CN105195743A - Preparation method of large single-weight tungsten plate blank or molybdenum plate blank - Google Patents
Preparation method of large single-weight tungsten plate blank or molybdenum plate blank Download PDFInfo
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- CN105195743A CN105195743A CN201410266065.0A CN201410266065A CN105195743A CN 105195743 A CN105195743 A CN 105195743A CN 201410266065 A CN201410266065 A CN 201410266065A CN 105195743 A CN105195743 A CN 105195743A
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Abstract
The invention discloses a preparation method of a large single-weight tungsten plate blank or a molybdenum plate blank, belonging to the field of manufacturing of metal tungsten and molybdenum plate blanks. The method comprises the following steps: reducing tungsten powder with the Fisher particle size of 2.5-4.0 mu m or reducing molybdenum powder with the Fisher particle size of 2.0-4.0 mu m is used as a raw material; uniformly mixing reduced tungsten powder or reduced molybdenum powder, putting the mixture into a compression mould, and preparing a raw blank by isostatic pressing; and sintering the raw blank in a hydrogen-protected intermediate frequency sintering furnace to obtain a large single-weight tungsten plate blank or a molybdenum plate blank after sintering. The preparation method reduces the occurrence of the conditions of low density, local looseness, cracks, edge and corner dropping, warping and the like which are easily caused when a large single weight tungsten-molybdenum plate blank with the single weight of more than 200kg is sintered, can prepare the large single weight tungsten-molybdenum plate blank with high density and uniform tissue, and avoids the occurrence of layering and cracking phenomena in the rolling process, wherein the density of the plate blank reaches 93-96% of the theoretical density.
Description
Technical field
The present invention relates to the manufacture field of tungsten, molybdenum plate blank, particularly relate to the preparation method of a kind of large substance tungsten slab or molybdenum plate blank.
Background technology
At present, substance is called large substance sheet material more than the rolling tungsten of 200kg, molybdenum board material, corresponding slab is called substance slab, rolling tungsten, the molybdenum board material of large substance are very high to the requirement of slab, large substance tungsten slab prepared by conventional method, density is less than 93%, and very easily occurs that local is loose, crackle, falls the situation of limit arrisdefect, layering, cracking can be caused in the follow-up operation of rolling, have a strong impact on rolling tungsten, molybdenum board material quality.
Summary of the invention
The technical problem to be solved in the present invention is to provide the preparation method of a kind of large substance tungsten slab or molybdenum plate blank, substance can be applicable to more than the tungsten of 200kg, molybdenum board material rolling, layering, cracking can not be caused in the operation of rolling, have a strong impact on the problem of rolling tungsten, molybdenum board material quality.
For solving the problems of the technologies described above, the invention provides the preparation method of a kind of large substance tungsten slab or molybdenum plate blank, comprising:
Be the reduction tungsten powder of 2.5 ~ 4.0 μm or Fisher particle size with Fisher particle size be that the reduction molybdenum powder of 2.0 ~ 4.0 μm is for raw material;
Described reduction tungsten powder or reduction molybdenum powder being mixed loads in casted die mould, adopts isostatic pressing to obtain green billet;
At hydrogen shield Intermediate frequency sintering furnace, described green billet is sintered, after having sintered, namely obtain large substance tungsten slab or molybdenum plate blank.
Compared with prior art, beneficial effect of the present invention is: to be the reduction tungsten powder of 2.5 ~ 4.0 μm or Fisher particle size owing to adopting Fisher particle size be, and the reduction molybdenum powder of 2.0 ~ 4.0 μm is raw material, and coordinate isostatic pressing to obtain green billet, decrease the density easily occurred when substance sinters more than the large substance tungsten slab of 200kg low, local is loose, crackle, fall the generation of the situations such as limit arrisdefect, the tungsten slab prepared or molybdenum plate blank density high, even tissue, tungsten or molybdenum plate blank density reach 93% ~ 96% of solid density, avoid layering in the operation of rolling, the generation of cracking phenomena.
Detailed description of the invention
Be clearly and completely described the technical scheme in the embodiment of the present invention below, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on embodiments of the invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to protection scope of the present invention.
