CN109967703A - A method of with a thickness of 80~1500 μm of wide cut amorphous thin ribbons, continuously big cooling rate is efficiently prepared - Google Patents
A method of with a thickness of 80~1500 μm of wide cut amorphous thin ribbons, continuously big cooling rate is efficiently prepared Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/06—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars
- B22D11/0622—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars formed by two casting wheels
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/06—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars
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- B22D11/0697—Accessories therefor for casting in a protected atmosphere
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- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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Abstract
The invention belongs to amorphous alloy preparation fields, and in particular to a method of use the double roller therapy wide cut amorphous thin ribbon that continuously big cooling rate is efficiently prepared with a thickness of 80~1500 μm.This method comprises the following steps: (1) smelting amorphous alloy by set component, its ingredient includes that zirconium base, copper-based, iron-based, Ni-based etc. form the method that amorphous metal of the limit cooling rate between 500~75000 DEG C/s designs its thin strip progressive forming, provides basic material for its post-processing procedure；(2) by forming the wide cut Cast Strip with a thickness of 80~1500 μm after strip casting process；(3) melting is carried out under inert atmosphere conditions, is shaped and is batched.For the problem that amorphous alloy preparation requires height to raw material and technology of preparing, there is not yet amorphous alloy Strip mass production, the present invention realizes 12m or more length, the amorphous band continuous casting and rolling process of 80~1500 μ m thicks.
Description
Technical field
The invention belongs to amorphous alloy preparation fields, and in particular to a kind of using double roller therapy, continuously big cooling rate efficiently prepares thickness
The method for the wide cut amorphous thin ribbon that degree is 80~1500 μm.
Background technique
Amorphous alloy, also referred to as glassy metal (Metallic Glass) or glassy alloy (Glassy Alloy) are applications
The alloy that one kind that modern quickly solidification metallurgical technology prepares is novel, special, state of matter is clearly distinguishable from crystalline state
Material.Since the unique atomic structural arrangement of amorphous alloy and metallic bond form, there is amorphous alloy compared to traditional crystalline state
The more excellent mechanical property of metal material, physical property and chemical property.This makes amorphous alloy in aerospace, weapons work
Industry, precision instrument, biologic medical and power Transmission etc. are with a wide range of applications.
The preparation of early stage amorphous alloy needs very big cooling velocity (> 106K/s), at that time amorphous alloy can only with powder,
The forms such as silk, strip exist, and greatly weaken the performance of amorphous alloy performance potential, limitation amorphous alloy answering in the industry
With.Therefore, since last century late nineteen eighties, the Forming ability of amorphous alloy how is improved, large-sized amorphous is prepared and closes
Gold becomes one of focus on research direction in new material research field.In the decades of the 1980s so far, by a large amount of
The effort of scholar, having developed Zr base, Ti base, Fe base, Co base, Ni base, Cu base, Pt base etc. largely there is big glass to be formed
The alloy system of ability；Develop a variety of bulk amorphous alloy such as water quenching, copper mold casting method, directional solidification method, amorphous powder extrusion
The technology of preparing of alloy.Wherein, had at home using the amorphous thin ribbon with excellent soft magnet performance that single-roller method produces
On a large scale, it is widely applied, makes outstanding contributions for the energy-saving and emission-reduction of China's electric system.Moreover, the system of block amorphous alloy
It is standby to be produced as structural material because of its excellent mechanical property with the same acquirement significant progress of application and be applied to electricity
Sub- product, sports equipment, auto parts etc..Currently, the most important production method of block amorphous alloy product applied in the market
It is casting die, since its own condition limits, small dimension product can only be produced.And as strip widely used in structural material
Material, still without reliable production method.Therefore, how to realize continuous, a large amount of, the stable production of amorphous alloy Strip, push away
The extensive use of dynamic block amorphous alloy, is one of current amorphous industry urgent problem.
Currently, the main production process of amorphous strip includes that single roller melt supercooled method, double roller melt supercooled method and casting mold are drawn
Casting.It is most widely used at present, have been used for industrialized production is single roller melt supercooled method, abbreviation single-roller method.Single-roller method production
Fe-based amorphous band there is excellent soft magnet performance, can be instead of silicon steel, permalloy to make transformer core, and then significantly
Transformer efficiency is improved, reduces the iron loss of distribution transformer, while reducing volume and weight.However single-roller method production technology limits
The thickness (about 20~50 μm) and width (being less than 220mm) of band.Double roller melt supercooled method abbreviation double roller therapy.It is opened based on double roller therapy
The continuous cast method for sending out block amorphous alloy a variety of.United States Patent (USP) (publication number US2006/0260782A1) discloses a kind of bulk amorphous alloy
Sheet alloy continuously stays in device and method, and device uses multiple groups minor diameter chill roll cooled alloy band in patent, due to
It, which arranges roller, can only apply smaller contact pressure, and system cooling rate can only achieve less than 10 DEG C/s, and the plate thickness of preparation is 0.1~
10mm, and it is only limitted to the molding of the strong Zr base noncrystal alloy containing Be of Forming ability, it can also reduce amorphous service life and stability.With
Technical idea is closer to is Chinese patent (107755652 A of publication number CN), it is cooling using crawler type, it is continuous to cast
Amorphous is made, contact force is smaller, and cooling rate is limited, can equally reduce the amorphous service life and prepare the ingredient design redundancy of amorphous.In
State patent (publication number CN1486800A) discloses a kind of block amorphous alloy continuous casting rolling technology, and molten metal in crucible is melted
Body injects in the water cooling roll of two relative rotation, prepares bulk amorphous alloy plate, bar etc., but the patent using double roll castings
Have no concrete technology protection node and implementer's case, while to smelting temperature, Insulation, flow control measure, cooling rate, casting
The detail parameters such as power do not carry out disclosure yet.And Roll-gap position can apply relatively large roll-force, to realize larger cooling rate,
Theoretically its cooling capacity is greater than single-roller method, and can be the preparation biggish amorphous alloy Strip of thickness specification.Casting mold is drawn
Casting, be the master alloy after a kind of melting melted in crucible, keep the temperature after be cast in the pass of water cooling through stem bar, and by with
Certain speed is to molding amorphous alloy with pulling force, the method for realization amorphous alloy continuously casting.Chinese patent (publication number
CN101543885A the device and method for) disclosing a kind of block amorphous alloy horizontal continuous-casting, the cooling of alloy rely primarily on
The slab of water cooled copper mould, solidification pulls constantly output by the draw bar of motor drive.
Summary of the invention
Height is required to raw material and technology of preparing for amorphous alloy preparation, there is not yet amorphous alloy Strip mass production
Problem, using double roller therapy, continuously big cooling rate efficiently prepares the width with a thickness of 80~1500 μm the purpose of the present invention is to provide a kind of
The method of width amorphous thin ribbon realizes 12m or more length, the amorphous band continuous casting and rolling process of 80~1500 μ m thicks.
The technical scheme is that
A method of with a thickness of 80~1500 μm of wide cut amorphous thin ribbons, continuously big cooling rate is efficiently prepared, according to the following steps
It carries out:
(1) alloy blowing enters in crucible, and can preheat diversion pipe and its position control is cleared up, can be pre-
It is quartz material liner inside thermal conductivity flow tube, and is attached to heating system, heating temperature is subject alloy setting temperature or more 100
~200 DEG C, logical cooling water conservation outside diversion pipe can be preheated；
(2) set component smelting amorphous master alloys, ingredient are as follows: zirconium base, copper-based, iron-based or ni-based amorphous alloy ingredient are pressed
System uniformly mixes 5~30 minutes after metal melt, starts temperature control；
(3) control of the alloy melt degree of superheat is 50~300 DEG C, and 99.999% or more bulk purity is used during temperature control
High-purity argon gas protection, melting chamber argon gas inside are micro-positive pressure, i.e. pressure is not less than 0.11MPa；
(4) in fusion process, forming cavity preparation is completed, step includes: that a) all valve bodies close on the cavity of forming cavity
It closes, argon gas is filled with after vacuumizing, 99.99% or more bulk purity keeps the micro-positive pressure for being not less than 0.11MPa；B) cloth stem bar into
Row preheating, cloth stem bar use slit cloth stream, are fit into fixed bit and postpone and are heated, and heating temperature is that subject alloy solidifies
More than temperature 100~200 DEG C；C) casting roll cooling temperature of circulating water is 3~5 DEG C, and total water-flowing amount is 70~90m3/h；D) prepare casting
Gas system afterwards, 0.6~0.8MPa of argon pressure, gas temperature control 4~6 DEG C；
(5) alloy melting, can preheat diversion pipe and cloth stem bar preheating, forming cavity be filled with after the completion of argon gas, use is rectilinear
Thin-belt casting rolling technique carries out amorphous thin ribbon preparation, into strip casting process: opening melting chamber slide valve, can preheat under diversion pipe
Drop, is docked with cloth stem bar, and medium frequency induction melting furnace topples over alloy in can preheat in diversion pipe；Cloth stem bar is suprasil material,
It is monitored by infrared monitoring camera, controlling cloth stem bar inner melt height by the tipping speed of medium frequency induction melting furnace is 40
~60mm, by liquid level, by alloy melt, by cloth stem bar, vertically uniform cloth is flowed in casting roll roll gap, and alloy melt is in roll gap
Liquid level controls 2~10mm, and alloy melt cooling velocity is 500~75000 DEG C/s, the cooling casting forming of alloy；After forming
Amorphous thin ribbon is exported through guide roller, and is further cooled down into gas system after casting, is purged and is cooled down using low temperature argon gas, gas
50~800 DEG C/s of body cooling velocity；
(6) after gas cooling, amorphous thin ribbon thickness range reaches 80~1500 μm, 110~550mm of width range；80~
Band volume is collected by batching in 800 μ m thick specification Cast Strips, and the Cast Strip more than 800 μ m thicks is not batched, directly received with provided in very thin tape form
Collection.
The described wide cut amorphous thin ribbon method that continuously big cooling rate is efficiently prepared with a thickness of 80~1500 μm, strip casting process
In, alloy is conducted heat by casting roll to be quickly cooled down, thin to regulate and control alloy by control roll casting speed, casting-rolling force size and roll gap size
It takes roll temperature out of, and alloy is gone out into roll temperature control in the crystallization temperature Tx for being close to or smaller than alloy；Roll casting speed be 0.20~
1.8m/s, the casting-rolling force that the control of casting-rolling force size is every 1cm width Cast Strip are 2~15kN, and casting roll roll gap opening width is set as
80~1500 μm, and do not set side seal board.
The described wide cut amorphous thin ribbon method that continuously big cooling rate is efficiently prepared with a thickness of 80~1500 μm, passes through cloth stream
The opening size of mouth lower end, casting roll gap values between rollers, roll casting speed, copper casting roll, steel casting roll, the casting-rolling technology of casting roll cooling water inflow
State modulator solidification cooling reaches 500~75000 DEG C/s.
The described wide cut amorphous thin ribbon method that continuously big cooling rate is efficiently prepared with a thickness of 80~1500 μm, zirconium base, copper
The yttrium that mass percent is 0.0045~0.020 is added in base, iron-based or ni-based amorphous alloy, for removing band in environment
O, N pollution entered.
The described wide cut amorphous thin ribbon method that continuously big cooling rate is efficiently prepared with a thickness of 80~1500 μm, using quartz
Material slit cloth stem bar cloth stream, slit opening width is according to different product thickness design；Cloth stem bar is online preheating, preheating temperature
Degree is 100~200 DEG C of alloy graining temperature or more, and the open end of cloth stem bar lower end is thermally conductive by tungsten alloy piece, cloth stem bar
End region temperature reaches near alloy graining temperature, and dam is equipped with inside cloth stem bar and rushes in row current stabilization；Using diversion pipe can be preheated
Liner is Ke Kuaisugenghuan quartz glass, and preheating temperature is 100~200 DEG C of alloy graining temperature or more, can preheat diversion pipe
The logical cooling water conservation in outside.
The described wide cut amorphous thin ribbon method that continuously big cooling rate is efficiently prepared with a thickness of 80~1500 μm, cloth stem bar are wide
It spends side and infrared monitoring camera is set, feed back to rollover control system and achieve the purpose that cloth flow control；Wherein, cloth stem bar lower end
Extended distance casting roll roll gap Kiss line height control range be 10~50mm, cloth stem bar inside liquid level height be 40~60mm.
The described wide cut amorphous thin ribbon method that continuously big cooling rate is efficiently prepared with a thickness of 80~1500 μm, casting roll use
The double roller that level is oppositely arranged, double roller two sides install backing roll additional, and casting roll diameter is 280~420mm, every group of backing roll diameter design
Greater than casting roll diameter 100mm.
The described wide cut amorphous thin ribbon method that continuously big cooling rate is efficiently prepared with a thickness of 80~1500 μm, melting chamber with
Forming cavity is using classification vacuum design, in which: melting chamber working vacuum degree reaches 1 × 10-2Pa is hereinafter, forming cavity suction reaches
To 1Pa or less；When casting condition, environment is in argon gas guard mode, is separated between melting chamber and forming cavity by slide valve, casting
It is opened before rolling beginning full of slide valve after argon gas.
The described wide cut amorphous thin ribbon method that continuously big cooling rate is efficiently prepared with a thickness of 80~1500 μm, using intermediate frequency
Induction melting furnace+high purity graphite (phosphorus content >=99.99wt%) crucible carries out amorphous alloy melting, and heating temperature is no more than metal
More than melt temperature 400 DEG C, oxidation and metallic element scaling loss are prevented.
The described wide cut amorphous thin ribbon method that continuously big cooling rate is efficiently prepared with a thickness of 80~1500 μm, amorphous mother close
The Cast Strip trimming waste material for being no more than 20wt% is added in golden supplied materials.
Advantage and beneficial effect of the present invention are:
1, for block amorphous alloy progressive forming process, big cooling rate and good stability are essential.And
Mode is simple, and alloy pool is wider because it is cast for general casting and rolling installation, so that cooling rate of the alloy in shallow supercooling liquid phase region is smaller, it is difficult
To form amorphous alloy.The characteristics of present invention is solidified according to bulk amorphous alloy takes in conjunction with double-roller rolling technology and gos deep into roll gap casting
Method, alloy pool is narrow, cooling rate is big, deformation is small.Its principle, structures and methods are there is not yet open report.
2, the present invention can pass through cloth stem bar slit width, casting roll gap values between rollers, teeming speed, copper casting roll, steel casting roll, casting roll
The casting-milling technology parameters such as cooling water inflow control solidification cooling reaches 500~75000 DEG C/s.Limit cooling rate is formed for series
The method that amorphous metal between 500~75000 DEG C/s designs its thin strip progressive forming provides base for its post-processing procedure
Plinth material.
3, the present invention uses quartz material slit cloth stem bar cloth stream, and slit opening width is according to different product thickness design
0.15~0.8mm.Cloth stem bar be can station preheat online, preheating temperature be alloy graining temperature more than 100~200 DEG C, cloth stream
The end of mouth is thermally conductive by tungsten alloy piece, and end region temperature reaches near alloy graining temperature.It is rushed in inside cloth stem bar equipped with dam
Row current stabilization.
4, the present invention has infrared monitoring camera by cloth stem bar width profile, feeds back to rollover control system and reaches cloth stream
The purpose of control.The wherein extended distance casting roll roll gap Kiss line of cloth stem bar lower end (Kiss line refers to the immediate line of double work roller)
Height control range is 10~50mm, and cloth stem bar inside liquid level height is 40~60mm.Casting system is using flow-teeming speed matching
Control alloy melt roll gap vertically flows freely strategy, cancels the side seal board of strip casting process.
5, casting system of the present invention improves lateral stability control using the bearing roller mode for installing casting roll additional, reduces casting machine transmission
Side and fore side thickness deviation.Casting roll diameter is 280~420mm, and it is straight that every group of backing roll diameter design is greater than working roll (casting roll)
Diameter 100mm, roll surface roughness Ra≤10 μm.
6, for the present invention using the diversion Design with preheating, can preheat diversion pipe liner is Ke Kuaisugenghuan quartz glass,
Preheating temperature is 100~200 DEG C of alloy graining temperature or more, can preheat logical cooling water conservation outside diversion pipe.
7, melting chamber of the present invention and forming cavity are classified vacuum design, and wherein melting chamber working vacuum degree reaches 1 × 10-2Pa with
Under, forming cavity suction reaches 1Pa hereinafter, being quickly filled with argon gas.When casting condition, environment is in argon gas guard mode, melts
It is separated between refining chamber and forming cavity by slide valve, casting is opened before starting full of slide valve after argon gas.
8, gas system is cooled down using low temperature argon gas purging after present invention casting, and cooling velocity is 50~800 DEG C/s.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the wide cut amorphous thin ribbon of the present invention casting and rolling device that continuously big cooling rate is efficiently prepared.In figure,
1 medium frequency induction melting furnace；2 high vacuum melting chambers；3 can preheat diversion pipe；4 slide valves；5 cloth stem bars and infrared photography monitoring fill
It sets；51 cloth stem bars；52 infrared monitoring cameras；6 forming cavities；7 support rollers；8 casting rolls；Gas system after 9 castings；10 batch and set
It is standby；11 rollover control systems.
Fig. 2 is 0.55 millimeters thick amorphous band schematic diagram.
Fig. 3 is microstructure photo (a) and XRD curve graph (b).In figure, 2 θ of abscissa represents the angle of diffraction (drgee), indulges
Coordinate intensity represents relative intensity (a.u.).
Fig. 4 is microstructure photo (a) and XRD curve graph (b).In figure, 2 θ of abscissa represents the angle of diffraction (drgee), indulges
Coordinate intensity represents relative intensity (a.u.).
Specific embodiment
As shown in Figure 1, the wide cut amorphous thin ribbon casting and rolling device that continuously big cooling rate is efficiently prepared of the present invention, specifically include that
Frequency induction melting furnace 1, high vacuum melting chamber 2 (chamber pressure < 0.1Pa), can preheat diversion pipe 3, slide valve 4, cloth stem bar with it is red
Outer camera monitoring device 5, forming cavity 6, support roller 7, casting roll 8, casting after gas system 9, taking-up equipment 10, tumble control system
System 11 etc., specific structure is as follows:
The bottom opening of high vacuum melting chamber 2 is corresponding with the top opening of forming cavity 6, the bottom of high vacuum melting chamber 2
Opening is communicated by slide valve 4 with the top opening of forming cavity 6；Setting medium frequency induction melting furnace 1 in high vacuum melting chamber 2, can
Diversion pipe 3 and rollover control system 11 are preheated, the side that diversion pipe 3 is located at medium frequency induction melting furnace 1 can be preheated, it can pre- thermally induced flow
Pipe 3 is vertically arranged, and lower port is corresponding with 51 upper port of cloth stem bar of 6 inner top of forming cavity；Medium frequency induction melting furnace 1 is installed
In on rollover control system 11, medium frequency induction melting furnace 1 is rotated by shaft around rollover control system 11, makes Medium frequency induction melting
Furnace 1 it is suitable for reading with can preheat the suitable for reading corresponding of diversion pipe 3.
Cloth stem bar and infrared photography monitoring device 5 include 52 two parts of cloth stem bar 51 and infrared monitoring camera, cloth stem bar
51 inside are equipped with dam and rush in row current stabilization, and the wider one side of cloth stem bar 51 is equipped with infrared monitoring camera 52, passes through infrared prison
Control camera 52 feeds back to rollover control system 11 and achievees the purpose that cloth flow control.When melting obtains in medium frequency induction melting furnace 1
When amorphous master alloy melt, being poured into can be preheated in diversion pipe 3, can be preheated diversion pipe 3 and be moved down across medium frequency induction melting furnace 1
Bottom opening and slide valve 4, amorphous master alloy melt can be preheated diversion pipe 3 and be entered in cloth stem bar 51.
Roll gap between the lower port of cloth stem bar 51 and two casting rolls 8 is corresponding, and branch is respectively set in the outside of two casting rolls 8
Roller 7 is supportted, the alloy melt in diversion pipe 3 can be preheated and pass through the roll gap that the uniform cloth of cloth stem bar 51 flows between two casting rolls 8, alloy
Melt forms Cast Strip continuously across gas system 9 after the casting of 8 lower section of casting roll, and Cast Strip is coiled by taking-up equipment 10.
In the specific implementation process, the wide cut amorphous thin ribbon of the present invention method that continuously big cooling rate is efficiently prepared is as follows: (1) pressing
Set component smelts amorphous alloy, and ingredient includes that zirconium base, copper-based, iron-based, Ni-based etc. form limit cooling rate 500~75000
DEG C/s between the amorphous metal method that designs its thin strip progressive forming, provide basic material for its post-processing procedure；(2) lead to
The wide cut Cast Strip with a thickness of 80~1500 μm is formed after crossing strip casting process；(3) under inert atmosphere conditions carry out melting, at
Shape is simultaneously batched.
In the following, the present invention is further illustrated with reference to the drawings and specific embodiments.
Embodiment one
Alloying component: (Zr53.5Hf1.5Cu30Al10Ni5)99.9O0.1(atomic percent at.%, similarly hereinafter)；
Cloth stream mode: go deep into roll gap cloth stream；
Preparation flow:
A. match 20kg raw material by atomic percent, put into medium frequency induction melting furnace, and 6 are evacuated to melting chamber
×10-2Pa is heated to it to alloy raw material and is completely melt, and in 1500 DEG C of continuation melting 10min.
B. in fusion process, forming cavity preparation is completed, step includes: that 1) all valve bodies close on the cavity of forming cavity
Close, be evacuated to 0.5Pa, after be filled with argon gas, 99.99% or more bulk purity keeps the micro-positive pressure of 0.12MPa；2) cloth stem bar
It is preheated, cloth stem bar uses slit cloth stream, is fit into fixed bit and postpones and is heated, and heating temperature is 1150 DEG C；3)
Casting roll cooling temperature of circulating water is 5 DEG C, and total water-flowing amount is 80m3/h；4) prepare gas system after casting, argon pressure
0.7MPa, gas temperature control 5 DEG C；5) roll gap opening width is set as 0.55mm.
C. vacuum pump is closed, the high-purity argon gas of bulk purity 99.999% is filled with into medium frequency induction melting furnace extremely
The micro-positive pressure of 0.12MPa opens slide valve, and diversion pipe can be preheated by putting down, by alloy melt by that can preheat diversion pipe (diversion pipe
Preheating temperature be 1150 DEG C) and the uniform cloth of cloth stem bar flow in casting roll roll gap.
Its parameter is as shown in table 1 below.
Table 1 tests major parameter
D. testing the cloth stem bar used is suprasil material.In experimentation, pass through infrared monitoring camera and crucible
It is 60mm that tipping speed, which monitors and controls cloth stem bar inner melt liquid level,.Alloy melt is passed through by alloy liquid pressure
The uniform cloth of cloth stem bar flows in casting roll roll gap, alloy melt is controlled in roll gap liquid level in 5~10mm, and do not set side seal
Plate, the cooling casting forming of alloy, alloy melt cooling velocity is 10000 DEG C/s；In strip casting process, alloy is conducted heat fast by casting roll
Quickly cooling but, by control roll casting speed, casting-rolling force size and roll gap size goes out roll temperature to regulate and control alloy thin band, and alloy is gone out
Roll temperature is controlled at about 400 DEG C；Amorphous thin ribbon gas system after guide roller exports casting and rolling device and enters casting after forming
Be cooled further to 100 DEG C hereinafter, gas system 100 DEG C/s of cooling velocity.
Test obtains 0.55 millimeters thick amorphous band, as shown in Figure 2.Its microstructure photo and XRD curve such as Fig. 3 institute
Show.Cast Strip matrix is amorphous microstructure it can be seen from Fig. 2-Fig. 3, and there is only few Crystal impurities.
Embodiment two
Alloying component: (Zr53.5Hf1.5Cu30Al10Ni5)99.9O0.1；
Cloth stream mode: go deep into roll gap cloth stream；
Preparation flow:
A. match 50kg raw material by atomic percent, put into medium frequency induction melting furnace, and 6 are evacuated to melting chamber
×10-2Pa is heated to it to alloy raw material and is completely melt, and in 1400 DEG C of continuation melting 20min.
B. in fusion process, forming cavity preparation is completed, step includes: that 1) all valve bodies close on the cavity of forming cavity
Close, be evacuated to 0.5Pa, after be filled with argon gas, 99.99% or more bulk purity keeps the micro-positive pressure of 0.11MPa；2) cloth stem bar
It is preheated, cloth stem bar uses slit cloth stream, is fit into fixed bit and postpones and is heated, and heating temperature is 1000 DEG C；3)
Casting roll cooling temperature of circulating water is 5 DEG C, and total water-flowing amount is 80m3/h；4) prepare gas system after casting, argon pressure
0.7MPa, gas temperature control 5 DEG C；5) roll gap opening width is set as 0.5mm.
C. vacuum pump is closed, the high-purity argon gas of bulk purity 99.999% is filled with into medium frequency induction melting furnace extremely
The micro-positive pressure of 0.11MPa opens slide valve, and diversion pipe can be preheated by putting down, by alloy melt by that can preheat diversion pipe (diversion pipe
Preheating temperature be 1150 DEG C) and the uniform cloth of cloth stem bar flow in casting roll roll gap.
Its parameter is as shown in table 2 below.
Table 2 tests major parameter
D. testing the cloth stem bar used is suprasil material.In experimentation, pass through infrared monitoring camera and crucible
It is 60mm that tipping speed, which monitors and controls cloth stem bar inner melt liquid level,.Alloy melt is passed through by alloy liquid pressure
The uniform cloth of cloth stem bar flows in casting roll roll gap, alloy melt is controlled in roll gap liquid level in 5~10mm, and do not set side seal
Plate, the cooling casting forming of alloy, alloy melt cooling velocity is 6000 DEG C/s；In strip casting process, alloy is conducted heat fast by casting roll
Quickly cooling but, by control roll casting speed, casting-rolling force size and roll gap size goes out roll temperature to regulate and control alloy thin band, and alloy is gone out
Roll temperature is controlled at about 400 DEG C；Amorphous thin ribbon gas system after guide roller exports casting and rolling device and enters casting after forming
Be cooled further to 100 DEG C hereinafter, gas system 80 DEG C/s of cooling velocity.
Test obtains 0.5mm thickness amorphous band.Its microstructure photo and XRD curve are as shown in Figure 4.It can be seen by Fig. 4
Out, Cast Strip is completely amorphous tissue.
Embodiment three
Alloying component: (Cu60Zr20Hf10Ti10)99.9O0.1；
Cloth stream mode: go deep into roll gap cloth stream；
Preparation flow:
A. match 30kg raw material by atomic percent, put into medium frequency induction melting furnace, and 7 are evacuated to melting chamber
×10-2Pa is heated to it to alloy raw material and is completely melt, and in 1500 DEG C of continuation melting 10min.
B. in fusion process, forming cavity preparation is completed, step includes: that 1) all valve bodies close on the cavity of forming cavity
Close, be evacuated to 0.5Pa, after be filled with argon gas, 99.99% or more bulk purity keeps the micro-positive pressure of 0.11MPa；2) cloth stem bar
It is preheated, cloth stem bar uses slit cloth stream, is fit into fixed bit and postpones and is heated, and heating temperature is 1150 DEG C；3)
Casting roll cooling temperature of circulating water is 5 DEG C, and total water-flowing amount is 80m3/h；4) prepare gas system after casting, argon pressure
0.7MPa, gas temperature control 5 DEG C；5) roll gap opening width is set as 0.5mm.
C. vacuum pump is closed, the high-purity argon gas of bulk purity 99.999% is filled with into medium frequency induction melting furnace extremely
The micro-positive pressure of 0.11MPa opens slide valve, and diversion pipe can be preheated by putting down, by alloy melt by that can preheat diversion pipe (diversion pipe
Preheating temperature be 1150 DEG C) and the uniform cloth of cloth stem bar flow in casting roll roll gap.
Its parameter is as shown in table 3 below.
Table 3 tests major parameter
D. testing the cloth stem bar used is suprasil material.In experimentation, pass through infrared monitoring camera and crucible
It is 60mm that tipping speed, which monitors and controls cloth stem bar inner melt liquid level,.Alloy melt is passed through by alloy liquid pressure
The uniform cloth of cloth stem bar flows in casting roll roll gap, alloy melt is controlled in roll gap liquid level in 5~10mm, and do not set side seal
Plate, the cooling casting forming of alloy, alloy melt cooling velocity is 8000 DEG C/s；In strip casting process, alloy is conducted heat fast by casting roll
Quickly cooling but, by control roll casting speed, casting-rolling force size and roll gap size goes out roll temperature to regulate and control alloy thin band, and alloy is gone out
Roll temperature is controlled at about 400 DEG C；Amorphous thin ribbon gas system after guide roller exports casting and rolling device and enters casting after forming
Be cooled further to 100 DEG C hereinafter, gas system 60 DEG C/s of cooling velocity.
Test obtains 0.5 millimeters thick amorphous band.
Example IV
Alloying component: Fe69C5Si3B5P8Cr3Al2Mo5；
Cloth stream mode: go deep into roll gap cloth stream；
Preparation flow:
A. match 20kg raw material by atomic percent, put into medium frequency induction melting furnace, and 8 are evacuated to melting chamber
×10-2Pa is heated to it to alloy raw material and is completely melt, and in 1500 DEG C of continuation melting 10min.
B. in fusion process, forming cavity preparation is completed, step includes: that 1) all valve bodies close on the cavity of forming cavity
Close, be evacuated to 0.5Pa, after be filled with argon gas, 99.99% or more bulk purity keeps the micro-positive pressure of 0.11MPa；2) cloth stem bar
It is preheated, cloth stem bar uses slit cloth stream, is fit into fixed bit and postpones and is heated, and heating temperature is 1200 DEG C；3)
Casting roll cooling temperature of circulating water is 5 DEG C, and total water-flowing amount is 80m3/h；4) prepare gas system after casting, argon pressure
0.7MPa, gas temperature control 5 DEG C；5) roll gap opening width is set as 0.5mm.
C. vacuum pump is closed, the high-purity argon gas of bulk purity 99.999% is filled with into medium frequency induction melting furnace extremely
The micro-positive pressure of 0.11MPa opens slide valve, and diversion pipe can be preheated by putting down, by alloy melt by that can preheat diversion pipe (diversion pipe
Preheating temperature be 1150 DEG C) and the uniform cloth of cloth stem bar flow in casting roll roll gap.
Its parameter is as shown in table 4 below.
Table 4 tests major parameter
D. testing the cloth stem bar used is suprasil material.In experimentation, pass through infrared monitoring camera and crucible
It is 60mm that tipping speed, which monitors and controls cloth stem bar inner melt liquid level,.Alloy melt is passed through by alloy liquid pressure
The uniform cloth of cloth stem bar flows in casting roll roll gap, alloy melt is controlled in roll gap liquid level in 5~10mm, and do not set side seal
Plate, the cooling casting forming of alloy, alloy melt cooling velocity is 5000 DEG C/s；In strip casting process, alloy is conducted heat fast by casting roll
Quickly cooling but, by control roll casting speed, casting-rolling force size and roll gap size goes out roll temperature to regulate and control alloy thin band, and alloy is gone out
Roll temperature is controlled at about 520 DEG C；Amorphous thin ribbon gas system after guide roller exports casting and rolling device and enters casting after forming
Be cooled further to 100 DEG C hereinafter, gas system 50 DEG C/s of cooling velocity.
Test obtains 0.25 millimeters thick amorphous band.
Embodiment five
Alloying component: Ni40Cu5Ti16Zr28Hf1Al10；
Cloth stream mode: go deep into roll gap cloth stream；
Preparation flow:
A. match 20kg raw material by atomic percent, put into medium frequency induction melting furnace, and 6 are evacuated to melting chamber
×10-2Pa is heated to it to alloy raw material and is completely melt, and in 1500 DEG C of continuation melting 10min.
B. in fusion process, forming cavity preparation is completed, step includes: that 1) all valve bodies close on the cavity of forming cavity
Close, be evacuated to 0.5Pa, after be filled with argon gas, 99.99% or more bulk purity keeps the micro-positive pressure of 0.11MPa；2) cloth stem bar
It is preheated, cloth stem bar uses slit cloth stream, is fit into fixed bit and postpones and is heated, and heating temperature is 1200 DEG C；3)
Casting roll cooling temperature of circulating water is 5 DEG C, and total water-flowing amount is 80m3/h；4) prepare gas system after casting, argon pressure
0.7MPa, gas temperature control 5 DEG C；5) roll gap opening width is set as 0.5mm.
C. vacuum pump is closed, the high-purity argon gas of bulk purity 99.999% is filled with into medium frequency induction melting furnace extremely
The micro-positive pressure of 0.11MPa opens slide valve, and diversion pipe can be preheated by putting down, by alloy melt by that can preheat diversion pipe (diversion pipe
Preheating temperature be 1150 DEG C) and the uniform cloth of cloth stem bar flow in casting roll roll gap.
Its parameter is as shown in table 5 below.
Table 5 tests major parameter
D. testing the cloth stem bar used is suprasil material.In experimentation, pass through infrared monitoring camera and crucible
It is 60mm that tipping speed, which monitors and controls cloth stem bar inner melt liquid level,.Alloy melt is passed through by alloy liquid pressure
The uniform cloth of cloth stem bar flows in casting roll roll gap, alloy melt is controlled in roll gap liquid level in 5~10mm, and do not set side seal
Plate, the cooling casting forming of alloy, alloy melt cooling velocity is 7000 DEG C/s；In strip casting process, alloy is conducted heat fast by casting roll
Quickly cooling but, by control roll casting speed, casting-rolling force size and roll gap size goes out roll temperature to regulate and control alloy thin band, and alloy is gone out
Roll temperature is controlled at about 520 DEG C；Amorphous thin ribbon gas system after guide roller exports casting and rolling device and enters casting after forming
Be cooled further to 100 DEG C hereinafter, gas system 80 DEG C/s of cooling velocity.
Test obtains 0.25 millimeters thick amorphous band.
Above-described embodiment is merely to illustrate technical characterstic of the invention, rather than is limiting the scope of the invention,
Purpose is elaborated to the present invention.But the equivalent substitution that all spirits accordingly are substantially done, without departing from the present invention
The scheme of technical spirit is all within protection scope of the present invention.
Claims (10)
1. a kind of wide cut amorphous thin ribbon method that continuously big cooling rate is efficiently prepared with a thickness of 80~1500 μm, which is characterized in that
It sequentially includes the following steps:
(1) alloy blowing enters in crucible, and can preheat diversion pipe and its position control is cleared up, can pre- thermal conductivity
Be quartz material liner inside flow tube, and be attached to heating system, heating temperature be subject alloy setting temperature or more 100~
200 DEG C, logical cooling water conservation outside diversion pipe can be preheated；
(2) set component smelting amorphous master alloys, ingredient are as follows: zirconium base, copper-based, iron-based or ni-based amorphous alloy are at fission are pressed
It is uniformly to be mixed 5~30 minutes after metal melt, starts temperature control；
(3) control of the alloy melt degree of superheat is 50~300 DEG C, and the high-purity of 99.999% or more bulk purity is used during temperature control
Argon gas protection, melting chamber argon gas inside are micro-positive pressure, i.e. pressure is not less than 0.11MPa；
(4) in fusion process, forming cavity preparation is completed, step includes: a) all valve bodies closures on the cavity of forming cavity, is taken out
Argon gas is filled with after vacuum, 99.99% or more bulk purity keeps the micro-positive pressure for being not less than 0.11MPa；B) cloth stem bar carries out pre-
Heat, cloth stem bar use slit cloth stream, are fit into fixed bit and postpone and are heated, and heating temperature is subject alloy setting temperature
Above 100~200 DEG C；C) casting roll cooling temperature of circulating water is 3~5 DEG C, and total water-flowing amount is 70~90m3/h；D) prepare gas after casting
Body cooling system, 0.6~0.8MPa of argon pressure, gas temperature control 4~6 DEG C；
(5) alloy melting, can preheat diversion pipe and cloth stem bar preheating, forming cavity be filled with after the completion of argon gas, using rectilinear strip
Casting-rolling technology carries out amorphous thin ribbon preparation, into strip casting process: melting chamber slide valve is opened, diversion pipe decline can be preheated,
It is docked with cloth stem bar, medium frequency induction melting furnace topples over alloy in can preheat in diversion pipe；Cloth stem bar is suprasil material, is passed through
Infrared monitoring camera monitoring, by the tipping speed of medium frequency induction melting furnace control cloth stem bar inner melt height be 40~
60mm, by liquid level, by alloy melt, by cloth stem bar, vertically uniform cloth is flowed in casting roll roll gap, and alloy melt is in roll gap liquid
Position height 2~10mm of control, alloy melt cooling velocity are 500~75000 DEG C/s, the cooling casting forming of alloy；It is non-after forming
Brilliant strip is exported through guide roller, and is further cooled down into gas system after casting, is purged and is cooled down using low temperature argon gas, gas
50~800 DEG C/s of cooling velocity；
(6) after gas cooling, amorphous thin ribbon thickness range reaches 80~1500 μm, 110~550mm of width range；80~800 μm
Band volume is collected by batching in thickness specification Cast Strip, and the Cast Strip more than 800 μ m thicks is not batched, directly collected with provided in very thin tape form.
2. the wide cut amorphous thin ribbon side that continuously big cooling rate is efficiently prepared according to claim 1 with a thickness of 80~1500 μm
Method, which is characterized in that in strip casting process, alloy is conducted heat by casting roll to be quickly cooled down, by controlling roll casting speed, casting-rolling force size
Regulate and control alloy thin band with roll gap size and go out roll temperature, and alloy is gone out into roll temperature control in the crystallization temperature for being close to or smaller than alloy
Spend Tx；The casting-rolling force that roll casting speed is 0.20~1.8m/s, the control of casting-rolling force size is every 1cm width Cast Strip is 2~15kN, casting
Roller gap opening width is set as 80~1500 μm, and does not set side seal board.
3. the wide cut amorphous thin ribbon side that continuously big cooling rate is efficiently prepared according to claim 1 with a thickness of 80~1500 μm
Method, which is characterized in that by the opening size of cloth stem bar lower end, casting roll gap values between rollers, roll casting speed, copper casting roll, steel casting roll,
The casting-milling technology parameter control solidification cooling of casting roll cooling water inflow reaches 500~75000 DEG C/s.
4. the wide cut amorphous thin ribbon side that continuously big cooling rate is efficiently prepared according to claim 1 with a thickness of 80~1500 μm
Method, which is characterized in that the yttrium that mass percent is 0.0045~0.020 is added in zirconium base, copper-based, iron-based or ni-based amorphous alloy
Element, for removing O, N for bringing into environment pollution.
5. the wide cut amorphous thin ribbon side that continuously big cooling rate is efficiently prepared according to claim 1 with a thickness of 80~1500 μm
Method, which is characterized in that use quartz material slit cloth stem bar cloth stream, slit opening width is according to different product thickness design；
Cloth stem bar is online preheating, and preheating temperature is 100~200 DEG C of alloy graining temperature or more, and the open end of cloth stem bar lower end is logical
Cross that tungsten alloy piece is thermally conductive, the end region temperature of cloth stem bar reaches near alloy graining temperature, and dam is equipped with inside cloth stem bar and rushes in row
Current stabilization；Use the liner that can preheat diversion pipe for Ke Kuaisugenghuan quartz glass, preheating temperature is alloy graining temperature or more
100~200 DEG C, logical cooling water conservation outside diversion pipe can be preheated.
6. the wide cut amorphous thin ribbon side that continuously big cooling rate is efficiently prepared according to claim 1 with a thickness of 80~1500 μm
Method, which is characterized in that infrared monitoring camera is arranged in cloth stem bar width profile, feeds back to rollover control system and reaches cloth flow control
Purpose；Wherein, the extended distance casting roll roll gap Kiss line height control range of cloth stem bar lower end is 10~50mm, in cloth stem bar
Portion's liquid level is 40~60mm.
7. the wide cut amorphous thin ribbon side that continuously big cooling rate is efficiently prepared according to claim 1 with a thickness of 80~1500 μm
Method, which is characterized in that for casting roll using the double roller that is oppositely arranged of level, double roller two sides install backing roll additional, and casting roll diameter is 280~
420mm, every group of backing roll diameter design are greater than casting roll diameter 100mm.
8. the wide cut amorphous thin ribbon side that continuously big cooling rate is efficiently prepared according to claim 1 with a thickness of 80~1500 μm
Method, which is characterized in that melting chamber and forming cavity are using classification vacuum design, in which: melting chamber working vacuum degree reaches 1 × 10- 2Pa is hereinafter, forming cavity suction reaches 1Pa or less；When casting condition, environment is in argon gas guard mode, melting chamber and at
It is separated between shape chamber by slide valve, casting is opened before starting full of slide valve after argon gas.
9. the wide cut amorphous thin ribbon side that continuously big cooling rate is efficiently prepared according to claim 1 with a thickness of 80~1500 μm
Method, which is characterized in that amorphous alloy melting is carried out using medium frequency induction melting furnace+high purity graphite crucible, heating temperature is no more than
More than metal melt temperature 400 DEG C, oxidation and metallic element scaling loss are prevented.
10. continuously big cooling rate is efficiently prepared for the wide cut amorphous thin ribbon according to claim 1 with a thickness of 80~1500 μm
Method, which is characterized in that the Cast Strip trimming waste material for being no more than 20wt% is added in amorphous master alloy supplied materials.
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| CN201910276737.9A CN109967703B (en) | 2019-04-08 | 2019-04-08 | Method for continuously and efficiently preparing wide amorphous thin strip with thickness of 80-1500 mu m at high cooling speed |
| PCT/CN2019/081935 WO2020206611A1 (en) | 2019-04-08 | 2019-04-09 | METHOD FOR CONTINUOUS AND HIGH-EFFICIENT PREPARATION OF WIDE AMORPHOUS THIN STRIP HAVING THICKNESS OF 80-1,500 μM AT HIGH COOLING SPEED |
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| CN114559001A (en) * | 2022-03-08 | 2022-05-31 | 太原科技大学 | High-temperature alloy double-roller casting and rolling process |
| CN115283629A (en) * | 2022-08-02 | 2022-11-04 | 太原科技大学 | Method for preparing nickel-based high-temperature alloy by using double-roller casting and rolling process |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115323492A (en) * | 2022-09-20 | 2022-11-11 | 周中波 | Device and method for preparing single crystal copper wire at low cost |
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