EP2226828A1 - Kaltkathode und verfahren zu ihrer herstellung - Google Patents

Kaltkathode und verfahren zu ihrer herstellung Download PDF

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Publication number
EP2226828A1
EP2226828A1 EP07873394A EP07873394A EP2226828A1 EP 2226828 A1 EP2226828 A1 EP 2226828A1 EP 07873394 A EP07873394 A EP 07873394A EP 07873394 A EP07873394 A EP 07873394A EP 2226828 A1 EP2226828 A1 EP 2226828A1
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Prior art keywords
cathode
workpiece
temperature
grains
plastic deformation
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EP07873394A
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English (en)
French (fr)
Inventor
Radik Rafikovich Mulyukov
Yulai Mukhametovich Yumaguzin
Linar Raisovich Zubairov
Rinat Khamzovich Khisamov
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Institute For Metals Superplasticity Problems Of Russian Academy Of Sciences (IMSP RAS)
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Institute For Metals Superplasticity Problems Of Russian Academy Of Sciences (IMSP RAS)
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Publication of EP2226828A1 publication Critical patent/EP2226828A1/de
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J1/00—Details of electrodes, of magnetic control means, of screens, or of the mounting or spacing thereof, common to two or more basic types of discharge tubes or lamps
    • H01J1/02—Main electrodes
    • H01J1/30—Cold cathodes, e.g. field-emissive cathode
    • H01J1/304—Field-emissive cathodes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
    • H01J9/02—Manufacture of electrodes or electrode systems
    • H01J9/022—Manufacture of electrodes or electrode systems of cold cathodes
    • H01J9/025—Manufacture of electrodes or electrode systems of cold cathodes of field emission cathodes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2201/00—Electrodes common to discharge tubes
    • H01J2201/30—Cold cathodes
    • H01J2201/304—Field emission cathodes

Definitions

  • the invention relates to the electronic engineering and, more specifically, to the fields thereof where the physical phenomenon of electron, or ion-electron, or cold emission is used, and concerns a cold cathode and a method for fabricating the same.
  • Cold cathodes operating on the principle of secondary electron, or ion-electron, or cold emission are used widely. They are utilized in such devices as vacuum devices and gas-discharge devices, including optical quantum generators, helium-neon lasers, detection devices, ion sources. The latter are used, in particular, as important components of widespread devices such as plasmatrons, mass spectrometers. Operation accuracy and efficiency of the aforementioned devices are determined by cold cathode characteristics. With advances in microelectronics and nanoelectronics, requirements for cold cathode characteristics are becoming more stringent.
  • cathodes made of aluminum, beryllium, magnesium, iron, nickel, tantalum, molybdenum and other metals or alloys based thereon are used as the cold cathodes [1].
  • the choice of a specific cathode material is governed by the requirements for the cathode service life and efficiency, in the latter case with regard to the most important emission characteristic of a metal or alloy, i.e. an electronic work function.
  • a reduction in the electronic work function value allows, e.g. in an ion source, a greater ionic current to be obtained at a lower value of applied voltage.
  • a reduction in the work function value e.g. in gas-discharge devices, allows a gas pressure to be decreased, thereby reducing the load on a vacuum system of the device, which eventually results in improving reliability of the device.
  • a cold cathode of a gas-discharge device is known in [3], said cathode being made of substantially pure aluminum which is doped with silicon in the amount of 0.5-1.65 wt.%.
  • silicon to aluminum promotes formation of homogeneous microstructure and reduction in the grain size, that in turn promotes improved resistance of the oxide layer and prevents cathode sputtering.
  • a cold cathode is known in [4] a material of which further comprises iron in the amount of 0.1-2.0 wt.%.
  • the addition of iron to an aluminum-silicon alloy reduces lattice parameters due to the formation of a homogeneous substitution solid solution in aluminum. Thereby, resistance of the cathode surface to ion bombardment is improved and sputtering is further reduced.
  • a cold cathode of a gas-discharge device is known in [5], where nickel with addition of aluminosilicate of cesium or rubidium in the amount of 0.5-25 wt.% is used as the cathode material, which allows stable operation of the cathode under intensive ion bombardment conditions and increases the emission current, including due to a reduced work function.
