CN1621172A - Method for preparing tungsten base high specific gravity alloy board - Google Patents
Method for preparing tungsten base high specific gravity alloy board Download PDFInfo
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- CN1621172A CN1621172A CN 200410103516 CN200410103516A CN1621172A CN 1621172 A CN1621172 A CN 1621172A CN 200410103516 CN200410103516 CN 200410103516 CN 200410103516 A CN200410103516 A CN 200410103516A CN 1621172 A CN1621172 A CN 1621172A
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Abstract
The present invention is the powder metallurgical and hot plastic treating process of producing high precision W-base great specific weight W-Ni-Fe alloy plate. The production process includes the successive steps of: mixing W powder, Ni powder, Fe powder and small amount of Co powder and Y powder of average granularity 2.8-3.2 microns, pressing into blank, sintering, canning rolling, annealing at 1000-1100 deg.c, and finish rolling. The plate has excellent mechanism performance and may be used widely in medical electronics, nuclear industry, chemical metallurgy and other industries.
Description
Technical field:
A kind of preparation method of tungsten base high specific gravity alloy board relates to the method that a kind of employing powder metallurgy and hot plastic processing method are produced high-precision tungsten base high-specific-gravity alloy (W-Ni-Fe) plate.
Technical background
At present, a large amount of tungsten base high specific gravity alloy board of demand aspect aviation device, radiation shield, ray baffle plate and chemical industry is because the restriction of production method makes its manufacturing cost than higher.Domestic and international production technology generally is divided into the rolling rolling vacuum heat method that adds of liquid-phase sintering, the cutting of sintered blank stockline and multi-pass that adds of powder smelting and produces.The sheet material that preceding two kinds of methods are produced is subjected to the restriction of specification, and its center line patterning method production cost is than higher, and the plate property deficiency of producing also is a problem, and all can not large-scale production; The third method is to adopt the powder metallurgy base to add follow-up thermoplasticity processing sheet material, because the material self character easily cracks, and repeatedly cycle heat treatment and little pass reduction are produced, yield rate is low like this, cost is high in the operation of rolling.
Summary of the invention
Purpose of the present invention is exactly in order to overcome the deficiency that above-mentioned prior art exists, and the preparation method of a kind of yield rate height, tungsten base high specific gravity alloy board material that cost of manufacture is low is provided.
The objective of the invention is to be achieved through the following technical solutions.
A kind of preparation method of tungsten base high specific gravity alloy board is characterized in that its preparation process is followed successively by:
A. with Fsss Fei Shi particle mean size batch mixing pressed compact in the cobalt Co powder of the tungsten W powder of 2.8～3.2 μ m and nickel powder, iron Fe powder, trace and yttrium Y powder batch mixer;
B. with blank under hydrogen protection, the sintering furnace inherence is warming up to 1490 ℃-1500 ℃ insulations with 15 ℃/min speed and made slab in 2 hours;
C. use corrosion resistant plate as sheath material the slab that makes, carry out pack rolling, rolling temperature is 700 ℃～900 ℃, and the working modulus of first passage is 25%～30% during cogging, every time working modulus is 18%～23% subsequently, and it is 6 * 10 in vacuum that total working modulus reaches at 45%～50% o'clock
-3Pa, temperature is under 1000 ℃～1250 ℃ conditions, insulation 1～2h carries out vacuum heat and eliminates stress; Be chosen in 700～900 ℃ subsequently and be rolled, every time working modulus reaches between 20%～25%, and total working modulus reaches at 70%～80% o'clock and can obtain good middle sheet material; Adopt 1000 ℃～1100 ℃ annealing temperatures again, carry out finally rolling.
Method of the present invention is characterized in that the nickel powder, the iron Fe powder that adopt are the carbonyl dust that adopts respectively in GJB1078, the GJB1081 standard.
Method of the present invention, the steel ball that adopts when it is characterized in that mixing powder and raw material weight were than for by 5: 2～5: 1, and mixing time is 12 hours, and drum rotation speed is 40～60r/min, and rested 20min at 6 hours.
Method of the present invention is characterized in that carrying out alkali cleaning before the vacuum heat, and the alkali lye proportioning is 85%NaOH+15%KNO
3, alkali liquid temperature: 380～500 ℃, the alkali cleaning time: 2～10 minutes, the alkali cleaning time arrived below the back temperature drop to 100 ℃, and water is rinsed well.
It is 1.2～1.7mm that method of the present invention adopts the cylindrical steel plate thickness, and rolling back is with the pickling jacket that comes off automatically.
