CN1142250A - Non-vaporising vacuum air-getter and method of obtaining the same - Google Patents
Non-vaporising vacuum air-getter and method of obtaining the same Download PDFInfo
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- CN1142250A CN1142250A CN95191862.1A CN95191862A CN1142250A CN 1142250 A CN1142250 A CN 1142250A CN 95191862 A CN95191862 A CN 95191862A CN 1142250 A CN1142250 A CN 1142250A
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- getter
- blank
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J7/00—Details not provided for in the preceding groups and common to two or more basic types of discharge tubes or lamps
- H01J7/14—Means for obtaining or maintaining the desired pressure within the vessel
- H01J7/18—Means for absorbing or adsorbing gas, e.g. by gettering
- H01J7/183—Composition or manufacture of getters
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Powder Metallurgy (AREA)
- Compressors, Vaccum Pumps And Other Relevant Systems (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Gas Separation By Absorption (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The proposed non-vaporising getter contains the following components: vanadium (V) - 20-35 wt.%; calcium (Ca) - 0.1-0.5 wt.%; and titanium (Ti) - the rest. The getter has a porosity of 25-65 % of its total volume. In order to obtain the getter in question, a method is proposed whereby a metal powder containing vanadium (V), calcium (Ca) and titanium (Ti) in the proportions indicated above is fed into a deformation zone at a bulk density of about 0.7-1.5 g/cm<3>. In the deformation zone, the powder is shaped by rolling, producing a getter blank in the form of a ribbon. The latter is cut into uniform sections which are then fed into a heating zone, where a pressure below 1 pa is established and maintained and the blank sections are heated to a temperature below 0.6 of the fusion temperature of the titanium-vanadium alloy and subsequently allowed to set. A getter is obtained with a porosity of 25-65 % of its total volume.
Description
The present invention relates to vacuum technique, relate in particular to getter of non-vaporising and preparation method thereof.
The present invention can be used as at electronic vacuum element-as cathode tube, optical converter, and gyrostat etc., at ultimate particle source and accelerator, as the thermonuclear apparatus of TOKAMAK T-15 type, middle generation is also kept the absorbent pump of high vacuum.
The present invention preferably is used in reduction and produces vacuum in the device of the heat transfer of constant temperature media from environment, this device comprises for example vacuum flask, the liquified gas storage bucket, pipeline-this pipeline of using from oil well transport gas and crude oil is heat-insulating, so that make the freezing conveying that does not influence material in the pipeline of environment.
The present invention also can be used for the purifying of rare gas element.
At present,, the stability of p type in the p-n junction and n type conduction has been set up strict restriction, and this conduction can be present in obnoxious flavour impurity in the semiconductor processes district (as CO in the high development of technical fields such as semiconductor production and application
2, CO, O
2, H
2O, N
2Deng).
By utilizing absorbent pump based on the getter of non-vaporising, above-mentioned detrimental impurity can be pumped from treatment zone, the adsorption rate of getter is depended in the reduction of detrimental impurity concentration level in the above-mentioned treatment zone.Therefore, the getter of developing high adsorption rate just seems extremely important.The someone attempts producing the getter (USSR inventors certificate No.1715496) of high rate of adsorption.This known getter divides three layers, one deck supporting layer, and it is by being selected from for example Fe, and the plastic material of Ni or its alloy is made, and other two layers of surface getter all is respectively to be made by zirconio material, and it contains for example aluminium of 16% weight, the zirconium of surplus; Or the vanadium of 30% (weight), the titanium of 20% (weight), the zirconium of surplus.
