CN103817342A - Manufacturing method for tungsten powder used for making crucible in pressed mode - Google Patents

Manufacturing method for tungsten powder used for making crucible in pressed mode Download PDF

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CN103817342A
CN103817342A CN201410096400.7A CN201410096400A CN103817342A CN 103817342 A CN103817342 A CN 103817342A CN 201410096400 A CN201410096400 A CN 201410096400A CN 103817342 A CN103817342 A CN 103817342A
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tungsten powder
crucible
manufacturing
tungsten
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CN103817342B (en
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容斌
段明
吴博
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ZHUZHOU JIABANG REFRACTORY METAL Co Ltd
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Abstract

The invention discloses a manufacturing method for tungsten powder used for making a crucible in a pressed mode. The manufacturing method is characterized by further comprising the following steps that A reduction is conducted, wherein blue tungsten powder is placed in a boat and fed into a tube furnace to be reduced, hydrogen flow ranges from10 m<3>/h to 25 m<3>/h, temperature ranges from 850 DEG C to 950 DEG C, time is 30 min, and the tungsten powder with different granularities is obtained, cooled and discharged out of the furnace; B primary screening is conducted, wherein the tungsten powder obtained in the step A is screened through a 180-mesh screen, and the screened tungsten powder is discharged for standby application; C blending is conducted, wherein the tungsten powder which has different granularities and is obtained in the step B is mixed in proportion for 3.5 hours; D secondary screening is conducted, wherein the tungsten powder obtained in the step C is screened through a 160-mesh screen, and screened materials are the tungsten powder. The manufacturing method is mainly used for the tungsten powder used for making the crucible in the pressed mode.

Description

A kind of for suppressing the preparation method of tungsten powder of crucible
Technical field
The present invention relates to a kind of preparation method of tungsten powder, relate in particular to a kind of for suppressing the preparation method of tungsten powder of crucible.
Background technology
Tungsten crucible is mainly used in the industry such as rare-earth smelting and Medium Frequency Induction Heating Furnace, is one of leading products in tungsten special-shaped product.Tungsten crucible is mainly to pass through isostatic cool pressing by tungsten powder to make blank, then passes through high temperature sintering in intermediate frequency furnace, finally becomes goods.Its density requirements is higher, and require longer service life, production high density, the tungsten crucible of high life, for the suppression performance of tungsten powder have relatively high expectations, compact strength require large, mouldability better, yield rate is just high.If tungsten powder compact strength is low, in pressing process, there will be blank to split the end or crackle appears in bottom, can cause a large amount of significant loss, product cost raises, and serviceability is poor, uncontested advantage on market.In order to reduce tungsten crucible cost, improve serviceability, improve the compact strength of tungsten powder, improve its suppression performance, be the problem that the present invention will solve.
Summary of the invention
The object of the present invention is to provide a kind of for suppressing the preparation method of tungsten powder of crucible, with improve tungsten powder compact strength, improve its suppression performance.
For achieving the above object, technical solution of the present invention is: a kind of for suppressing the preparation method of tungsten powder of crucible, it is characterized in that following steps:
A. reduction: blue tungsten powder is placed in to boat and sends into tube furnace at hydrogen flowing quantity 10-25m 3under/h, temperature is reduced, and temperature is controlled at 850-950 ℃, 30 minutes time, obtains varigrained tungsten powder and comes out of the stove after cooling;
B. once screening: the tungsten powder that steps A is obtained is crossed 180 mesh sieves, gets the lower tungsten powder of sieve stand-by;
C. close and criticize: the varigrained tungsten powder that step B is obtained is arranged in pairs or groups in proportion and mixed 3.5 hours;
D. regrading: the mixing tungsten powder that step C is obtained is crossed 160 mesh sieves, and screenings is product.
The invention has the beneficial effects as follows:
Due to the tungsten powder that adopts tube furnace (four pipe furnaces) to produce, carry out by a certain percentage thickness collocation, its particle mean size is 2.8 μ m-3.2 μ m, compact strength≤1.6MPa when the original employing of compact strength>=2.2MPa(is thick, thin tungsten powder is arranged in pairs or groups, evidence tungsten powder compact strength is controlled at 1.8-2.4MPa and is advisable, too high elastic after effect is on the contrary large, in the time of compacting crucible, there will be crackle), compacting qualification rate is brought up to more than 90% by 50%, and the tungsten crucible density of being produced by tungsten powder has exceeded 18.5g/cm 3, be improved service life, cost.
Table 1 technological parameter and the tungsten powder particle-size table of comparisons
Figure BDA0000477348620000021
Figure BDA0000477348620000031
Table 2 tungsten powder thickness blending powder table
Figure BDA0000477348620000032
Table 3 closes batch tungsten powder Analysis of Physical table
The specific embodiment
Below in conjunction with embodiment, the present invention and the specific embodiment thereof are described in further detail.
The invention is characterized in following steps:
A. reduction: blue tungsten powder is placed in to boat and sends into tube furnace at hydrogen flowing quantity 10-25m 3under/h, temperature is reduced, and temperature is controlled at 850-950 ℃, 30 minutes time, obtains varigrained tungsten powder and comes out of the stove after cooling;
B. once screening: the tungsten powder that steps A is obtained is crossed 180 mesh sieves, gets the lower tungsten powder of sieve stand-by;
C. close and criticize: the varigrained tungsten powder that step B is obtained is arranged in pairs or groups in proportion and mixed 3.5 hours;
D. regrading: the mixing tungsten powder that step C is obtained is crossed 160 mesh sieves, and screenings is product.
Below provide embodiments of the invention
Example 1
15,20,20,25m reduction: the blue tungsten powder 2.5kg that is 15 μ by granularity packs in heat-resisting guiding principle boat, sends into tubular reduction furnace (four pipe furnaces) and is respectively at hydrogen flowing quantity: 3under/h, reduce, corresponding temperature is respectively: 950 ℃, 930 ℃, 850 ℃, 900 ℃, the time is 30 minutes, and the corresponding tungsten powder particle-size obtaining is respectively 4.5 μ m, 3.2 μ m, 2.3 μ m, 1.5 μ m, comes out of the stove after cooling; Once screening: the tungsten powder after coming out of the stove is crossed to 180 mesh sieves, get the lower tungsten powder of sieve stand-by; Close and criticize: by tungsten powder 300kg under the sieve of tungsten powder 200kg, 1.5 μ m under the sieve of tungsten powder 200kg, 2.3 μ m under the sieve of tungsten powder 300kg, 3.2 μ m under the sieve of 4.5 μ m, collocation mixes 3.5 hours; Regrading: mixed tungsten powder is crossed to 160 mesh sieves, and extracting screen underflow is product---the tungsten powder of compacting crucible, its particle mean size is 2.9 μ m.
Example 2
16,21,21,25m hydrogen flowing quantity is respectively: 3/ h, temperature correspondence is respectively 940 ℃, 920 ℃, 850 ℃, 900 ℃, and the time is 30 minutes, the corresponding tungsten powder particle-size obtaining is respectively 4.4 μ m, 3.0 μ m, 2.2 μ m, 1.4 μ m, comes out of the stove after cooling, after mixing, obtaining particle mean size is 2.8 μ m, and all the other are with example 1.
Example 3
14,19,21,25m hydrogen flowing quantity is respectively: 3/ h, temperature correspondence is respectively 950 ℃, 920 ℃, 860 ℃, 900 ℃, and the time is 30 minutes, the corresponding tungsten powder particle-size obtaining is respectively 4.6 μ m, 3.3 μ m, 2.2 μ m, 1.4 μ m, comes out of the stove after cooling, after mixing, obtaining particle mean size is 3.0 μ m, and all the other are with example 1.
Once the object of screening and regrading is all to remove the mechanical entrainment in tungsten powder.

