KR100239823B1 - A combination of materials for integrated getter and mercury-dispensing devices, devices thus obtained, and a process for the introduction of mercury inside electron - Google Patents

Abstract

The mercury injection mixture according to the invention comprises mercury and a mercury injection intermetallic compound (A) containing a second metal selected from a mixture thereof, such as titanium, zirconium and preferably Ti ₃ Hg, and a facilitating alloy or Intermetallic Compound (B) It is composed of copper, tin, and an accelerated alloy (B) or an intermetallic compound (A) containing at least one metal selected from rare earths, in particular a mixed metal (MM). A method of injecting mercury into an electron tube, a method of injecting mercury into an open tube of one of the mercury injection apparatuses, and then sealing the open tube within 600 seconds to 900 degrees Celsius within 10 seconds to 1 minute. It describes a method of heating the mercury injection device to obtain free crystals of mercury at a temperature in the range, and also a mercury injection device comprising the mixture, in particular further comprising a getter material (C).

Description

Mercury distribution mixture with getter material and how to inject it into an electron tube

1 is a perspective view of one embodiment of a mercury injection device according to the present invention.

2 and 2a are a plan view and another sectional view taken along the line II-II of FIG. 2, respectively, of another embodiment of the mercury injection device according to the present invention.

3, 3a and 3b respectively show a plan view of another embodiment of a mercury injection device according to the invention and a cross sectional view of two possible configurations according to line III-III of FIG.

Figure 4 is a ternary diagram showing an alloy according to the present invention.

* Explanation of symbols for main parts of the drawings

10 tablet (tablet) 20 ring-shaped device

21 metal support 31 strip

The present invention relates to a mixture of a mercury injection material used in admixture with a getter material and a method of injecting mercury into an electron tube.

For example, the use of small amounts of mercury in electron tubes such as mercury arc rectifiers, lasers, various types of alphanumeric display devices, and in particular fluorescent lamps, is well known in the art.

The precise injection of mercury into these devices is very important for the quality of these devices, especially for ecological reasons. In fact, the high toxicity of mercury causes serious environmental pollution if these devices containing these materials are at the end of their lifetime or if these devices are accidentally destroyed. This natural ecological problem leads to the use of as little mercury as possible to the extent appropriate for the use of electron tubes. This was eventually taken into account in the area of legislation, and the scope of international regulations has recently set a maximum limit on the amount of mercury that can be injected into these devices. For example, for a standard fluorescent lamp, the total amount of mercury used is less than 10 mg per fluorescent lamp. Has been presented.

Mercury can be injected into the electron tube in the form of a liquid. However, first of all, the use of liquid mercury has problems related to storage and handling in plants for producing electron tubes, since mercury has a high vapor pressure at room temperature. Next, a common drawback of the technique of injecting liquid mercury into the interior of an electron tube is the difficulty in injecting a small amount of mercury, approximately 1 microliter, accurately and reproducibly. Is taken more than the required dose.

Due to these drawbacks, technological advances have been made in various alternatives to the use of free forms of liquid mercury.

Techniques for using liquid mercury contained in capsules are known in some conventional literature. Such methods are disclosed, for example, in US Pat. Nos. 4,823,047 using metal capsules, 4,754,183, and US Pat. Nos. 4,182,971 and 4,278,908 using mercury storage containers made of glass. After the tube is closed, mercury is released by a heat treatment method that damages the vessel. This method typically has some drawbacks. The first of these is the complexity of the manufacture of such capsules and the fixing of the capsules in the interior of the tube, which is especially complicated when the capsule is injected into the interior of a small sized tube. Secondly, breakage of capsules, especially when the capsules are made of glass, can cause fragments of material that can degrade the quality of the tube. US Pat. No. 4,335,326 discloses that mercury-containing capsules are shields against such fragments. Disclosed is an assembly that is configured to be positioned in turn within the capsule to act as a. In addition, the release of mercury is often intense enough to damage the internal structure of the tube. Finally, such a structure still has the drawbacks of the liquid mercury used, and thus cannot completely solve the problem of injecting mercury accurately and reproducibly up to several milligrams.

U.S. Patent 4,808,136 and European Patent Application 568,317 disclose the use of tablets or spheres made of a mercury-soaked porous material, after which the fluorescent lamp is closed. Mercury is released. However, this method also requires complicated manipulations when putting mercury into such tablets, so the amount of mercury released is difficult to regenerate.