Preparation comprises following operation based on the method for the getter of zirconium:
-will form supporting layer and be selected from for example Fe, the powdered material of Ni or its alloy, and form
The aluminium that comprises 16% (weight) (Al) of getter layer and the zirconium (Zr) of surplus, or the zirconium based powdered material of the zirconium (Zr) of the titanium (Ti) of the vanadium of 30% (weight) (V), 20% (weight) and surplus infeeds in the distorted area simultaneously, makes zirconio material be fed to the both sides of the material that forms supporting layer.In described distorted area, above-mentioned powdered material is being shaped by rolling, and the result has made three layers of zonal getter blank.After above-mentioned getter blank left the distorted area, it was cut into standard film, for example 200mm.The standard film of above-mentioned getter blank is placed into the heating zone of keeping vacuum, is heated to 950-1000 ℃, and this blank has been sintered and has made and had the product that improves mechanical property as a result, and the tensile strength that is about to getter material is by for example 6.3kg/mm
2Be increased to 6.8kg/mm
2, and increased adsorption rate, for example at getter in 900 ℃ down after the activation, when the amounts of hydrogen of absorption is 1.3m
3During Pa/kg, the adsorption rate under the room temperature reaches 1.9 meters
3/ rice
2Second.
Although tensile strength increases to some extent, but the getter layer of known getter material shows low physical strength, because the getter layer is by making based on the material of Zr-Al or Zr-V-Ti alloy, a large amount of intermetallic compounds is arranged in this material, therefore having increased its hardness and fragility.When this getter uses under alternate load, they will lose efficacy, and be because cracked and cause mostly.In addition, the aluminum base alloy that contains 16% (weight) aluminium has increased the consumption of the energy, because activate the temperature (about 900 ℃) that this class getter is had relatively high expectations.
In addition, known getter is for such as H
2, O
2, CO
2, CO, N
2Loading capacity Deng gas is low, because by Fe, the getter that Ni or its alloy are made is a neutral to gas adsorption, also because the porosity of getter layer is low, has only about 20%.There are many difficulties in the method for the getter of above-mentioned preparation non-vaporising in operation, also be difficult to because will reach best fit between supporting layer thickness and getter layer thickness, the high loss meeting that is exactly powdered material in addition causes the getter cost to rise.
Known in addition a kind of getter (RF patent No. No.1750256) with the non-vaporising that improves physical strength and improved adsorption rate.This known getter contains the vanadium (V) of 20-35% (weight), the calcium of 0.1-0.5% (weight) and the titanium of surplus.
When this getter uses under alternate load, show the physical strength of increase, this is because vanadium material of solid solution in titanium has high-ductility.The element calcium that exists in the getter material helps the raising of gettering rate, because calcium to oxygen the chemically reactive of height is arranged, to form calcium oxide (CuO), and calcium oxide particle is dispersed between the metallic particles, plays the effect of antiwelding agent, thereby has improved the porosity of getter.
Above-mentioned getter is made by following method.
To contain 20-35% (weight) vanadium, the calcium of 0.1-0.5% (weight), surplus is that the metal-powder of titanium infeeds in the distorted area, wherein above-mentioned powdered material is by the zonal getter blank of rolling formation.After this blank band leaves the distorted area, be cut into standard film, this sheet is sent to the heating zone again.
In above-mentioned heating zone, produce and keep the pressure that is lower than 1Pa, then with blank heating to being lower than 0.6 times of vanadium-titanium alloy fusing point, for example to 850 ℃, insulation then.The getter of making like this is that porosity is 22% plate, when hydrogen adsorptive capacity is 1.3m
3During Pa/kg, its adsorption rate at room temperature is 1.8 meters
3/ rice
2Second.This getter is 300-350 ℃ of activation.
The getter of above-mentioned composition can be described as the getter of low activation temperature, and this feature makes absorbent pump as long as lower energy consumption.But because adsorption rate is lower, the application of this getter is restricted, and for example, is used as a level in the stage pump device that it can not use in semiconductor production.
The getter that the purpose of this invention is to provide a kind of non-vaporising is when hydrogen adsorptive capacity is 1.3m
3During Pa/kg, its hydrogen adsorption speed at room temperature is for being higher than 2 meters
3/ rice
2Second, this is the reason that big surface in contact is arranged because of it and gas to be pumped.
Purpose of the present invention realizes that by a kind of getter of non-vaporising it contains the vanadium of 20-35% (weight), the calcium of 0.1-0.5% (weight), and the titanium of surplus, its porosity is 25-65% (volume).
