Apparatus and method of manufacturing metallic or inorganic strands having a thickness in the micron range by melt spinning
10987728 · 2021-04-27
Assignee
Inventors
Cpc classification
B22D11/0611
PERFORMING OPERATIONS; TRANSPORTING
International classification
Abstract
Apparatus for producing elongate strands of metal comprises a rotatable wheel having a circumferential surface, at least one nozzle for directing a molten metal onto the circumferential surface and a collection means for collecting solidified strands of metal formed. The solidified strands are formed on the circumferential surface from the molten metal and are separated from the circumferential surface by centrifugal force generated by rotation of the wheel. The circumferential surface has a circumferentially extending structure having circumferentially extending edges and recesses formed between or bounded by the edges, and by an apparatus for controlling a gas pressure applied to the liquid metal which moves the liquid metal through the nozzle opening and delivers it to the circumferential surface of the rotatable wheel. The nozzle has a rectangular cross-section with a width of the nozzle opening in the circumferential direction of rotation of the wheel and a length transverse to the circumferential surface of the wheel which is greater than the width. A method and a wheel adapted for use in the apparatus are also claimed.
Claims
1. An apparatus for producing elongate strands of metal, the apparatus comprising a rotatable wheel having a circumferential surface, the circumferential surface having circumferentially extending edges and recesses formed between or bounded by the edges, each recess of the recesses defining a depth and a width with the depth being greater than 100 μm and the width being greater than 100 μm, a nozzle defining a nozzle opening having a width of between 10 μm to 100 μm for directing a molten metal onto the circumferential surface and to form solidified strands of metal on the circumferential surface from the molten metal, wherein the nozzle has a rectangular cross-section having a width of the nozzle opening in the circumferential direction of rotation of the wheel and a length transverse to the circumferential surface of the wheel which is greater than the width W, and wherein an apparatus is provided for controlling a gas pressure applied to the liquid metal which moves the liquid metal through the nozzle opening and delivers it to the circumferential surface of the rotatable wheel, wherein said wheel is mounted and configured to rotate within a chamber having an atmosphere at a higher pressure than ambient pressure.
2. The apparatus in accordance with claim 1, wherein the circumferential recesses defining the edges have a radial depth greater than 50 μm; and/or wherein the recesses have a cross-sectional shape selected from the group of members consisting of semi-circular, symmetrically v-shaped, asymmetrically v-shaped, rectangular and trapezoidal.
3. The apparatus in accordance with claim 1, there being peripherally extending lands at the circumferential surface of the wheel, each land being disposed between two circumferentially extending recesses.
4. The apparatus in accordance with claim 3, wherein said lands have widths of 1 mm or less.
5. The apparatus in accordance with claim 1, wherein the metal strands have the form of ribbons having a width of 200 μm or less.
6. The apparatus in accordance with claim 1, wherein the metal strands have a thickness of 50 μm or less.
7. The apparatus in accordance with claim 1, wherein the metal strands have at least one transverse dimension of 50 μm or less and a length at least ten times greater than said at least one transverse dimension.
8. The apparatus in accordance with claim 1, wherein the rotatable wheel is temperature controlled.
9. The apparatus in accordance with claim 1, wherein the wheel is made of one of a metal, a metal alloy, a ceramic material and graphite or is a wheel of a base material having a layer or type made of one of a metal, a metal alloy, a ceramic material, graphite and a vapour deposited carbon; and/or wherein said wheel is mounted to rotate within the chamber having the atmosphere, the atmosphere being at least one of air and an inert gas.
10. The apparatus in accordance with claim 1, wherein a deflector is provided upstream of the nozzle in the direction of rotation of the wheel to deflect boundary layer gas from the circumferentially extending surface prior to depositing molten metal on the surface via the nozzle.
11. The apparatus in accordance with claim 1, wherein the gas pressure applied to the molten metal is selected in the range from 50 mbar to 1 bar overpressure relative to a pressure external to the nozzle.
12. The apparatus in accordance with claim 1, wherein a motor is adapted to drive the wheel at a frequency of greater than 85 Hz for a copper wheel having a diameter of 200 mm.
13. The apparatus in accordance with claim 1, wherein the circumferential surface of the wheel has transversely extending features to control the length of the strands produced.
14. The apparatus in accordance with claim 1, wherein the material of the wheel is selected so that it does not readily bond to the molten metal.