  • a method for fabricating the cathode involves the use of hot plastic deformation, in particular, hot forging, die forming, rolling, for producing a cathode workpiece.
  • the cathodes can be also fabricated using powder metallurgy techniques, in particular, by compacting a mixture of powders into a desired cathode configuration and then sintering the compacted material [5].
  • a drawback of the techniques associated with changing the alloy composition by addition of special additives [3, 4, 5] is that it is impossible to fabricate a cathode having predetermined properties with a high degree of accuracy, which is caused by the fact that it is difficult to keep the same alloy composition in different melts. This is the reason for indication of rather wide ranges of the additive amounts in the known solutions.
  • Such cathodes cannot be interchangeable when used in the aforementioned state-of-the-art devices.
  • methods for fabricating cold cathodes that involve changing the alloy composition by addition of special additives have limited capabilities for improving the cathode efficiency.
  • changing the composition of any commercial alloy is extremely uneconomic.
  • a method for fabricating the same [6] involves using cold plastic deformation for strengthening a near-surface layer of the cathode.
  • the plastic deformation is carried out by rolling a working surface of the cathode by a distributing ball head.
  • the strengthening via plastic deformation results in improving durability of the cathode.
  • This technique is however reported to be unacceptable for processing beryllium due to its high hardness and brittleness. That is, capabilities of the cold plastic deformation carried out in this fashion are also restricted.
  • a cathode (cathode target) and a method for fabricating the same are known in [7].
  • the method comprises the steps of providing a cathode workpiece of a metal or alloy, subjecting the cathode workpiece to cold deformation in two stages into a desired cathode configuration.
  • the first stage comprises cold rolling a card-shaped workpiece (card blank) with rolling directions varied, which is necessary to avoid formation of a pronounced texture.
  • a cylinder or cup shape is imparted to the semi-finished cathode.
  • the workpiece can be subjected to thermal treatment, such as high-temperature tempering or annealing, to relieve internal stresses.
  • the cathode has a homogeneous texture and a uniform fine-grained structure with a grain size of 15 ⁇ m and greater.
  • the known methods for fabricating a cold cathode using plastic deformation do not involve techniques that could remarkably improve the cold cathode efficiency owing to a reduction in the work function, that is, the manufacturing capabilities thereof are also restricted as in the case of changing the alloy composition.
  • SPD methods include equal-channel angular pressing (ECAP) and torsion under quasi-hydrostatic pressure on a Bridgemen anvil-type setup [9, 10].
  • a closest prior art (prototype) to the present invention is a cold cathode and a method for fabricating the same as disclosed in [11].
  • an experimental cathode sample was fabricated from tungsten of 99.99% purity by an SPD deformation method, namely, by torsion under quasi-hydrostatic pressure on a Bridgemen anvil-type setup to a true logarithmic degree of strain e ⁇ 7. Thereby, a structure with a nanometric grain size of about 100 nm was obtained in the sample.
  • An electronic work function was determined by measuring the contact potential difference, more precisely the difference between the work function of the cathode sample subjected to the SPD and having the nanometric grain size and the work function of a cathode sample in a normal coarse-grained state. It was found that the formation of a structure with nanometric size of grains leads to a reduction in the work function of the metal. The reduction of the work function for tungsten with the grain size of about 100 nm was ⁇ 0.8 eV. Complex studies of the sample were conducted, including transmission electron microscopy and also numerical simulation of the experiment.
  • Such a tube of current includes the grain boundaries per se and their vicinities of about 10 nm wide.
  • the SPD leads to a remarkable improvement in the cold cathode strength, which may result in an increase of its durability [6].
  • the ability appears to use cold deformation for strengthening a cold cathode of brittle materials.
  • the SPD is generally carried out under the conditions of all-around compression, as with the ECAP, or under the conditions close to all-around compression, as with the torsion under quasi-hydrostatic pressure at a Bridgemen anvil-type setup.
  • the object of the invention is to improve a method for fabricating a cold cathode using severe plastic deformation, which is capable of further improving the cathode efficiency through a reduction of the electronic work function, and also to expand manufacturing capabilities of the method for fabricating cold cathodes from various metals and alloys.