For example, the use of amalgams of mercury containing indium, bismuth or zinc is well known. However, such amalgams have a drawback that the melting temperature is low, and there is also a problem that the vapor pressure of mercury is high even when the temperature is not so high. For example, the zinc amalgam published in the advertisement of "APL Engineering Materials Incorporated (APL)" has a vapor pressure that corresponds to about 90% of the vapor pressure of liquid mercury at 43 ° C. Therefore, these amalgams must withstand the heat treatment for the manufacture of fluorescent lamps to which they are injected.

These problems are overcome by U.S. Patent No. 3,657,589 filed by the inventor of the present invention, which uses an intermetallic compound of mercury having the general formula Ti _x Zr _y Hgz, where x and y are each 0 to 13 Variable between, sum (x + y) varies between 3 and 13, and z is 1 or 2.

These compounds have a varying onset temperature of mercury release, depending on the specific compound, but are stable up to about 500 ° C. both in the air and in vacuum, thus allowing the assembly of the electron tube assembly to reach a temperature of about 500 ° C. It is suitable for operation. After closing the electron tube, mercury is released from the mixture by activation, which typically occurs by heating mercury between 750 ° C and 900 ° C for about 30 seconds. Such heating can be achieved by causing heating of the metallic support of the compound for laser radiation or mercury injection. Particular preference is given to using Ti3Hg compounds manufactured and marketed under the trade name "St505" by the present application, in particular the St505 compound being a "stegsolve" contained within a ring-shaped container. (STAHGSORB Commercially available in the form of a powder compressed under the trade name) or in the form of a compressed powder contained in a pill or tablet; (GEMEDIS Commercially available in the form of a powder laminated on a strip of metal under the trade name "

These materials offer several advantages over the prior art:

(1) As mentioned above, the materials avoid defects of mercury vapor during the production cycle of the tube, which can reach temperatures of about 350 ° C to 400 ° C,

(2) As mentioned in U. S. Patent No. 3,657, 589, the getter material is a mercury liquor aimed at the chemical action of gases such as CO, Co ₂ , O ₂ , H ₂ and H ₂ O that interfere with the action of the tube. Can be easily added to the mouth mixture, the getter material is activated during isothermal heat treatment for mercury release, and

(3) Provides advantages that the amount of mercury released can be easily controlled and reproduced.

Although the materials are quite convenient to use with desirable chemical-physical properties, these materials have the drawback that the stored mercury is not released completely during the activation process. In fact, methods for producing mercury storage electrode tubes can be achieved by using two free-form glass elements, for example by using a closed tube or low melt glass, which is sealed by glass fusion, such as the sealing of fluorescent lamps. Frit sealing to weld. During this operation, the mercury injector may experience an indirect temperature rise to a temperature of about 600 ° C. At this stage, the device discharges the gases and vapors released by the molten glass to the atmosphere in almost all industrial processes. In this case, the mercury injection material undergoes surface oxidation and the final result is less than about 40% of the total mercury content during the activation process. In the special case of a small circular fluorescent lamp, an indirect temperature rise to about 500 ° C. occurs during the sealing of the circular fluorescent lamp and the bending of the mercury injection material. In this case, the yield of mercury during the activation process is about 20% or less of the total mercury content of the device.

Mercury not released during the activation is slowly released during the lifetime of the electron tube.

Along with the fact that the electron tube must operate from the beginning of its life cycle, this feature leads to the need to inject into the mercury injection device an amount of mercury at least twice the theoretical requirement.

In order to overcome this problem, patent application EP-A-091.297 proposes to add nickel (Ni) or copper (Cu) powder to Ti ₃ Hg or Zr ₃ Hg compounds. According to this patent, the addition of nickel and copper to the mercury injection compound allows the dissolution of the mixture obtained as described above to allow release of almost all mercury in seconds. In this patent, the dissolution is Ni-Ti, having a temperature range of about 880 ° C. for a composition of 34% Cu 66% -Ti to 1280 ° C. for a composition of 19% Ni 81% -Ti, in an atomic ratio. Although it is described as occurring at the process temperatures of Ni-Zr, Cu-Ti, and Cu-Zr systems, the wrong dissolution temperature of 770 ° C is suggested for a composition of 96% Ni 4% -Ti. The patent changes that the mercury infusion compound is made during the treatment process, which requires protection. For this purpose, it is proposed to close the mixture vessel with steel, copper or nickel thin plates which break down during activation by mercury vapor pressure generated inside the vessel. This solution is not completely satisfactory, in fact, mercury can explode violently and cause damage to the outlet of the tube, as is the case with capsules, and the container requires welding of small metal members. The manufacture of is very complicated. In addition, this patent does not present experimental data to demonstrate the desirable mercury release properties for the proposed mixture. As a result, in contrast to those disclosed in US Patent Application No. 3,657,589, which is cited in this patent, the getter material necessary for the desired operation of the fluorescent lamp is not mixed in the same apparatus.