Above-mentioned getter has a large amount of open pores on its surface.The result makes it and gas to be pumped that big surface in contact be arranged, thereby has increased gas adsorption speed, and promptly working as hydrogen adsorptive capacity is 1.3m
3During Pa/kg, its hydrogen adsorption speed at room temperature is greater than 2 meters
3/ rice
2Second.Porosity less than the hydrogen adsorption speed of 25% getter less than 2 meters
3/ rice
2Second, this has limited its range of application.Porosity can not be used as less than 25% getter, a level in the stage pump that for example uses in semiconductor production.
Porosity is higher than 65% getter and has lower physical strength, and when using under alternate load, this will cause it cracked and lost efficacy.This getter can not be used for for example night vision equipment, gyrostat etc.
Therefore,, cause its open porosity also high, thereby make it after 300-350 ℃ of activation, have higher adsorption rate (1.5-3 doubly) because the overall porosity of getter of the present invention is higher.
Another object of the present invention provides a kind of method of making the getter of above-mentioned non-vaporising, comprises using having dendritic particulate powder stock comes to form 25-65% in this material porosity.
This target is that the preparation method by the getter material of non-vaporising described below realizes, this method comprises: the vanadium that will contain 20-35% (weight), the calcium of 0.1-0.5% (weight), surplus is that the metal-powder of titanium infeeds the distorted area, wherein above-mentioned powder is by the zonal getter blank of rolling formation, this blank band is after leaving the distorted area, be cut into standard film, this sheet is sent to a heating zone again, in this heating zone, produce and keep the pressure that is lower than 1Pa, this blank is heated to 0.6 times the temperature that is lower than titanium-vanadium alloy fusing point, insulation again, having made porosity is the getter of 22-65% (volume), the about 0.7-1.5g/cm of the tap density of metal-powder of the present invention
3
The tap density of metal-powder has determined hole quantity and the size in the shaping blank.Know all that generally tap density numerical value is less, then the finished product porosity is big more, and vice versa.
Experiment shows, when the vanadium that contains 20-35% (weight), and the calcium of 0.1-0.5% (weight), surplus is that the tap density of metal-powder of titanium is near 0.7g/cm
3The time, the porosity of the getter that obtains is about 65%, and is about 1.5g/cm when the tap density of above-mentioned powder
3The time, the porosity that obtains getter is about 25%.
Infeed when being less than 70% (weight) particle grain size less than 50 μ m in the metal-powder of distorted area, the tap density of metal-powder is about 1.5g/cm like this
3When being less than 20% (weight) particle grain size less than 50 μ m in the above-mentioned metal-powder, the tap density of above-mentioned powder will be about 0.7g/cm
3
Preferably, the getter blank should be heated between about 950 ℃ of about 750-.This temperature range is determined by admissible maximum collapse amount, and the physical strength of gained getter and porosity thereof (25-65%) can be kept whereby.Be heated in the heating zone when above-mentioned blank under the situation of 750 ℃ of less thaies, then, a little less than the combination, cause the getter physical strength lower between particle because the diffusive migration of atoms metal is lower.When above-mentioned blank heating when being higher than 950 ℃, very big contraction takes place, cause the porosity of getter to reduce, thereby reduced adsorption rate.
When the porosity of getter blank was lower than 45%, the standard film of above-mentioned blank may curl.
Known banded blank physical strength is low, and when porosity increased, its physical strength descended.Experiment shows, when the porosity of getter blank takes place to curl greater than 45% the time, causes blank to lose efficacy.
By the example of following particular, will be more clear to other purpose of the present invention and advantage.
Non-vaporising getter according to the present invention contains the vanadium of 20-35% (weight), the calcium of 0.1-0.5% (weight), and surplus is a titanium, its porosity is about 25-65% (volume).
Getter of the present invention is 1.3m at hydrogen adsorptive capacity
3During Pa/kg, the hydrogen adsorption speed under room temperature is greater than 2 meters
3/ rice
2Second, this getter is activated under 300-350 ℃.
This character allows this getter to be used for ultimate particle source and accelerator, and the absorbent pump that uses in the thermonuclear apparatus of high pump rate is provided in restriceted envelope such as need.