  • the object is attained in the case a method for fabricating a cold cathode, according to which a cathode workpiece of a metal or alloy is subjected to severe plastic deformation to transform an initial structure of the workpiece into a fragmented structure comprising fragments of nanometric size or into a mixed structure comprising grains and fragments of nanometric size, is characterized in that after the severe plastic deformation the cathode workpiece is subjected to a low-temperature annealing for transforming at least part of said fragments into grains of nanometric size at a temperature not lower than the operating temperature T oper of the cathode.
  • severe plastic deformation or SPD (also referred to as “intensive plastic deformation” in the Russian literature) is understood the plastic deformation of a metallic material up to highest degrees of plastic strain (up to some thousands percent) at relatively low homologous temperatures (typically below 0.3 of the melting temperature), which leads to subdivision of grains in the initial structure of the material.
  • the severe plastic deformation of the cathode workpiece is carried out at a degree e ⁇ 4, where e is the true logarithmic degree of strain.
  • the lower limit of strain degree e is determined by the attainment of nanometric size of elements of the cathode workpiece structure (i.e. grains and fragments) and by the provision for a desired effect of the work function reduction.
  • the upper limit of strain degree e may be substantially any one, and is selected so that to maximize the refinement of grains and fragments and to minimize manufacturing costs. Therefore, a preferred range of the strain degree e is from 4 to 20, more preferably from 5 to 10, and most preferably from 6 to 8.
  • the initial structure of the cathode workpiece before the severe plastic deformation may be substantially any one, such as a grained structure (e.g. a coarse-grained structure with grains of a size much higher than 10 ⁇ m, or a fine-grained structure with grains of a size slightly higher than 1 ⁇ m), or even a partially fragmented structure possibly obtained at preceding deformation steps if they are desirable.
  • a grained structure e.g. a coarse-grained structure with grains of a size much higher than 10 ⁇ m, or a fine-grained structure with grains of a size slightly higher than 1 ⁇ m
  • a partially fragmented structure possibly obtained at preceding deformation steps if they are desirable.
  • the severe plastic deformation of the cathode workpiece is carried out by torsion under quasi-hydrostatic pressure on a Bridgemen anvil-type setup, which often allows the required degree of strain to be attained in a single pass and, hence, allows the manufacturing costs to be reduced.
  • the low-temperature annealing of the cathode workpiece is carried out at a temperature selected in the temperature range of from T oper to 0.4 ⁇ T melt , where T melt is the melting temperature of said metal or alloy.
  • T melt is the melting temperature of said metal or alloy.
  • the lower annealing temperature limit should be not lower than the cathode operating temperature T oper to avoid thermal instability of the cathode structure during its service.
  • the upper annealing temperature limit is restricted by the grain size in the workpiece structure not going beyond the nanometric range (i.e. does not exceed 1 ⁇ m) and is determined by maximizing the work function reduction effect as a result of the annealing.
  • the annealing temperature is selected in the range of from T oper to 0.3 ⁇ T melt , and most preferably in the range of from 0.1 ⁇ T melt to 0.25 ⁇ T melt .
  • the low-temperature annealing of the cathode workpiece is carried out for a time period of from 1 minute to 100 hours, and more preferably from 0.5 hour to 2 hours.
  • the annealing time limits in accordance with the invention may be substantially any ones, and are selected so that to maximize the work function reduction effect and to minimize manufacturing costs, provided the grain size in the workpiece structure does not fall outside the nanometric range (i.e. does not exceed 1 ⁇ m).
  • the annealing time and temperature in accordance with the invention are preferably selected with regards to each other. Typically, the higher the annealing temperature, the shorter the annealing time, and vice versa.
  • the at least part of said fragments transformed into grains during the low-temperature annealing is from 10 to 100%, more preferably from 20 to 100%, and even more preferably from 30 to 100%, of their number in the fragmented or mixed structure of the workpiece after the severe plastic deformation.
  • the cathode workpiece after the low-temperature annealing has a predominantly grained structure, i.e. comprises at least 50% grains, and in the best case it has a substantially grained structure, i.e. comprises at least 90% grains.