It is therefore an object of the present invention to provide an improved mixture for injecting mercury into an electron tube so that at least one of the problems of the prior art can be overcome.

In particular, it is an object of the present invention to provide an improved mixture for mercury injection which can release at least 60% of mercury during the activation step so that the amount of mercury used even after partial oxidation has occurred.

Another object of the present invention is to provide a mixture having the activity of the getter even after the act of activating to release mercury.

Another object of the present invention is to provide a mercury injection device comprising a mixture.

It is a further object of the present invention to provide a method of injecting mercury using the device according to the invention into an electrode tube which requires the above components.

According to the invention, the above and other objects have the general formula Ti _x Zr _y Hg _z , where x and y are each given between 0 and 13, and the sum (x + y) is given between 3 and 13. And z is given as 1 or 2) mercury injected intermetallic compound (A) and the following points in a ternary diagram based on the weight percent composition: a) Cu63% -Sn36.5% -MM0.5%, b A) formed by Cu63% -Sn10% -MM27%, c) Cu30% -Sn10% -MM60%, d) Cu3% -Sn37% -MM60%, and e) Cu3% -Sn96.5% -MM0.5% It is achieved by a mercury injection mixture having a composition that fits within a polygon, which is composed of a promoter alloy or intermetallic compound (B) comprising at least one metal selected from copper, tin, and rare earths.

Further objects and advantages of the present invention will become apparent from the following detailed description with reference to the accompanying drawings.

Component (A) of the mixture according to the invention is an intermetallic compound, which is identical to the molecular formula Ti _x Zr _y Hg _z , as described in U.S. Patent No. 3,657,589, referenced for further explanation. Of the materials consistent with the molecular formula Zr ₃ Hg, Ti ₃ Hg is particularly preferred.

The promoting alloy (B) of the mixture according to the invention will be defined as a promoter after having a suitable release of mercury from component (A). This component is an intermetallic compound comprising a metal alloy or copper, tin and a metal selected from rare earths and rare earth mixtures. Because these metals have similar chemistries, the use of a mixture of rare earth metals is preferred because the single element is difficult to separate and expensive to operate, and on the other hand, in the present patent application, even if a rare earth mixture is used, The same results can be achieved as with cows. The rare earth mixture is known in the art as "misch metal" and the abbreviated name of this mixed metal is MM and will be dealt with in the remainder of the description and in the claims.

The weight ratio of copper, tin, and MM varies within a wide range, but the preferred result is a) Cu63% -Sn36.5% -MM0.5% b) Cu63% -Sn10 in the ternary diagram based on the weight ratio % -MM27% c) Cu30% -Sn10% -MM60% d) Cu3% -Sn37% -MM60% e) Cu3% -Sn96.5% -MM0.5%.

Alloys containing 63% or more of copper require a high melting temperature and very high temperatures at the same time that the alloy is activated, whereas alloys containing less than about 3% of copper have a very low melting point. There is a drawback of having a low viscosity liquid phase at various temperatures of about 600 ° C. to 800 ° C. reached during the production of the fluorescent lamps. Alloys containing more than 60% by weight of mixed metals by weight may react excessively and cause vigorous reactions during both the manufacturing and activation steps of the fluorescent lamp. As a result, alloys containing tin in the percent by weight up to 10% again reach a high melting point.

Particularly preferred characteristics are a) Cu63% -Sn36.5% -MM0.5% b) Cu63% -Sn10% -MM27% f) Cu50% -Sn10% -MM40% g) Cu30 in the ternary diagram based on the weight composition ratio % -Sn30% -MM40% h) Cu 30% -Sn69.5% -MM0.5% occurs within the composition range as described above in the polygon formed.