The embodiment of the present invention provides the preparation method of a kind of large substance tungsten slab or molybdenum plate blank, comprises the following steps:
Be the reduction tungsten powder of 2.5 ~ 4.0 μm or Fisher particle size with Fisher particle size be that the reduction molybdenum powder of 2.0 ~ 4.0 μm is for raw material;
Described reduction tungsten powder or reduction molybdenum powder being mixed loads in casted die mould, adopts isostatic pressing to obtain green billet;
At hydrogen shield Intermediate frequency sintering furnace, described green billet is sintered, after having sintered, namely obtain large substance tungsten slab or molybdenum plate blank.
In said method, reduction tungsten powder preferably adopts the mass percentage of tungsten in chemical constituent to be more than or equal to 99.95% tungsten powder, and reduction molybdenum powder preferably adopts the mass percentage of molybdenum in chemical constituent to be more than or equal to the molybdenum powder of 99.95%.The reduction tungsten powder or the reduction molybdenum powder that adopt above-mentioned Fei Shi density and purity are raw material, and coordinate isostatic pressing to obtain green billet and hydrogen shield Intermediate frequency sintering furnace sintering, ensure that the density of obtained tungsten slab or molybdenum plate blank is high.
In said method, the compacting pressure of isostatic pressing green billet is 180 ~ 250MPa, and the dwell time is 1.5 ~ 5min.
In said method, sinter described green billet at hydrogen shield Intermediate frequency sintering furnace, be 2000 DEG C ~ 2350 DEG C to tungsten green billet sintering temperature, the heating-up time is 10 ~ 15h, and temperature retention time is 16 ~ 30h; To molybdenum green billet sintering temperature 1800 DEG C ~ 2100 DEG C, heating-up time 8 ~ 15h, temperature retention time is 15 ~ 30h.
Below in conjunction with specific embodiment, preparation method of the present invention is described further.
Embodiment 1
Select W >=99.95%, Fisher particle size is 2.53 μm of reduction tungsten powders; The tungsten powder that reduced by the 200kg mixed loads in casted die mould, and adopts the method for isostatic pressing to obtain green billet, compacting pressure 200MPa, dwell time 2min; Hydrogen shield Intermediate frequency sintering furnace is used to carry out blank sintering, sintering temperature 2300 DEG C, heating-up time 12h, insulation 18h, obtained tungsten slab after sintering.
The tungsten steel slab surface free from flaw, spot, spar, dirty trace, bubbling and the superfusion phenomenon that sinter out, density 18.4g/cm
3, reach 95.6% of solid density, crackle loose without local, fall the situations such as limit arrisdefect and warpage.
Embodiment 2
Select Mo >=99.95%, Fisher particle size is 2.42 μm of reduction molybdenum powders.The molybdenum powder that reduced by the 300kg mixed loads in casted die mould, and adopts the method for isostatic pressing to obtain green billet, compacting pressure 200MPa, dwell time 3min.Hydrogen shield Intermediate frequency sintering furnace is used to carry out blank sintering, sintering temperature 2000 DEG C, heating-up time 10h, insulation 17h, obtained molybdenum plate blank after sintering.
The molybdenum plate blank surface free from flaw, spot, spar, dirty trace, bubbling and the superfusion phenomenon that sinter out, density 9.73g/cm
3, reach 95.1% of solid density, crackle loose without local, fall the situations such as limit arrisdefect and warpage.
The density that this preparation method easily occurs when decreasing the large substance tungsten slab sintering of substance more than 300kg is low, local is loose, crackle, fall the generation of the situations such as limit arrisdefect and warpage, prepare the large substance tungsten slab of high-compactness, even tissue, slab density reaches 93% ~ 96% of solid density, avoids the generation of layering in the operation of rolling, cracking phenomena.
The above; be only the present invention's preferably detailed description of the invention, but protection scope of the present invention is not limited thereto, is anyly familiar with those skilled in the art in the technical scope that the present invention discloses; the change that can expect easily or replacement, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claims.
Claims (4)
1. a preparation method for large substance tungsten slab or molybdenum plate blank, is characterized in that, comprise the following steps:
Be the reduction tungsten powder of 2.5 ~ 4.0 μm or Fisher particle size with Fisher particle size be that the reduction molybdenum powder of 2.0 ~ 4.0 μm is for raw material;
Described reduction tungsten powder or reduction molybdenum powder being mixed loads in casted die mould, adopts isostatic pressing to obtain green billet;
At hydrogen shield Intermediate frequency sintering furnace, described green billet is sintered, after having sintered, namely obtain large substance tungsten slab or molybdenum plate blank.
2. the preparation method of large substance tungsten slab according to claim 1 or molybdenum plate blank, is characterized in that, the compacting pressure of described isostatic pressing green billet is 180 ~ 250MPa, and the dwell time is 1.5 ~ 5min.
3. the preparation method of large substance tungsten slab according to claim 1 and 2 or molybdenum plate blank, it is characterized in that, describedly at hydrogen shield Intermediate frequency sintering furnace, described green billet to be sintered, it is 2000 DEG C ~ 2350 DEG C to tungsten green billet sintering temperature, heating-up time is 10 ~ 15h, and temperature retention time is 16 ~ 30h; To molybdenum green billet sintering temperature 1800 DEG C ~ 2100 DEG C, heating-up time 8 ~ 15h, temperature retention time is 15 ~ 30h.
4. the preparation method of large substance tungsten slab according to claim 1 and 2 or molybdenum plate blank, is characterized in that, in described reduction tungsten powder chemical constituent, the mass percentage of tungsten is more than or equal to 99.95%; In reduction molybdenum powder chemical constituent, the mass percentage of molybdenum is more than or equal to 99.95%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109894472A (en) * | 2019-03-14 | 2019-06-18 | 安泰天龙钨钼科技有限公司 | A kind of milling method of big L/D ratio molybdenum crucible spinning molybdenum plate |
| CN111254396A (en) * | 2020-01-21 | 2020-06-09 | 洛阳高新四丰电子材料有限公司 | Preparation method of molybdenum-tungsten alloy sputtering target material |
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| CN102041402A (en) * | 2009-10-23 | 2011-05-04 | 西安格美金属材料有限公司 | Preparation method of low-oxygen molybdenum alloy and application thereof |
| CN102699627A (en) * | 2012-01-04 | 2012-10-03 | 洛阳科威钨钼有限公司 | Process for manufacturing large, single and heavy molybdenum plate |
| CN102699326A (en) * | 2012-01-04 | 2012-10-03 | 洛阳科威钨钼有限公司 | Process for manufacturing large, single and heavy tungsten plate |
| CN103157795A (en) * | 2013-03-26 | 2013-06-19 | 金堆城钼业股份有限公司 | Preparation method of large-scale molybdenum plate blank |
| 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 |
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- 2014-06-13 CN CN201410266065.0A patent/CN105195743A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101642811A (en) * | 2009-06-29 | 2010-02-10 | 金堆城钼业股份有限公司 | Preparation method of molybdenum product with heavy single weight |
| CN102041402A (en) * | 2009-10-23 | 2011-05-04 | 西安格美金属材料有限公司 | Preparation method of low-oxygen molybdenum alloy and application thereof |
| CN102699627A (en) * | 2012-01-04 | 2012-10-03 | 洛阳科威钨钼有限公司 | Process for manufacturing large, single and heavy molybdenum plate |
| CN102699326A (en) * | 2012-01-04 | 2012-10-03 | 洛阳科威钨钼有限公司 | Process for manufacturing large, single and heavy tungsten plate |
| CN103157795A (en) * | 2013-03-26 | 2013-06-19 | 金堆城钼业股份有限公司 | Preparation method of large-scale molybdenum plate blank |
| 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 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109894472A (en) * | 2019-03-14 | 2019-06-18 | 安泰天龙钨钼科技有限公司 | A kind of milling method of big L/D ratio molybdenum crucible spinning molybdenum plate |
| CN111254396A (en) * | 2020-01-21 | 2020-06-09 | 洛阳高新四丰电子材料有限公司 | Preparation method of molybdenum-tungsten alloy sputtering target material |
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