  • a machining or plastic working of the cathode workpiece is carried out after the severe plastic deformation and the low-temperature annealing, wherein the deformation temperature in the plastic working of the cathode workpiece is regulated so that to preserve the nanometric size of grains. Moreover, any further cathode processing, if necessary, is carried out so that to preserve the nanometric size of grains.
  • the object of the invention is attained in the case a cold cathode of a metal or alloy having a structure comprising grains of nanometric size and obtained by severe plastic deformation, is characterized in that the cathode has a predominantly grained structure with the grains of nanometric size, said structure being obtained by the method according to any of embodiments of the invention.
  • SPD severe plastic deformation
  • a subdivision of initial grains occurs to form fragments finer than the initial grains, which fragments represent disoriented regions separated by unformed boundaries of dislocational type.
  • the fragments transform into grains of about the same size as the fragments, with grain-type boundaries being formed between them.
  • the formation of grains and their respective boundaries proceeds more intensively in pure metals, than in alloys, due to hindered boundary migration in alloys.
  • a subdivision of the newly formed grains occurs further in the course of SPD. The above processes proceed simultaneously and continuously while SPD is being carried out.
  • both grains of nanometric size and fragments of nanometric size are inevitably present in the metal or alloy, i.e. the metal or alloy has a mixed structure or a fragmented structure after the SPD. Meanwhile, alloys generally have a fragmented structure for the reason mentioned above.
  • the former pattern was revealed, in particular, in additional studies of the structure of a sample made of tungsten, and the latter pattern was revealed in studies of the structure of a sample made of the AMG6 aluminum alloy.
  • Boundaries of fragments have a dislocational nature, i.e. they are crystallographically unformed, and remain such during and after the deformation.
  • the unformed fragment boundaries cannot provide a further reduction in the electronic work function.
  • the work function in cathode samples with a completely fragmented structure after the SPD may not differ from that in cathode samples having a coarse-grained (above 1 ⁇ m) structure obtained by conventional methods.
  • a transformation of the mixed structure into a predominantly grained or even completely grained structure preferably takes place at the low-temperature annealing.
  • the annealing temperature sufficient only for transformation of fragments into grains does not result in increasing the sizes of structure elements.
  • the nanometric size of grains remains approximately equal to the size of fragments.
  • the sizes of grains may be several nanometers greater, preferably in the range of ⁇ 20-30 nm, than the fragment sizes. Boundaries of the formed nanometric-size grains give an additionally contribution to the electronic work function reduction with respect to the contribution which gives SPD alone, in case of a less fragmented structure, e.g. as in the method for fabricating a cathode of tungsten. With a predominantly fragmented structure after SPD, only annealing can provide the work function reduction effect described in [11].
  • a low-temperature annealing temperature for most of metals and alloys traditionally used for cold cathode fabrication is recommended to be selected from about 0.1 ⁇ T melt to about 0.2 ⁇ T melt . It has been experimentally found that such an annealing temperature is well suited to both substantially pure metals such as nickel, tungsten, titanium, molybdenum, and alloys such as AMG6, E125, etc. Annealing at a lower temperature frequently fails to lead to sufficient modifications in the strained sample structure. Furthermore, a cold cathode may warm up during its service, typically from room temperature to an operating temperature in the order of 50-100°C, so the annealing temperature should not be below the cathode operating temperature to avoid thermal instability of the cathode structure during service.
  • the method in accordance with the present invention allows severe plastic deformation capabilities to be more completely used for reducing the electronic work function value.
  • the SPD can be used to improve efficiency of a cathode made of substantially any metal or alloy conventionally used for this purpose.
  • the use of SPD alone cannot result in improvement of efficiency of a cathode made of a metal or alloy prone to intense fragmentation under SPD.
  • a cold cathode and a method for fabricating the same in accordance with the invention are more cost-effective as compared to the closest prior art because the cathode is fabricated from commercial alloys without incorporating additional additives to reduce the electronic work function.
  • a method in accordance with the invention allows to improve the cold cathode strength.
  • the strength improvement is to a somewhat less amount than in the closest prior art due to a partial removal of SPD-induced work hardening during the low-temperature annealing.