Particularly preferred alloys have a composition ratio Cu40% -Sn30% -MM30% consistent with point i) in the configuration of the ternary diagram of FIG.

The weight ratio between the intermetallic material (A) and the promoting alloy (B) according to the present invention is in a very wide range, but is usually in the range of 20: 1 to 1:20, preferably 10: 1 to 1: 5. Is in the range of.

The intermetallic compound (A) and the promoting alloy (B) according to the present invention can be used in various physical forms which are not identical for these two components. For example, the promotion alloy (B) can be found in the intermetallic compound (A) in powder form close to the promotion alloy (B) by the coated form and flow of the metal support. However, the most preferred results are obtained when the two components A and B are in the form of suitable powders which are smaller than 250 μm and preferably have partial dimensions in the range of 10 μm to 125 μm.

In a second embodiment, the present invention relates to a mercury injection device using a mixture of the intermetallic compound (A) and the promotion alloy (B).

As mentioned above, one of the advantages of the inventive mixtures related to the prior art construction is that it does not require the protection of the machine from the above environmental conditions. Therefore, the mercury injection device of the present invention can be manufactured in most other shapes of geometric shapes, and the mixtures (A and B) can usually be used on or without a metallic support. Some zones of the electron tube for mercury injection devices tend to require the presence of getter material to remove gases of the kind such as CO ₂ , CO ₂ , H ₂ , O ₂ , or water vapor for the desired operation of the device. . That is, this is for example in the case of fluorescent lamps. An important advantage provided by the mixtures of the present invention is that evaporation of mercury leaves a reaction residue with getter activity. The amount of gas that can be absorbed by the residue and the rate of absorption are sufficient to ensure adequate vacuum for many patent applications. In order to increase the overall gas absorption rate and capacity of the device, it is first possible to add another getter material (C) according to the method described in the above-mentioned US patent application Ser. No. 3,657,589. Clearly, the amount of getter material (C) in this patent application is lower than that required in the prior art apparatus used in the same patent application. Among other materials, the getter material is, for example, materials such as titanium, zirconium, tantalum, niobium, vanadium, and mixtures thereof, or nickel , Alloys with other materials, such as iron and aluminum, and patented, manufactured and sold under the names St101 or the intermetallic compounds Zr ₂ Fe and Zr ₂ Ni, and filed under the names St198 and St199, respectively. Such as alloys having a composition of Zr84% -Al16% based on weight percent. The getter material is activated during the heat treatment by mercury being released inside the tube.

The getter material (C) may be present in a variety of physical shapes, but is preferably used in the form of fine powder having a fragment size of less than 250 μm and preferably between 10 μm and 125 μm.

The ratio between the mixture of the intermetallic compound (A) and the promoting alloy (B) and the total weight of the getter material (C) is usually in the range of about 10: 1 to 1:10, preferably 5: 1 to 1 It is in the range of: 2.

Some possible embodiments of the device according to the invention are shown in the following referenced figures.

In the first embodiment, the apparatus of the present invention usually has a cylindrical or equilateral hexagonal shape for simplicity of production, and is a mixture (or getter material (C) of the intermetallic compound (A) and the promotion alloy (B)). The possibility of having a tablet 10 in the form of compressed and unsupported powder of)) can be simply constructed and the parallel hexagonal shape is shown in FIG.

In the case of supported materials, the mercury injection device may take the form of a ring 20 shown in FIG. 2 showing a plan view of the device and in FIG. 2 a showing a cross section according to line II-II of the device 20. . In this case, the apparatus consists of a support 21 having the shape of an annular channel comprising a mixture (or getter material (C)) of the intermetallic compound (A) and the promotion alloy (B). This support is usually a metal material, preferably an alloy of nickel-steel sheet.

Instead, the device may be made in the form of a strip 30 shown in FIG. 3 showing a plan view of the device and in FIGS. 3 a and 3b drawn along III-III of the device 30. In this case, the support 31 is preferably made of a strip and is preferably attached by the cold compression of the mixture of intermetallic compound (A) and the promotion alloy (B) (or getter material (C)) in operation. Is made of an alloy of nickel-steel sheet. In this case, whenever a getter material (C) is needed, the mixture of the intermetallic compound (A) and the promotion alloy (B) and the getter material (C) are on one side of the strip shown in FIG. 3A. Or simultaneously mixed on both sides, or a mixture of the intermetallic compound (A) and the promoting alloy (B) flows on one side of the strip, and the getter material (C) is shown in FIG. On the opposite side.