Claims (1)

1. for suppressing the preparation method of tungsten powder for crucible, it is characterized in that following steps:
Reduction: blue tungsten powder is placed in to boat and sends into tube furnace temperature under hydrogen flowing quantity 10-25m3/h and reduce, temperature is controlled at 850-950 ℃, 30 minutes time, obtains varigrained tungsten powder and comes out of the stove after cooling;
B. once screening: the tungsten powder that steps A is obtained is crossed 180 mesh sieves, gets the lower tungsten powder of sieve stand-by;
C. close and criticize: the varigrained tungsten powder that step B is obtained is arranged in pairs or groups in proportion and mixed 3.5 hours;
D. regrading: the mixing tungsten powder that step C is obtained is crossed 160 mesh sieves, and screenings is product.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106141198A (en) * 2015-04-02 2016-11-23 上海六晶科技股份有限公司 The method of ultrafine tungsten powder is prepared in a kind of direct-reduction
CN110614379A (en) * 2019-09-18 2019-12-27 河源普益硬质合金厂有限公司 Purification treatment method for superfine tungsten powder

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GB772067A (en) * 1954-05-06 1957-04-10 Egyesuelt Izzolampa Improvements in the manufacture of tungsten powder and articles made therefrom
JPS61242902A (en) * 1985-04-19 1986-10-29 Natl Res Inst For Metals Production of ultrafine particle of high-melting metallic oxide
CN101318223A (en) * 2008-07-14 2008-12-10 中南大学 Method for manufacturing heavy pressure blank strength tungsten powder with ammonium metatungstate and ammonium paratungstate
CN101642816A (en) * 2008-08-05 2010-02-10 江西稀有稀土金属钨业集团有限公司 Process for producing tungsten powder
CN102161101A (en) * 2011-05-31 2011-08-24 赣州虹飞钨钼材料有限公司 A method of preparing high purity tungsten material used for very large scale integrated circuits
CN103240421A (en) * 2013-05-27 2013-08-14 江西稀有稀土金属钨业集团有限公司 Method and system for producing high compact strength tungsten powder

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谢中华等: "钨粉制备工艺对压坯强度影响的研究", 《中国钨业》, vol. 25, no. 6, 31 December 2010 (2010-12-31), pages 28 - 30 *
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106141198A (en) * 2015-04-02 2016-11-23 上海六晶科技股份有限公司 The method of ultrafine tungsten powder is prepared in a kind of direct-reduction
CN110614379A (en) * 2019-09-18 2019-12-27 河源普益硬质合金厂有限公司 Purification treatment method for superfine tungsten powder

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