  • the invention provides the possibility of using cold deformation for strengthening a cold cathode made of brittle materials.
  • a setup for ECAP-pressing has a more complex design and, thus, several passes are performed to reach a required degree of strain, but an intermediate cathode workpiece can be produced in the form of a rod of a predetermined diameter which can be separated into semi-finished products of a predetermined thickness by cutting techniques.
  • the SPD can be also used to consolidate particles or clusters of atoms obtained by techniques conventional in the field of powder metallurgy.
  • a thus preformed block can be used as the cold cathode workpiece.
  • the cost of such a cold cathode will be higher, so this embodiment of the method seems to be the least economically sound.
  • SPD methods have certain restrictions associated with small dimensions of workpieces to be processed and with the necessity to make the workpieces into specified shapes: a rod for the ECAP or a disc for the torsion under quasi-hydrostatic pressure.
  • a cold cathode in accordance with a method of the present invention, it is possible to use, for example, as in [1], aluminum, beryllium, iron, nickel, tungsten, tantalum, molybdenum, titanium, niobium, zirconium and other metals or alloys based thereon, i.e. materials conventionally used for fabrication of a cold cathode.
  • a cold cathode material commercially pure nickel (Ni 99.98 wt.%), commercially pure tungsten (99.99 wt.%), a commercial aluminum alloy (AMG6 having a nominal composition, in wt.%: Mg 6.3%; Mn 0.6%; Cu ⁇ 0.1%; Zn ⁇ 0.2%; Fe ⁇ 0.4%; Si ⁇ 0.4%, the balance Al) and a commercial zirconium alloy (E125 having a nominal composition, in wt.%: Nb 2.5%, the balance Zr).
  • AMG6 having a nominal composition, in wt.%: Mg 6.3%; Mn 0.6%; Cu ⁇ 0.1%; Zn ⁇ 0.2%; Fe ⁇ 0.4%; Si ⁇ 0.4%, the balance Al
  • a commercial zirconium alloy E125 having a nominal composition, in wt.%: Nb 2.5%, the balance Zr.
  • the presented examples do not exclude the possibility of using all other metals and alloys which a cold cathode can be fabricated from.
  • a cathode workpiece was deformed by an SPD method, in particular, by torsion under quasi-hydrostatic pressure on a Bridgemen anvil-type setup ( Fig. 1 ).
  • a cathode workpiece is denoted by the reference number 1 and blocks of an anvil are denoted by the reference number 2.
  • discs 10 mm in diameter and 0.2 mm in thickness were cut out from a commercial hot-pressed rod of AMG6 alloy, as well as from ingots of nickel and tungsten and of E125 alloy.
  • the disc workpieces were put between two blocks of the anvil and were compressed under pressure P ⁇ 7 GPa at room temperature.
  • the structure obtained by the severe plastic deformation had the following elements: in the form of predominantly fragments of nanometric size in the cathode workpieces of E125 and AMG6 alloys, and in the form of fragments and predominantly grains of nanometric size in cathode workpieces of tungsten and nickel. Deformation of all the workpieces was performed up to the true logarithmic degree of strain e ⁇ 7.
  • An average size of the fragments and grains in the cathode workpieces of nickel and tungsten was about 100 nm. The extent of fragmentation of the nickel workpiece was greater than that of the tungsten workpiece.
  • An average size of the fragments in the cathode workpieces of AMG6 alloy was about 100 nm.
  • An average size of the grains and fragments in the cathode workpiece of E125 alloy was about 90 nm.
  • the cathode workpieces were subjected to a low-temperature annealing.
  • the annealing was carried out at the following temperatures:
  • the annealing time was about 1 hour in this case.
  • the low-temperature annealing was carried out in vacuum in an electric furnace.
  • the finished cold cathode samples were disc-shaped, 10 mm in diameter and ⁇ 0.1 mm in thickness. An appearance of one experimental sample of the finished cold cathode is shown in Fig. 2 .
  • the cathode can be used as a component of an ion source.
  • the work function was measured by a contact potential difference method [12].
  • a relative work function variation ⁇ was determined directly from the shift of delay lines relative to each other for the cathode samples fabricated by the invented method and the closest prior art method.
