578A (en) | ZnAl target preparation method and prepared ZnAl target | |
| CN102826856B (en) | High-purity low-density ITO target material and preparation method thereof | |
| CN102241508B (en) | Preparation method of high density BaTi2O5 bulk | |
| CN104342619A (en) | Method for manufacturing molybdenum target material | |
| CN105112859A (en) | Method for preparing Na-doped molybdenum planar targets | |
| CN103320636B (en) | Novel method for quickly preparing high-performance Mg2Si0.3Sn0.7-based thermoelectric material | |
| CN106129241B (en) | The method that solid reaction process prepares stacking faults chalcogenide thermoelectric material | |
| CN103447530A (en) | Method for preparing pure titanium miniature parts on basis of multi-physical-field activated sintering | |
| CN103909264A (en) | High-performance Cu2Se block thermoelectric material with nanopore structure and rapid preparation method of high-performance Cu2Se block thermoelectric material | |
| CN104402450A (en) | Method for quickly preparing Ti2AlN ceramic powder on the basis of thermal explosion reaction at low temperature | |
| CN102581282A (en) | Process for preparing large-specification tungsten plate billet by means of resistance sintering | |
| CN101570321A (en) | Method for preparing BixSbyTe(3-z) thermoelectric material with high performance and nano structure | |
| CN104874796B (en) | WC Ni miniature parts, cutting tool and preparation method thereof are prepared based on multiple physical field activated sintering |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |