CN1442254A - Spray casting-suction casting method and equipment for preparing large non crystal alloy - Google Patents

Spray casting-suction casting method and equipment for preparing large non crystal alloy Download PDF

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Publication number
CN1442254A
CN1442254A CN 03121418 CN03121418A CN1442254A CN 1442254 A CN1442254 A CN 1442254A CN 03121418 CN03121418 CN 03121418 CN 03121418 A CN03121418 A CN 03121418A CN 1442254 A CN1442254 A CN 1442254A
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chamber
vacuum
mould
furnace chamber
valve
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惠希东
寇宏超
陈俊
崔新发
陈国良
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University of Science and Technology Beijing USTB
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University of Science and Technology Beijing USTB
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Abstract

A spray casting-suction casing apparatus for preparing great non-crystal alloy block is composed of upper and lower furnace chambers, water-cooled partition between said chambers, heating body consisting of one Mo sheet layer and 6 reflecting screen layers, mould made of quartz glass or graphite arranged in said heating body and passing through said partition, U-shaped seals, plug pulling unit for the quartz glass (or graphit) plug of the circular hole on the bottom of mould, and water-cooled copper mould made of red copper.

Description

A kind of spray to cast-suction casting method and equipment for preparing bulk amorphous alloys
Technical field:
The invention belongs to the spray to cast-suction casting technical field of bulk amorphous alloys, a kind of vacuum spray to cast-suction casting preparation method and relevant device thereof of bulk amorphous alloys particularly is provided.
Background technology:
Block non-crystalline alloy material is a class advanced material that develops rapidly nineteen nineties.Compare with traditional crystal alloy material, bulk amorphous alloys has the ability of more excellent mechanical property, anti-multiple dielectric corrosion, good soft magnetism, hard magnetic property and unique physicalies such as expansion characteristics, and this makes bulk amorphous alloys have very tempting application prospect.The early 1990s, A.Inoue, T Zhang and T.Masumoto.Mater.Trans., JIM, 30 (1989), 965 and U.S. A.Peker and W.L.Johnson, Appl.Phys.Lett., 63 (1993), 2342 by design of alloy, has broken through desired high speed cooling (＞10 in traditional non-crystaline amorphous metal preparation 6K/s) restriction, make the routine casting technology under the speed of cooling condition that can reach (10 1-10 -2K/s) can prepare block non-crystalline alloy material, thereby the epoch that the amorphous alloy that is through with mainly can only exist with low-dimensional forms such as powder, silk, strips make the research of amorphous alloy and application stride into a brand-new era.
Year is devoted to develop new bulk amorphous alloys system and preparation method surplus the bulk amorphous alloys nearly ten.Up to now, developed bulk amorphous alloys systems such as Zr base, Ln base, Ti base, Cu base, Fe base, Mg base and Pd base, the most representative alloy has: C.Fan, A.Takeuchi and A.Inoue.Mater.Trans., JIM, the Zr of 40 (1999), 42 preparations 60Al 10Cu 20Pd 10Bulk amorphous alloys; A.Leonhard, L.Q.Xing, M.Heilmaier and SchultzNanostructure Materials, the Zr of 10 (1998), 805 preparations 57Al 10Ni 8Cu 20Ti 5Bulk amorphous alloys; A.Pekerand W.L.Johnson Appl.Phys.Lett., the Zr of 63 (1993), 2342 preparations 40Ti 14Ni 11Cu 10Be 25Bulk amorphous alloys.
Exploring new Peparation of Bulk Amorphous Solid method also is one of its developing direction.It is several that the large block amorphous method of current preparation mainly contains pressure model casting, atomizing amorphous powder extrusion process, directional solidification method, water quenching and vacuum suction casting technique etc.A.Inoue.Mater.Trans. for example, JIM, 36 (1995), 866 utilize the pressure model casting to prepare the Mg-Ln-TM amorphous of block, Ln-Al-TM amorphous and Zr base block amorphous alloy etc.The ultimate principle of this method is: by high-frequency induction heating fusing, piston certain speed and pressure under hydraulic action moves forward mother alloy, and molten metal is squeezed in the copper mold under the protection of argon gas, relies on strong water-cooled and forms bulk amorphous.A.Inoue, Zhang Tao, US5740854 have proposed arc melting and have added the method for inhaling casting and prepare bulk amorphous alloy, and its basic functional principle is: the method fusing mother alloy that at first utilizes arc melting, copper mold divides two chambeies up and down, and the copper mold cavity of resorption is in the vacuum state of sealing.After the mother alloy fusing, open the baffle plate between copper mold up and down, in the water cooled copper mould below liquid alloy is inhaled under the pull of vacuum effect, the strong cold-working that relies on water cooled copper mould is with preparing bulk amorphous alloy, the shortcoming of this equipment is that copper mold is made complexity, both consider the shape of sample, considered the vacuum-sealing problem of copper mold again.
Summary of the invention:
Purpose of the present invention proposes the preparation method that the bulk amorphous alloys that combines is cast in a kind of new spray to cast-suction, design the two chambers spray to cast-suction casting machine that to control melt temperature of the new suitable preparation large size amorphous alloy material of a cover, and utilize this equipment to prepare large size non-crystaline amorphous metal exemplar.
The present invention combines the melt spray to cast with inhaling the casting technology, provide employing melt temperature control technique to add double-chamber vacuum spray to cast-suction casting technology and prepared the method and apparatus of large size non-crystaline amorphous metal, vacuum spray to cast-suction casting machine schematic diagram such as accompanying drawing 1.Equipment mainly is made of following part: mechanical pump 1, lobe pump 2, molecular pump 3, valve 4, bell 5, bell locking mechanism 6, last furnace chamber 7, molybdenum sheet heating element 8, thermopair 9, conducting copper 10, supply transformer 11, following chamber fire door 12, following furnace chamber 13, water cooled copper mould 14, graphite cannula 15, radiation screen 16, plumbago crucible 17, the bar 18 of drawing the cork.
The inventive point of this equipment is: this equipment is made up of last furnace chamber 7 and 13 two furnace chambers of following furnace chamber, and last furnace chamber is separated by one deck cooled plate with following furnace chamber, and last furnace chamber keeps 5 * 10 in heat-processed -3～5 * 10 -4The Pa negative pressure state then becomes the barotropic state of 1atm during spray to cast.Following furnace chamber is in 5 * 10 all the time -3～5 * 10 -4The negative pressure state of Pa.Heating element 6 is made up of 1 layer of molybdenum sheet and 6 layers of radiation shield, and Heating temperature can reach 1600 ℃, and can be incubated 120 hours under this temperature.Mould 17 is placed in the heating element, adopting quartz glass or graphite manufacturing, the outside dimension of mould is 10～50mm, highly be 200～500mm, mould passes waterbaffle, adopts the sealing of U-shaped circle at the waterbaffle place, and the bottom design of mould has the circular hole of diameter 2～10mm, this hole is blocked with silica glass or graphite plug during molten alloy, and the filling chamber utilizes the mechanism 18 of drawing the cork that plug is gone out.Water cooled copper mould 14 adopts the red copper manufacturing, and structure is a built-up type, and garden shape diameter of bore is 2～30mm, and tabular inner cavity size is 1mm * 5mm * 10mm～10mm * 50mm * 100mm, and heat-eliminating medium is 5～30 ℃ a water.
Processing method of the present invention is: at first in electric arc furnace with bulk amorphous alloys element Zr; Ti; Cu; Al; Be; Nb; Ta; W; Fe; Co; Ni; C; P; B; 4～7 kinds of elements among the Pd are in following ratio (atomic percent) Zr:40～80% of preparing burden; Ti:5～10%; Cu:5～50%; Al:3～20%; Be:5～25%; Nb:2～15%; Ta:1～10%; W:1～10%; Co:1～10%; Ni:5～50%; C:1～10%; P:5～20%; B:1～10%; Pd:5～60%, molten joining adopted the high-purity argon gas protection in the process.Pack into mother alloy in the plumbago crucible 17 and be placed in the furnace chamber 7, lock 6 and 12.Order is driven mechanical pump 1 and lobe pump 2, to 1 * 10 -2Open molecular pump 3 after the Pa vacuum tightness again, valve-off 4-1 opens valve 4-3 simultaneously, takes out upper and lower furnace chamber vacuum to condition of high vacuum degree 5 * 10 -3～5 * 10 -4Pa;
Switch power supply, according to setting program heating mother alloy, utilize thermopair to carry out thermometric and temperature control simultaneously, heating makes mother alloy fusing and overheated 100～200 ℃ to 900～1200 ℃ rapidly to 800～1000 ℃ of temperature, closing valve 4-4 makes down vacuum chamber 13 continue pumping high vacuum to 5 * 10 -3～5 * 10 -4Pa, opening valve 4-5, to charge into 1 atmospheric purity for last vacuum chamber 7 be 99.8% argon gas, utilize the mechanism that draws the cork to mention the bar 18 of drawing the cork simultaneously, melt is owing to be subjected to the effect of vacuum chamber pressure reduction up and down, fill type fast and enter water cooled copper mould 14, powered-down is simultaneously opened valve 4-4 and is continued vacuum chamber is up and down vacuumized; When furnace temperature is reduced to below 80～100 ℃, stop to vacuumize, open purging valve and make the air admission vacuum chamber, open down vacuum chamber fire door 12 and take out sample.
The invention has the advantages that;
1, the present invention combines the melt spray to cast with inhaling the casting technology, has realized the high speed filling and fine and close shaping of melt;
2, adopt the melt temperature control technique, can control fusing, temperature of superheat, the overheated time of mother alloy, help control
System influences all multifactor of amorphous formation ability;
3, the invention enables whole technological process all under high vacuum environment, to carry out, adopt plumbago crucible, reduced melt
Oxidation and the pollution of crucible material, thereby just can make the bulk amorphous alloys material with the material of ordinary purity
Material greatly reduces manufacturing cost;
4, because the increase of vacuum chamber, so be particularly suitable for the preparation of large-size bulk amorphous alloy material.
Description of drawings:
Fig. 1 is double-chamber vacuum spray to cast of the present invention-suction casting machine synoptic diagram, and wherein mechanical pump 1, lobe pump 2, molecular pump 3, valve 4, bell 5, bell locking mechanism 6, last furnace chamber 7, molybdenum sheet heating element 8, thermopair 9, conducting copper 10, supply transformer 11, following chamber fire door 12, following furnace chamber 13, water cooled copper mould 14, graphite cannula 15, radiation screen 16, plumbago crucible 17, the bar 18 of drawing the cork.
Fig. 2 is the Zr of the various size of the present invention's preparation 40Ti 14Ni 11Cu 10Be 25The bulk amorphous alloys bar.
Fig. 3 is Zr 40Ti 14Ni 11Cu 10Be 25The X-ray diffractogram of bulk amorphous alloys bar.
Fig. 4 is Zr 40Ti 14Ni 11Cu 10Be 25The TEM image of bulk amorphous alloys bar.
Embodiment:
Select highly purified 5 kinds of pure metal for use, i.e. Zr (99.99wt%), Ti (99.995wt%), Cu (99.95wt%), Ni (99.95wt%), Be (99.999wt%).With atomic percent be: Zr is 40, and Cu is 10, and Ni is 11, and Ti is 5, and Be is the allotment of 25 ratio, is under 99.8% the argon shield in purity, uses the purification technique of liquid mother alloy, utilizes arc melting method and makes mother alloy.In order to ensure the homogeneity of each constituent element in the mother alloy, mother alloy is by remelting three times.The surface of mother alloy spindle is polished away surperficial oxide skin by mechanical grinding, is crushed to fritter then and uses the alcohol wash surface.The broken plumbago crucible of putting into of these mother alloy fritters utilizes device as shown in Figure 1, and principle of work is prepared Zr as shown in Figure 2 as described above 40Ti 14Ni 11Cu 10Be 25Bar.Utilize the X-ray diffractometer check, this bar diffraction spectra has only a roomy diffraction peak as shown in Figure 3 on the curve, and therefore not tangible the and corresponding diffraction peak existence of crystallization phases can confirm that this bar is an amorphous alloy.
Utilize the microtexture of transmission electron microscope (TEM) observation sample.The TEM sample prepares with ion milling, and preparation temperature is 250K.The TEM image of this bar can see that as shown in Figure 4 organizing almost completely of showing in the image is made up of single amorphous phase, and is on all four on this and the X-ray diffraction spectrum result.

Claims (2)

1, a kind of vacuum spray to cast-suction casting method for preparing bulk amorphous alloys, it is characterized in that: at first in electric arc furnace with bulk amorphous alloys element Zr, Ti, Cu, Al, Be, Nb, Ta, W, Fe, Co, Ni, C, P, B, 4～7 kinds of elements among the Pd are by following atomic percent batching Zr:40～80%, Ti:5～10%, Cu:5～50%, Al:3～20%, Be:5～25%, Nb:2～15%, Ta:1～10%, W:1～10%, Co:1～10%, Ni:5～50%, C:1～10%, P:5～20%, B:1～10%, Pd:5～60%, molten joining adopted the high-purity argon gas protection in the process, pack into mother alloy in the plumbago crucible (17) and be placed in the furnace chamber (7), lock bell locking mechanism (6) and following chamber fire door (12); Order is driven mechanical pump (1) and lobe pump (2), to 1 * 10 -2Open molecular pump (3) after the Pa vacuum tightness again, valve-off (4-1) is opened valve (4-3) simultaneously, takes out upper and lower furnace chamber vacuum to condition of high vacuum degree 5 * 10 -3～5 * 10 -4Pa; Switch power supply, according to setting program heating mother alloy, utilize thermopair (9) to carry out thermometric and temperature control simultaneously, it is also overheated 100～200 ℃ to 900～1200 ℃ to 800～1000 ℃ of temperature post-heating mother alloy to be melted, closing valve (4-4) makes down vacuum chamber (13) continue pumping high vacuum to 5 * 10 -3～5 * 10 -4Pa, opening valve (4-5), to charge into 1 atmospheric purity for last vacuum chamber (7) be 99.8% argon gas, utilize the mechanism that draws the cork to mention the bar of drawing the cork (18) simultaneously, melt is owing to be subjected to the effect of vacuum chamber pressure reduction up and down, fill type fast and enter water cooled copper mould (14), powered-down is simultaneously opened valve (4-4) and is continued vacuum chamber is up and down vacuumized; When furnace temperature is reduced to 80-100 ℃, stop to vacuumize, open purging valve and make the air admission vacuum chamber, open down vacuum chamber fire door (12) and take out sample.
2, a kind of equipment according to the described preparation bulk amorphous alloys of claim 1 vacuum spray to cast-suction casting, by (1) mechanical pump, (2) lobe pump, (3) molecular pump, (4) valve, (5) bell, (6) bell locking mechanism, (7) go up furnace chamber, (8) molybdenum sheet heating element, (9) thermopair, (10) conducting copper, (11) supply transformer, (12) are the chamber fire door down, (13) furnace chamber under, (14) water cooled copper mould, (15) graphite cannula, (16) radiation screen, (17) plumbago crucible, (18) bar of drawing the cork is formed; It is characterized in that: this equipment is made up of last furnace chamber (7) and (13) two furnace chambers of following furnace chamber, and last furnace chamber is separated by one deck cooled plate with following furnace chamber, and last furnace chamber keeps 5 * 10 in heat-processed -3～5 * 10 -4The Pa negative pressure state then becomes the barotropic state of 1atm during spray to cast, following furnace chamber is in 5 * 10 all the time -3～5 * 10 -4The negative pressure state of Pa, heating element (6) is made up of 1 layer of molybdenum sheet and 6 layers of radiation shield; Mould (17) is placed in the heating element, adopting quartz glass or graphite manufacturing, the outside dimension of mould is 10～50mm, highly be 200～500mm, mould passes waterbaffle, adopts the sealing of U-shaped circle at the waterbaffle place, and the bottom design of mould has the circular hole of diameter 2～10mm, this hole is blocked with silica glass or graphite plug during molten alloy, and the filling chamber utilizes the mechanism (18) that draws the cork that plug is gone out; Water cooled copper mould (14) adopts the red copper manufacturing, and structure is a built-up type, and garden shape diameter of bore is 2～30mm, and tabular inner cavity size is 1mm * 5mm * 10mm～10mm * 50mm * 100mm.
CN 03121418 2003-03-28 2003-03-28 Spray casting-suction casting method and equipment for preparing large non crystal alloy Pending CN1442254A (en)

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Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1304620C (en) * 2005-08-17 2007-03-14 北京科技大学 Method for jet deposition formation to preparing lanthanum matrix massive amorphous alloy
CN100366781C (en) * 2005-02-05 2008-02-06 中国科学院物理研究所 Erbium-base lorge-cube non-crystal alloy and making method
CN100457328C (en) * 2006-08-09 2009-02-04 中国科学院金属研究所 Method for semi-continuously preparing TiAl base alloy automobile air valve and components with similar shape
CN102358933A (en) * 2011-09-28 2012-02-22 清华大学 Ti-based block amorphous alloy with great amorphous forming ability and preparation method thereof
CN101644537B (en) * 2009-09-03 2012-07-18 张保国 Double-chamber vacuum oriented smelting furnace and use method thereof
CN103170605A (en) * 2013-03-14 2013-06-26 华中科技大学 Preparation method and preparation device of amorphous alloy fine part based on vacuum suction casting
CN103834822A (en) * 2014-02-28 2014-06-04 西北工业大学 Smelting and casting method and casting device of titanium-based amorphous composite material
CN105478727A (en) * 2015-12-28 2016-04-13 北京科技大学 Mold for preparing amorphous ring and process thereof
CN105903931A (en) * 2016-05-04 2016-08-31 上海大学 High-flux preparation device and method for array type bulk amorphous alloys
CN106424662A (en) * 2016-11-25 2017-02-22 西北有色金属研究院 Equipment and method of preparing cobalt-based alloy welding wire through counter-gravity vacuum suction casting
CN111842845A (en) * 2020-07-31 2020-10-30 吉林大学 Multifunctional special casting smelting furnace and application thereof
CN111922318A (en) * 2020-08-05 2020-11-13 兰州理工大学 Near-net forming die for zirconium-based amorphous flexible gear and preparation method thereof
CN112916832A (en) * 2021-01-25 2021-06-08 中国科学院金属研究所 Vacuum suction casting device and method for high-melting-point, high-activity and high-purity alloy
CN113774292A (en) * 2021-09-10 2021-12-10 中国工程物理研究院材料研究所 U-based amorphous alloy and preparation method and application thereof

Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100366781C (en) * 2005-02-05 2008-02-06 中国科学院物理研究所 Erbium-base lorge-cube non-crystal alloy and making method
CN1304620C (en) * 2005-08-17 2007-03-14 北京科技大学 Method for jet deposition formation to preparing lanthanum matrix massive amorphous alloy
CN100457328C (en) * 2006-08-09 2009-02-04 中国科学院金属研究所 Method for semi-continuously preparing TiAl base alloy automobile air valve and components with similar shape
CN101644537B (en) * 2009-09-03 2012-07-18 张保国 Double-chamber vacuum oriented smelting furnace and use method thereof
CN102358933A (en) * 2011-09-28 2012-02-22 清华大学 Ti-based block amorphous alloy with great amorphous forming ability and preparation method thereof
CN103170605B (en) * 2013-03-14 2015-12-09 华中科技大学 A kind of preparation method of the non-crystaline amorphous metal micro-workpiece based on suction pouring and device
CN103170605A (en) * 2013-03-14 2013-06-26 华中科技大学 Preparation method and preparation device of amorphous alloy fine part based on vacuum suction casting
CN103834822A (en) * 2014-02-28 2014-06-04 西北工业大学 Smelting and casting method and casting device of titanium-based amorphous composite material
CN103834822B (en) * 2014-02-28 2015-11-18 西北工业大学 Titanium-based amorphous matrix material melting and casting method and casting device
CN105478727A (en) * 2015-12-28 2016-04-13 北京科技大学 Mold for preparing amorphous ring and process thereof
CN105478727B (en) * 2015-12-28 2017-07-18 北京科技大学 A kind of mould and its technique for being used to prepare amorphous ring
CN105903931A (en) * 2016-05-04 2016-08-31 上海大学 High-flux preparation device and method for array type bulk amorphous alloys
CN106424662A (en) * 2016-11-25 2017-02-22 西北有色金属研究院 Equipment and method of preparing cobalt-based alloy welding wire through counter-gravity vacuum suction casting
CN111842845A (en) * 2020-07-31 2020-10-30 吉林大学 Multifunctional special casting smelting furnace and application thereof
CN111922318A (en) * 2020-08-05 2020-11-13 兰州理工大学 Near-net forming die for zirconium-based amorphous flexible gear and preparation method thereof
CN112916832A (en) * 2021-01-25 2021-06-08 中国科学院金属研究所 Vacuum suction casting device and method for high-melting-point, high-activity and high-purity alloy
CN113774292A (en) * 2021-09-10 2021-12-10 中国工程物理研究院材料研究所 U-based amorphous alloy and preparation method and application thereof

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