15. A method for producing elongate strands of metal having at least one transverse dimension of 50 μm or less and a length at least ten times greater than said at least one transverse dimension, the method comprising the steps of directing a molten metal through a nozzle having a rectangular cross-section with a width of a nozzle opening in a circumferential direction of rotation of a rotating wheel and a length transverse to a circumferential surface of the rotating wheel which is greater than the width onto the circumferential surface of the rotating wheel, by applying a gas pressure to the molten metal to move it through the nozzle opening and deliver it to the circumferential surface of the rotating wheel, providing the circumferential surface of the rotating wheel with circumferentially extending edges and recesses formed between or bounded by the edges and collecting solidified strands of metal formed on the circumferential surface from the molten metal and separated from the circumferential surface by centrifugal force generated by rotation of the rotating wheel, the method further comprising the steps of controlling the width of the nozzle opening, controlling the gas pressure applied to the molten metal to move it through the nozzle opening and deliver it to the circumferential surface of the rotating wheel and controlling a speed of rotation of the rotating wheel to reduce a flow of molten metal onto the circumferential surface of the rotating wheel to a level at which it is concentrated by the forces that are acting at said circumferentially extending edges and recesses formed between or bounded by the edges and using these edges to concentrate the molten metal at the edges to produce the desired elongate strands of metal, the nozzle opening having a width of between 10 μm to 100 μm and wherein the rotating wheel is mounted and configured to rotate within a chamber having an atmosphere at a higher pressure than ambient pressure.
16. The method in accordance with claim 15, wherein the flow of molten metal is reduced to a level at which the elongated strands have a width of 200 μm to 1 μm.
17. The method in accordance with claim 15, wherein the metal strands have a thickness of 50 μm to 1 μm.
Description
(1) The invention will now be described in further detail and by way of example only with reference to the accompanying drawings and various examples of the method of the invention. In the drawings there are shown:
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(25) Turning now to the schematic drawing of the melt spinning process shown in
(26) The pressure P applied to the molten metal can also be used to change the flow rate. Clearly a relatively large pressure leads to a higher flow rate than a relatively lower pressure. A minimum pressure P is always required in order to force the molten metal through the nozzle N, as gravity alone is not normally sufficient to ensure adequate flow, particularly with a relatively small width W of the nozzle opening. In fact this is advantageous because otherwise some form of valve would be necessary and a valve for regulating the flow of molten metal is technically challenging. It should be noted that the pressure difference ΔP is dependent on the metal used and on the width of the nozzle opening in the circumferential direction. It is also dependent on the length of the nozzle opening in a direction parallel to the axis of rotation of the wheel. The length of the nozzle opening can be varied within wide limits. For laboratory experiments values of 10 to 12 mm have been found useful. In production much greater lengths could be selected in dependence on the axial width of the circumferential surface of the wheel.
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(28) The grooves or recesses G can have a cross-sectional shape selected from the group comprising semi-circular, symmetrically v-shaped, asymmetrically v-shaped, rectangular and trapezoidal and grooves G of this kind are shown in
(29) When lands are provided they generally have widths of 1 mm or less.
(30) As can be seen from
(31) The overall aim of the tests carried out to date is to investigate whether the melt spinning process can produce thin fibers with diameters in the micron range, for industrial applications such as light weight, mechanically strengthened textiles (textiles reinforced by the metal strands), filters and catalytically active materials. The actual apparatus used is shown in
(32) The cover for closing the port 16 can be a hinged or removable glass cover permitting the material collected in the cylindrical extension 18 to be observed, removed and filmed as required.