For preparation has the getter of above-mentioned character, the invention provides a kind of method, it comprises following operation:
To contain 20-35% (weight) vanadium, 0.1-0.5% (weight) calcium, surplus is a titanium, tap density is at about 0.7-1.5g/cm
3Metal-powder infeed the distorted area, the following particle grain size of 70% (weight) imposes the power that surpasses above-mentioned metal-powder ultimate compression strength, for example 1 ton/centimetre less than 50 μ m to this distorted area in the described metal-powder
2, make metallic particles generation plastic deformation.
Then, it is even that metal-powder rolling is formed density, and porosity is greater than the banded blank of the finished product porosity.The length of blank band has little thickness much larger than its width, and its intensity is enough to guarantee it is sent in the heating zone.Rolling result is that to make width be 15-80mm, and thickness is the blank band of for example 0.4-0.8mm.Above-mentioned metal-powder experience continuous molding in rolling, the volume of powder is because the particulate density of arranging increases and reduces in this powder, and is certain although weight still keeps.
After the blank band leaves the distorted area, be cut into standard film, length for example is 200, the sheet of 70mm etc. is sent in the heating zone.Make this heating zone generation and keep the pressure that is lower than 1Pa, wherein the chemically reactive gas dividing potential drop (except the hydrogen) in this heating zone should be lower than 1 * 10
-2Pa, and make the getter blank heating to the temperature that is lower than 0.6 times of titanium-vanadium alloy fusing point, insulation then.Keep Heating temperature in 750-950 ℃ of scope.This temperature range is by the physical strength of keeping the gained getter, and promptly tensile strength is 1-6kg/mm
2Decide with the maximum collapse amount that porosity allowed of required 25-65%.
A variation instance of particular of the present invention, if the porosity of getter is lower than 45%, then the standard film of this getter blank can curl.Known banded blank can show low physical strength, and when porosity increased, physical strength reduced.Experiment shows when porosity is curled greater than 45% blank generation, causes this blank to lose efficacy.Embodiment 1
The vanadium that will contain 28.45% (weight), the calcium of 0.31% (weight), the titanium of 71.24% (weight), tap density γ=1.17g/cm
3Metal-powder infeed in the distorted area, the particle grain size of 57% (weight) ratio (q) is less than 50 μ m in the described metal-powder.Using the roller of diameter as 100mm in the distorted area, is under the 1.5m/min in roll speed (V), the form metal powder.It is 0.5mm that the result has made thickness (h), and width is the uniform banded getter blank of the density of 30mm, and its porosity is greater than the porosity of the finished product.Above-mentioned metal-powder is continuous molding when rolling.Leave after the above-mentioned distorted area, described banded getter blank is cut into the standard film of length 200mm, then, above-mentioned blank sheet is sent in the heating zone, in the heating zone, produce and keep the pressure of 0.025Pa,, and be incubated 1 hour again with the temperature (T) of blank heating to 850 ℃.After the cooling, take out blank.The finished product porosity (P) is 43%, and tensile strength is 2.1kg/cm
2
When hydrogen adsorptive capacity (Q) is 1.3m
3During Pa/kg, the getter that the present invention makes is in 350 ℃ of (T
AkT) activation is after 15 minutes down, the hydrogen adsorption speed (S) in the time of 20 ℃ is 4.0 meters
3/ rice
2Second.Embodiment 2
The vanadium that will contain 27.20% (weight), the calcium of 0.21% (weight), the titanium of 72.61% (weight), tap density γ=0.98g/cm
3Metal-powder infeed in the distorted area, the particle grain size of 48% (weight) ratio (q) is less than 50 μ m in the described metal-powder.In the distorted area, use with embodiment 1 in identical roller be rolled the form metal powder.It is 0.5mm that the result has made thickness (h), and width is the uniform banded getter blank of the density of 30mm, and its porosity is greater than the porosity of the finished product.Leave after the above-mentioned distorted area, above-mentioned banded getter blank is cut into standard film, and the standard film that porosity (P) is lower than 45% above-mentioned getter blank takes place to curl and becomes the volume of internal diameter 80mm, and the length of above-mentioned standard film is 2.96m.Then the getter blank that curls is sent in the heating zone, generation and keep the pressure of the 0.025Pa heating zone in blank heating to 850 ℃, is incubated 1 hour again.After the cooling, take out curling blank, the gained getter has big adsorption surface, and it is also bigger than the surface of embodiment 1 getter.The porosity (P) of curling getter is 38.5%, when after activating 15 minutes under 350 ℃, when hydrogen adsorptive capacity (Q) is 1.3m
3During Pa/kg, its adsorption rate to hydrogen under 20 ℃ is 3.3 meters
3/ rice
2Second.