  • the reduction of the work function results in improving the cold cathode efficiency, e.g. when the cathode is operated in an ion source.
  • the ion source is an electric vacuum device intended to produce a directional flow of ions, whose action is based on the use of various kinds of electric discharges in a gas (inert gases, hydrogen) or metal vapors.
  • a simplest ion source is a diode cell ( Figs. 3 , 4 ) comprising a bulb filled with an inert gas; and properties of the ion source are determined by the electron flow/gas medium interaction and by the electric field between electrodes (an anode and a cathode).
  • a characteristic of the operation efficiency of an ion source with a cold cathode is the ability to produce a higher operating current of ion beam at a lower operating voltage, as well as to provide ion beam of homogeneous composition and ionic current of constant density.
  • the cathode operation efficiency is dependent on cathode material properties, in particular, on the electronic work function. The lower the electronic work function is, the greater is the secondary ion-electron emission ratio and, hence, the ion beam intensity.
  • curve 1 is a current-voltage characteristic of a diode cell with the cold cathode fabricated by the method in accordance with the invention from nickel, E125 and AMG6 alloys and tungsten, respectively;
  • curve 2 is a current-voltage characteristic of a diode cell with the cold cathode fabricated by the closest prior art method from the same materials.
  • the AMG alloy had a typical partially recrystallized structure of a hot-pressed intermediate product. Coarse inclusions of primary phases were present in the matrix. Chemical analysis revealed that the composition of light-color particles corresponds to an Al 10 Mg 2 Mn phase, while the composition of dark particles corresponds to a Mg 2 Si phase.
  • the matrix structure became fragmented in construction and was comprised substantially of fragment elements with the average size of ⁇ 100 nm.
  • Nonuniform contrast in the fragment body was an evidence of the presence of severe distortions in the crystal lattice and of high internal stresses, while the absence of diffused contrast was an evidence of dislocational nature of boundaries and their unformed state.
  • Annealing at a temperature of 75°C for about 1 hour did not result in appreciable modifications of the AMG6 alloy fragmented structure.
  • the fragmented structure transformed into a predominantly grained structure comprising ⁇ 60% of grains.
  • the process was accompanied by a slight coarsening of grains (up to ⁇ 130 nm).
  • a further temperature increase to 250°C activated the normal grain growth that has formed an equilibrium and equiaxial structure with the average grain size of ⁇ 540 nm.
  • a further increase of the annealing temperature was accompanied by a substantial coarsening of the grains.
  • the grain size increased to 2 ⁇ m after annealing at 300°C. Therefore, in the present experiment conditions, the temperature of low-temperature annealing in accordance with the invention for AMG6 alloy was found to be from 75°C to 250°C.
  • the obtained data also allowed a microhardness of the sample to be determined in various structural states.
  • the microhardness was evaluated in accordance with the Russian State Standard GOST 9450-76.
  • Fig. 15 shows the relationship between microhardness and annealing temperature and, consequently, grain size for AMG6 alloy. According to the obtained relationship, a microhardness of the cold cathode sample subjected to SPD and low-temperature annealing is 2.5 times higher than that of the sample in coarse-grained state. This results in 2.5 times higher strength of the cathode and, as has been already mentioned for some alloys, extends its service life. Moreover, the microhardness of the sample after SPD and low-temperature annealing is insignificantly lower than that after SPD only due to a partial removal of work hardening (cold work).

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EP07873394A 2007-12-28 2007-12-28 Kaltkathode und verfahren zu ihrer herstellung Withdrawn EP2226828A1 (de)

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CN111519147A (zh) * 2020-03-18 2020-08-11 赣州有色冶金研究所 一种择优取向的钽靶材及其制备方法以及一种扭转装置

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Publication number Priority date Publication date Assignee Title
CN111519147A (zh) * 2020-03-18 2020-08-11 赣州有色冶金研究所 一种择优取向的钽靶材及其制备方法以及一种扭转装置
CN111519147B (zh) * 2020-03-18 2022-03-11 赣州有色冶金研究所有限公司 一种择优取向的钽靶材及其制备方法

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