(33) The following experiments were conducted:
COMPARATIVE EXAMPLE 1
(34) In the first experiment melt spun ribbons were generated on a standard copper wheel B with a diameter of 200 mm and a smooth circumferential surface 32 (indicated in
(35) The specific parameters used were as follows:
(36) TABLE-US-00001 Weight of metal sample 10 g Length L of nozzle opening 10 mm Width W of nozzle opening 0.4 mm Temp. of wheel RT Gas in chamber Argon Pressure in chamber 12 400 mbar Temp. of gas in chamber 12. RT Temperature of molten metal 1350° C. Pressure applied to molten metal 200 mbar (overpressure) Speed of wheel 30 Hz Diameter of wheel 200 mm Distance between wheel and orifice 0.2 mm
ILLUSTRATIVE EXAMPLE 1
(37) Using the same apparatus as in
(38) To investigate the microstructure of the melt-spun ribbons shown in
INVENTIVE EXAMPLE 1
(39) For this example the aim was to make the single ribbons finer by promoting the break-up of the liquid melt on the copper wheel by reducing the volume of the liquid pool forming on the wheel between the wheel surface and the orifice of the crucible K. This concept was based on the recognition that single ribbons with 1 mm widths would have been generated on the flat surfaces in between the semicircular grooves, if the breakup of the ribbon material could be promoted to reach completion. In this example, this was achieved using the same structured surface as in Illustrative Example 1, and the same set of parameters as in Comparative Example 1 but by increasing the speed of rotation of the wheel B to 60 Hz corresponding to a surface speed of the wheel of 37.5 m/s. The resultant ribbons are shown in
(40) The mass and size distribution of the strands shown in the photograph of
(41) Total mass=9.70 g (100%)
(42) Mass of agglomerated strands=2.83 g (29%);
(43) Length of the strands: plural centimetres (10 cm);
(44) Typical width: ca. 1.3 mm
(45) Mass of remaining material: 6.73 g (69%) Mass of material lost; =0.14 g (1%).
(46) The diagrams of
INVENTIVE EXAMPLE 2
(47) In this example the same basic set-up was retained as for Inventive Example 1 but the pressure on the melt was reduced to 100 mbar in order to reduce the deposition rate of the melt onto the spinning wheel. This resulted in two types of metal strands:
(48) Metallic strands in the form of agglomerations of similar strands with homogenous diameters and of several cm's length and strands in the form of a fiber mix including all the remaining fiber products.
(49) The following results were obtained:
(50) Total mass 6.06 g (100%),
(51) Mass of agglomerated strands 4.18 g (69%)
(52) Average width 389 μm+/−167 μm
(53) Average thickness 28 μm+/−7 μm
(54) Length of strands ca 10 cm
(55) Residual mix 1.66 g (27%)
(56) Length several mm's,
(57) Average width of ca. 20 μm
(58) Material loss 0.22 g (4%)
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INVENTIVE EXAMPLE 3
(61) In this case the parameters used were as follows:
(62) Material lead (Pb)
(63) Surface structure, size and speed of rotation of copper wheel as in inventive example 1
(64) TABLE-US-00002 Weight of metal sample 9.04 g Nominal length of nozzle opening 10 mm Nominal width of nozzle opening 0.4 mm Temp of wheel RT (~23° C.) Gas in chamber Argon Pressure in chamber 12 400 mbar Temp. of gas in chamber 12 RT Ejection temperature 400° C. < T.sub.ejection < 700° C. Ejection pressure 100 mbar Speed of wheel 60 Hz Diameter of wheel 200 mm Distance between nozzle and wheel 0.3 mm Average width of the resultant ribbon 0.7 +/− 0.05 mm Average thickness of the resultant ribbon 59 μm +/− 23 μm
(65) The ribbons produced in this way are shown in
INVENTIVE EXAMPLE 4
(66) In this case the parameters used were as follows:
(67) Material Aluminium (Al)
(68) TABLE-US-00003 Weight of metal sample 4.85 g Nominal length of nozzle opening 10 mm Nominal width of nozzle opening 0.4 mm Temp of wheel RT (~25° C.) Gas in chamber Argon Pressure in chamber 12 400 mbar Temp. of gas in chamber 12 RT Ejection temperature 900° C. Ejection pressure 200 mbar Speed of wheel 60 Hz Diameter of wheel 200 mm Distance between nozzle and wheel 0.3 mm Average width of the resultant ribbon 2.0 +/− 0.3 mm Average thickness of the resultant ribbon 46 μm +/− 10 μm
(69) In the following further examples will be given of fibres produced using different parameters of the melt spinning process using a structured wheel. In all the following examples the wheel is a copper wheel having various groove configurations which are illustrated in the summary of
EXAMPLE 5
(70) TABLE-US-00004 Material: Fe40Ni40B20 Experiment MS03 Nominal length of nozzle opening 10 mm Nominal width of nozzle opening 400 μm Temp of wheel RT (~23° C.) Gas in chamber Argon Pressure in chamber 12 400 mbar Temp. of gas in chamber 12 RT Ejection temperature 1350° C. Ejection pressure 200 mbar Speed of wheel 30 Hz Diameter of wheel 200 mm Distance between nozzle and wheel 0.3 mm Average width of the resultant ribbon Textured ribbon, lamella with the profile of the grooved structure, see FIG. 17 Average thickness of the resultant ribbon Experiment failed
(71) The textured ribbon produced in this experiment is shown in photographs with different magnifications in
EXAMPLE 6
(72) TABLE-US-00005 Material: Fe40Ni40B20 Experiment MS23 Nominal length of nozzle opening 10 mm Nominal width of nozzle opening 400 μm Temp of wheel RT (~23° C.) Gas in chamber Argon Pressure in chamber 12 400 mbar Temp. of gas in chamber 12 RT Ejection temperature 1350° C. Ejection pressure 200 mbar Speed of wheel 85 Hz Diameter of wheel 200 mm Distance between nozzle and wheel 0.3 mm Average width of the resultant ribbon Textured ribbon, the lamella breaks up and no longer follows the shape of the groove Average thickness of the resultant ribbon Experiment failed
(73) The textured ribbon produced in this experiment is shown in photographs with different magnifications in
EXAMPLE 7
(74) TABLE-US-00006 Material: Fe40Ni40B20 Experiment MS34 Nominal length of nozzle opening 10 mm Nominal width of nozzle opening 100 μm Temp of wheel RT (~23° C.) Gas in chamber Argon Pressure in chamber 12 400 mbar Temp. of gas in chamber 12 RT Ejection temperature 1350° C. Ejection pressure 400 mbar Speed of wheel 85 Hz Diameter of wheel 200 mm Distance between nozzle and wheel 0.3 mm Width of the resultant ribbons Max 171.4 μm, min 10.4 μm Thickness of the resultant ribbon <5 μm
(75) The fibres produced in this experiment are shown in photographs with different magnifications in
EXAMPLE 8
(76) TABLE-US-00007 Material: Fe40Ni40B20 Experiment MS031 Nominal length of nozzle opening 10 mm Nominal width of nozzle opening 100 μm Temp of wheel RT (~23° C.) Gas in chamber Argon Pressure in chamber 12 400 mbar Temp. of gas in chamber 12 RT Ejection temperature 1350° C. Ejection pressure 400 mbar Speed of wheel 85 Hz Diameter of wheel 200 mm Distance between nozzle and wheel 0.3 mm Average width of the resultant ribbons Max 146.2 μm, min8.4 μm Thickness of the resultant ribbons <5 μm
(77) The fibres produced in this experiment are shown in photographs with different magnifications in
EXAMPLE 9
(78) TABLE-US-00008 Matterial: Fe40Ni40B20 Experiment MS37 Nominal length of nozzle opening 10 mm Nominal width of nozzle opening 50 μm Temp of wheel RT (~23° C.) Gas in chamber Argon Pressure in chamber 12 400 mbar Temp. of gas in chamber 12 RT Ejection temperature 1350° C. Ejection pressure 1000 mbar Speed of wheel 85 Hz Diameter of wheel 200 mm Distance between nozzle and wheel 0.3 mm Width of the resultant ribbons Max 48.4 μm, min 9.3 μm Thickness of the resultant ribbon <5 μm
(79) The fibres produced in this experiment are shown in photographs with different magnifications in
EXAMPLE 10
(80) TABLE-US-00009 Material: Fe40Ni40B20 Experiment MS33 Nominal length of nozzle opening 10 mm Nominal width of nozzle opening 100 μm Temp of wheel RT (~23° C.) Gas in chamber Argon Pressure in chamber 12 400 mbar Temp. of gas in chamber 12 RT Ejection temperature 1350° C. Ejection pressure 400 mbar Speed of wheel 60 Hz Diameter of wheel 200 mm Distance between nozzle and wheel 0.3 mm Width of the resultant fobres Max 75.1 μm, min 2.8 μm Thickness of the resultant fibres <5 μm
(81) The fibres produced in this experiment are shown in photographs with different magnifications in
EXAMPLE 11
(82) TABLE-US-00010 Material: Stainless steel V2A Experiment MS058 Nominal length of nozzle opening 10 mm Nominal width of nozzle opening 75 μm Temp of wheel RT (~23° C.) Gas in chamber Argon Pressure in chamber 12 400 mbar Temp. of gas in chamber 12 RT Ejection temperature 1550° C. Ejection pressure 800 mbar Speed of wheel 95 Hz Diameter of wheel 200 mm Distance between nozzle and wheel 0.3 mm Width of the resultant fibres Max 144 μm, min 2.3 μm Thickness of the resultant fibres <5 μm
(83) The values of all the examples 5 to 11 are summarized—together with other relevant values—in the Table of