After using the metal-powder of different stacking densities and applying different sintering temperatures, the gained that experimentizes the results are shown in the table.
Table
| Numbering | Constituent content (weight %) | ????γ ??(g/cm 3) | ?q (％) | ?T (℃) | ?p (％) | ?h ?mm | S (rice 3/ rice 2Second), 20 ℃, Q=1.3m 3Pa/kg ，T akT=350 ℃, 15 minutes | ||
| ???V | ??Ca | ?Ti | |||||||
| ?1 ?2 ?3 ?4 ?5 | ?28.45 ?27.20 ?27.20 ?27.20 ?32.2 | ?0.31 ?0.21 ?0.21 ?0.21 ?0.18 | Surplus-" "--" "- | ????1.17 ????0.98 ????1.46 ????0.8 ????0.77 | ?57 ?48 ?68 ?26 ?18 | ?850 ?850 ?780 ?900 ?860 | ?43 ?38.5 ?32 ?52 ?54 | ?0.5 ?0.5 ?0.65 ?0.71 ?0.68 | ????4.0 ????3.3 ????2.9 ????5.2 ????7.3 |
Wherein γ is the tap density of metal-powder
Q is that particle diameter is less than 50 μ m proportion of particles
T is a Heating temperature
P is the getter porosity
H is a getter thickness
S is a hydrogen adsorption speed
T is an adsorption temp
Q is a hydrogen adsorptive capacity
TakT is the getter activation temperature
When porosity according to the present invention is 30% getter, be the first step that the sheet of 180 * 30 * 0.8mm is formed the multi stage magnetic pump with 40 chip sizes, it is 0.3-2m to the adsorption rate of hydrogen
3/ s, this pump is contained in the accelerator that is used for semiconductor production.
Claims (5)
1. contain 20-35% (weight) vanadium, 0.1-0.5% (weight) calcium, surplus is the getter of the non-vaporising of titanium, the porosity that it is characterized in that described getter is 25-65% (volume).
2. method for preparing the getter of non-vaporising comprises following operation:
The vanadium that will contain 20-35% (weight), the calcium of 0.1-0.5% (weight), surplus is that the metal-powder of titanium infeeds in the distorted area, wherein above-mentioned metal-powder is shaped by rolling, the result makes zonal getter blank, after leaving above-mentioned distorted area, described blank band is cut into standard film, and further be sent to a heating zone, in this heating zone, produce and keep the pressure that is lower than 1Pa, and with above-mentioned getter blank heating to the temperature that is lower than 0.6 times of titanium-vanadium alloy fusing point, then insulation, the result has made the getter of porosity at 25-65% (volume), it is characterized in that, infeed that the tap density of above-mentioned metal-powder is about 0.7-1.5g/cm in the distorted area
3
3. according to the method for claim 2, it is characterized in that infeeding be lower than 70% (weight) ratio in the metal-powder in the above-mentioned distorted area particle grain size less than 50 μ m.
4. according to the method for claim 2 or 3, it is characterized in that described getter blank heating arrives about 750-950 ℃ temperature.