Method of the present invention adopts high-quality W, Ni, Fe powder, and adds powder such as micro-Co and Y, rationally controls Ni: the Fe ratio, and through special batch mixing and sintering process acquisition high-quality slab.The adding of Co and Y powder makes the W-W intercrystalline in the alloy have less dihedral angle and good wetability, helps improving the thermoplasticity of material, does not change density and other physical property of material simultaneously.Select pack rolling in the operation of rolling, the working modulus of first passage and every time working modulus are subsequently answered control rate during the control cogging, and reach at 45%～50% o'clock in total working modulus and adopt vacuum heat to eliminate stress, be rolled again and obtain good middle sheet material, annealing again, carry out final rolling after, the sheet material of acquisition has very good mechanical properties, can be widely used in the W-Ni-Fe sheet material of industries such as medical electronics, nuclear military project, chemical metallurgy, machining.Method of the present invention, production procedure is few, is suitable for mass production W-Ni-Fe sheet material.
The specific embodiment
A kind of preparation method of tungsten base high specific gravity alloy board is characterized in that its preparation process is followed successively by: a. is with Fsss Fei Shi particle mean size batch mixing pressed compact in the cobalt Co powder of the tungsten W powder of 2.8～3.2 μ m and nickel powder, iron Fe powder, trace and yttrium Y powder batch mixer; B. with blank under hydrogen protection, the sintering furnace inherence is warming up to 1490 ℃-1500 ℃ insulations with 15 ℃/min speed and made slab in 2 hours; C. use corrosion resistant plate as sheath material the slab that makes, carry out pack rolling, rolling temperature is 700 ℃～900 ℃, and the working modulus of first passage is 25%～30% during cogging, every time working modulus is 18%～23% subsequently, and it is 6 * 10 in vacuum that total working modulus reaches at 45%～50% o'clock
-3Pa, temperature is under 1000 ℃～1250 ℃ conditions, insulation 1 ~ 2h carries out vacuum heat and eliminates stress; Be chosen in 700～900 ℃ subsequently and be rolled, every time working modulus reaches between 20%～25%, and total working modulus reaches at 70%～80% o'clock and can obtain good middle sheet material; Adopt 1000～1100 ℃ of annealing temperatures again, carry out final rolling after, the total working modulus of sheet material can reach 90%～98.8%.
In order to produce the high-quality ingot blank, the present invention at first sets about from raw material, material powder adopts GJB, and tungsten powder Fsss (Fei Shi particle mean size) is strict controlled in nickel (Ni) powder between 2.8～3.2 μ m, iron (Fe) powder adopts the carbonyl dust in GJB1078, the GJB1081 standard respectively; Adopt steel ball and raw material to press 5: 2～5: 1 proportionings when mixing powder, carry out batch mixing in the drum-type batch mixer, mixing time was 12 hours, and drum rotation speed is 40～60r/min, and rested 20min at 6 hours.After adopting liquid-phase sintering blank is carried out the stainless steel pack rolling, in the rolling mill practice, adopt during cogging between first pass reduction 25%～30%, and eliminate the materials processing sclerosis, be beneficial to follow-up rolling acquisition high-performance sheet material by vacuum heat.Must carry out alkali cleaning, alkali lye proportioning: 85%NaOH+15%KNO to material before the vacuum heat
3, alkali liquid temperature: 380 ℃～500 ℃ alkali cleaning times: 2～10 minutes, should be slowly after the alkali cleaning material frame be proposed from alkali lye, empty dried alkali lye is placed on below the first-class material of the material platform temperature drop to 100 ℃ then, and water is rinsed well.After rolling, need not reject jacket, directly roll and be thinned to the following soda acid of 10.0mm and wash the back and just come off automatically.
Through the continuous rolling application of vacuum that adds, when total deformation reached 85%, follow-up processing can directly be rolled down to 0.1～0.3mm without application of vacuum.When the following finished product of 0.5mm is rolling, can adopts the cold rolling surface quality that improves sheet material, and select for use rational final pass deflection can control template.
Embodiment 1
With cobalt Co powder and the yttrium Y powder of Fsss Fei Shi particle mean size at the tungsten W powder of 2.8～3.2 μ m and nickel powder, iron Fe powder, trace, in steel ball and raw material weight ratio are 5: 2 batch mixer, mixing time was 12 hours, and drum rotation speed is 40r/min, and rested 20min at 6 hours.Pressed compact, under the hydrogen protection, the sintering furnace inherence is warming up to 1490 ℃ of insulations with 15 ℃/min speed and made slab in 2 hours with blank; With the slab thickness that makes be the 1.2mm corrosion resistant plate as sheath material, carry out pack rolling, rolling temperature is 700 ℃, the working modulus of first passage is 25% during cogging, and every time working modulus is 18%% subsequently, and total working modulus reaches at 45% o'clock, carry out alkali cleaning, the alkali lye proportioning is 85%NaOH+15%KNO
3, alkali liquid temperature: 380 ℃, alkali cleaning 10 minutes, the alkali cleaning time arrives below the back temperature drop to 100 ℃, and water is rinsed well.Be 6 * 10 in vacuum again
-3Pa, temperature is under 1000 ℃ of conditions, insulation 2h carries out vacuum heat and eliminates stress; Be chosen in 700 ℃ subsequently and be rolled, every time working modulus reaches between 20%, and total working modulus reaches at 70% o'clock and can obtain good middle sheet material; Adopt 1000 ℃ of annealing temperatures again, carry out finally rolling.Rolling back is with the pickling jacket that comes off automatically.
Embodiment 2
With cobalt Co powder and the yttrium Y powder batching of Fsss Fei Shi particle mean size at the tungsten W powder of 2.8～3.2 μ m and nickel powder, iron Fe powder, trace, in steel ball and raw material weight ratio are 5: 1 batch mixer, mixing time was 12 hours, and drum rotation speed is 60r/min, and rested 20min at 6 hours.Pressed compact, under the hydrogen protection, the sintering furnace inherence is warming up to 1500 ℃ of insulations with 15 ℃/min speed and made slab in 2 hours with blank; C. with the slab thickness that makes be the 1.7mm corrosion resistant plate as sheath material, carry out pack rolling, rolling temperature is 900 ℃, the working modulus of first passage is 30% during cogging, and every time working modulus is 23% subsequently, and total working modulus reaches at 50% o'clock, carry out alkali cleaning, the alkali lye proportioning is 85%NaOH+15%KNO
3, alkali liquid temperature: 500 ℃, the alkali cleaning time: 2 minutes, below the temperature drop to 90 ℃, water was rinsed well after the alkali cleaning.Be 6 * 10 in vacuum again
-3Pa, temperature is under 1250 ℃ of conditions, is incubated 1 hour and carries out vacuum heat to eliminate stress; Be chosen in 900 ℃ subsequently and be rolled, every time working modulus reaches between 25%, and total working modulus reaches at 80% o'clock and can obtain good middle sheet material; Adopt 1000 ℃ of annealing temperatures again, carry out finally rolling.Rolling back is with the pickling jacket that comes off automatically.
Embodiment 3
With cobalt Co powder and the yttrium Y powder batching of Fsss Fei Shi particle mean size at the tungsten W powder of 2.8～3.2 μ m and nickel powder, iron Fe powder, trace, in steel ball and raw material weight ratio are 5: 2 batch mixer, mixing time was 12 hours, and drum rotation speed is 50r/min, and rested 20min at 6 hours.Pressed compact, under the hydrogen protection, the sintering furnace inherence is warming up to 1495 ℃ of insulations with 15 ℃/min speed and made slab in 2 hours with blank; C. with the slab thickness that makes be the 1.5mm corrosion resistant plate as sheath material, carry out pack rolling, rolling temperature is 800 ℃, the working modulus of first passage is 28% during cogging, and every time working modulus is 20% subsequently, and total working modulus reaches at 48% o'clock, carry out alkali cleaning, the alkali lye proportioning is 85%NaOH+15%KNO
3, alkali liquid temperature: 450 ℃, alkali cleaning 7 minutes, the alkali cleaning time arrives below the back temperature drop to 80 ℃, and water is rinsed well.Be 6 * 10 in vacuum again
-3Pa, temperature is under 1100 ℃ of conditions, insulation 1.5h carries out vacuum heat and eliminates stress; Be chosen in 850 ℃ subsequently and be rolled, every time working modulus reaches between 23%, and total working modulus reaches at 75% o'clock and can obtain good middle sheet material; Adopt 1050 ℃ of annealing temperatures again, carry out finally rolling.Rolling back is with the pickling jacket that comes off automatically.
Claims (5)
1. the preparation method of a tungsten base high specific gravity alloy board is characterized in that its preparation process is followed successively by:
A. with Fsss Fei Shi particle mean size batch mixing pressed compact in the cobalt Co powder of the tungsten W powder of 2.8～3.2 μ m and nickel powder, iron Fe powder, trace and yttrium Y powder batch mixer;
B. with blank under hydrogen protection, the sintering furnace inherence is warming up to 1490 ℃-1500 ℃ insulations with 15 ℃/min speed and made slab in 2 hours;
C. use corrosion resistant plate as sheath material the slab that makes, carry out pack rolling, rolling temperature is 700 ℃～900 ℃, and the working modulus of first passage is 25%～30% during cogging, every time working modulus is 18%～23% subsequently, and it is 6 * 10 in vacuum that total working modulus reaches at 45%～50% o'clock
-3Pa, temperature is under 1000 ℃～1250 ℃ conditions, insulation 1～2h carries out vacuum heat and eliminates stress; Be chosen in 700～900 ℃ subsequently and be rolled, every time working modulus reaches between 20%～25%, and total working modulus reaches at 70%～80% o'clock and can obtain good middle sheet material; Adopt 1000 ℃～1100 ℃ annealing temperatures again, carry out final rolling after.
2. the preparation method of a kind of tungsten base high specific gravity alloy board according to claim 1 is characterized in that the nickel powder, the iron Fe powder that adopt are the carbonyl dust that adopts respectively in GJB1078, the GJB1081 standard.
3. the preparation method of a kind of tungsten base high specific gravity alloy board according to claim 1 method of the present invention, the steel ball that adopts when it is characterized in that mixing powder is by 5: 2～5: 1 with the raw material weight ratio, mixing time was 12 hours, and drum rotation speed is 40～60r/min, and rested 20min at 6 hours.
4. the preparation method of a kind of tungsten base high specific gravity alloy board according to claim 1 method of the present invention is characterized in that carrying out alkali cleaning before the vacuum heat, and the alkali lye proportioning is 85%NaOH+15%KNO
3, alkali liquid temperature: 380～500 ℃, the alkali cleaning time: 2～10 minutes, the alkali cleaning time arrived below the back temperature drop to 100 ℃, and water is rinsed well.
5. to adopt the cylindrical steel plate thickness be 1.2～1.7mm to the preparation method of a kind of tungsten base high specific gravity alloy board according to claim 1 method of the present invention, and rolling back is with the pickling jacket that comes off automatically.
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| CN 200410103516 CN1290635C (en) | 2004-12-30 | 2004-12-30 | Method for preparing tungsten base high specific gravity alloy board |
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| CN 200410103516 CN1290635C (en) | 2004-12-30 | 2004-12-30 | Method for preparing tungsten base high specific gravity alloy board |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102380614A (en) * | 2011-11-11 | 2012-03-21 | 西安瑞福莱钨钼有限公司 | Method for preparing tungsten-nickel-iron alloy thin plate |
| CN102383016A (en) * | 2011-11-02 | 2012-03-21 | 中南大学 | Microwave sintering and heat treatment method for preparing high-performance tungsten-based high-density alloy |
| CN102517426A (en) * | 2011-12-21 | 2012-06-27 | 贵州航天控制技术有限公司 | Heat treatment method of high specific gravity alloy |
-
2004
- 2004-12-30 CN CN 200410103516 patent/CN1290635C/en active Active
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102383016A (en) * | 2011-11-02 | 2012-03-21 | 中南大学 | Microwave sintering and heat treatment method for preparing high-performance tungsten-based high-density alloy |
| CN102383016B (en) * | 2011-11-02 | 2013-04-24 | 中南大学 | Microwave sintering and heat treatment method for preparing high-performance tungsten-based high-density alloy |
| CN102380614A (en) * | 2011-11-11 | 2012-03-21 | 西安瑞福莱钨钼有限公司 | Method for preparing tungsten-nickel-iron alloy thin plate |
| CN102380614B (en) * | 2011-11-11 | 2013-06-12 | 西安瑞福莱钨钼有限公司 | Method for preparing tungsten-nickel-iron alloy thin plate |
| CN102517426A (en) * | 2011-12-21 | 2012-06-27 | 贵州航天控制技术有限公司 | Heat treatment method of high specific gravity alloy |
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| CN1290635C (en) | 2006-12-20 |
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Assignee: Xi'an Refra Tungsten & Molybdenum Co., Ltd. Assignor: Xibu Metal Material Co., Ltd. Contract record no.: 2011610000054 Denomination of invention: Method for preparing tungsten base high specific gravity alloy board Granted publication date: 20061220 License type: Exclusive License Open date: 20050601 Record date: 20110629 |