5. according to each method among the claim 2-4, it is characterized in that the porosity of described getter blank is lower than 45%, described standard film takes place to curl.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| RU9494045576A RU2073737C1 (en) | 1994-12-29 | 1994-12-29 | Nondusting tape gas absorber and method of manufacture thereof |
| RU94045576 | 1994-12-29 | ||
| US08/868,232 US5814241A (en) | 1994-12-29 | 1997-06-03 | Non-vaporizing getter and method of obtaining the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1142250A true CN1142250A (en) | 1997-02-05 |
| CN1068907C CN1068907C (en) | 2001-07-25 |
Family
ID=26653809
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN95191862A Expired - Lifetime CN1068907C (en) | 1994-12-29 | 1995-12-21 | Non-vaporising vacuum air-getter and method of obtaining the same |
Country Status (5)
| Country | Link |
|---|---|
| EP (1) | EP0765012B1 (en) |
| JP (1) | JP3231780B2 (en) |
| CN (1) | CN1068907C (en) |
| RU (1) | RU2073737C1 (en) |
| WO (1) | WO1996021958A2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101678458B (en) * | 2007-04-04 | 2012-12-12 | 联邦科学和工业研究组织 | Titanium flat product production |
| CN104745864A (en) * | 2013-12-26 | 2015-07-01 | 北京有色金属研究总院 | A preparing process of a titanium-based getter |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| IT1297013B1 (en) | 1997-12-23 | 1999-08-03 | Getters Spa | GETTER SYSTEM FOR THE PURIFICATION OF THE WORKING ATMOSPHERE IN PHYSICAL STEAM DEPOSITION PROCESSES |
| JP4889947B2 (en) * | 2005-01-14 | 2012-03-07 | パナソニック株式会社 | Gas adsorption alloy |
| RU2620234C2 (en) * | 2015-10-12 | 2017-05-23 | Акционерное общество "Научно-производственное предприятие "Исток" имени А.И. Шокина" (АО "НПП "Исток" им. Шокина") | Method for producing non-evaporable getter |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS51132108A (en) * | 1975-05-13 | 1976-11-17 | Matsushita Electric Ind Co Ltd | Alloy for hydrogen storage |
| US4079523A (en) * | 1976-11-08 | 1978-03-21 | The International Nickel Company, Inc. | Iron-titanium-mischmetal alloys for hydrogen storage |
| DE3031471C2 (en) * | 1980-08-21 | 1985-11-21 | Daimler-Benz Ag, 7000 Stuttgart | Alloy for storing hydrogen |
| SU1120867A1 (en) * | 1983-01-28 | 1986-09-07 | Предприятие П/Я Г-4601 | Cathode-ray tube |
| DE3425055C1 (en) * | 1984-07-07 | 1985-07-25 | Daimler-Benz Ag, 7000 Stuttgart | Getter substance |
| SU1715496A1 (en) * | 1989-02-06 | 1992-02-28 | Центральный научно-исследовательский институт черной металлургии им.И.П.Бардина | Method of manufacturing triple-layer band of non-atomized gas adsorbent |
-
1994
- 1994-12-29 RU RU9494045576A patent/RU2073737C1/en not_active IP Right Cessation
-
1995
- 1995-12-21 CN CN95191862A patent/CN1068907C/en not_active Expired - Lifetime
- 1995-12-21 JP JP52158696A patent/JP3231780B2/en not_active Expired - Fee Related
- 1995-12-21 WO PCT/RU1995/000276 patent/WO1996021958A2/en active IP Right Grant
- 1995-12-21 EP EP95942805A patent/EP0765012B1/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101678458B (en) * | 2007-04-04 | 2012-12-12 | 联邦科学和工业研究组织 | Titanium flat product production |
| CN104745864A (en) * | 2013-12-26 | 2015-07-01 | 北京有色金属研究总院 | A preparing process of a titanium-based getter |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1068907C (en) | 2001-07-25 |
| EP0765012A2 (en) | 1997-03-26 |
| WO1996021958A2 (en) | 1996-07-18 |
| EP0765012B1 (en) | 1999-07-07 |
| WO1996021958A3 (en) | 1996-09-06 |
| RU94045576A (en) | 1996-10-27 |
| JP3231780B2 (en) | 2001-11-26 |
| JPH09509986A (en) | 1997-10-07 |
| EP0765012A4 (en) | 1997-02-20 |
| RU2073737C1 (en) | 1997-02-20 |
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