In a further aspect, the present invention relates to a method for injecting mercury into an electron tube by the device described above. That is, the present invention relates to a promoted alloy comprising a mercury-containing intermetallic compound (A) comprising a second metal selected from mercury and titanium, zirconium and mixtures thereof, and at least one metal selected from copper, tin and rare earth metals or An intermetallic compound (B) and also a getter material (C), wherein the material (A, B) is contained in a metal support having an annular channel shape and a mixture of the materials (A, B) is stripped. Introducing into an open tube of one of the devices rolled on the surface of the shaped support, and between 600 ° C. and 900 ° C. for a time between 10 seconds and 1 minute after sealing the tube to obtain free crystals of mercury. Consists of heating the device to temperature. The method comprises injecting the mercury injection mixture, preferably inside the electrode tube in the device 10, 20 or 30, and then heating the mixture to obtain a free form of mercury. The heating step takes place with any suitable means such as, for example, by discharging, by high frequency contact heating, or by causing the high frequency contact heating to flow through the support when made of a material having high electrode resistance. May be The heating method is effective at a temperature for releasing mercury from the mercury injection mixture contained in the range of 600 ° C to 900 ° C for about 10 seconds to 1 minute. At temperatures below 600 ° C., most of the mercury is not injected into all regions, and at temperatures above 900 ° C., there is a risk of diffusion of toxic gases due to emissions from some of the electron tubes adjacent to the device, or from some of the composition of the metal vapor.

The invention is further illustrated by the following examples. These non-limiting embodiments are intended to educate a method for practicing the present invention, and show some embodiments showing the completeness of the present invention, which is considered to be the most desirable. Examples 1 to 3 relate to the preparation of mercury injecting materials and accelerators, whereas Examples 4 to 9 relate to tests for mercury release after heat treatment, which virtually experiment with gas tightness. There is. All metals used in the preparation of alloys and compounds for the following tests have a purity of at least 99.5%. Examples 10 to 14 relate to a test for the functionality of the residual getter material remaining after the release of mercury. All ratios in the configurations of this example are based on weight percentages unless otherwise specified.

[First Embodiment]

The first embodiment shows the composition of the mercury injection material Ti ₃ Hg.

143.7 g of titanium is placed in the steel pedestal and degassed by superheating at a temperature of about 700 ° C. and a pressure of 10 ⁻⁶ mbar per 30 minutes. After cooling the titanium powder in an inert atmosphere, 200.6 g of mercury is injected into the pedestal by a quartz tube. The pedestal is heated at about 750 ° C. for 3 hours and then closed. After cooling, the extract is pulverized until a powder is produced that passes through a standard body having a body size of 120 μm.

The extract consists essentially of Ti ₃ Hg as confirmed by a diffractometric test in powder form.

Second Embodiment

The second embodiment relates to the preparation of a promotion alloy (B) which forms part of the mixture of the present invention.

40 g of copper, 30 g of tin, and MM 30 g in powder form are placed in an aluminum pedestal and then injected into a vacuum induction furnace. The misch metal used is composed of about 50% cerium by weight, 30% lanthanum, 15% neodymium, and the other rare earths.

The mixture is heated at a temperature of about 900 ° C., maintained for 5 minutes at a temperature of 900 ° C. to recover homogeneity, and finally poured into a ingot mold. Each ingot is pulverized in a blade mill and the powder is sieved as in the first embodiment. The composition of the alloy produced is copper 40% -tin 30% -MM30%, consistent with point i) in the diagram of FIG.

Third Embodiment

The third embodiment relates to the preparation of an accelerating alloy which forms part of the mixture of the present invention. The progress of the second embodiment is repeated using 60 g of copper, 30 g of tin, and MM 10 g in powder form. The composition of the alloy produced is 60% copper-30% -MM10% copper, consistent with point i) in the diagram of FIG.

Fourth to Ninth Embodiment

Examples 4 through 9 illustrate mercury release after heat treatment in air which simulates the conditions of the glass material mixture which is encountered during the device closing the tube (hereinafter, generally referred to as airtight). It has to do with testing. The fourth to seventh embodiments are prepared by injecting a single element (fourth embodiment), and are provided with only copper, tin and only the above-mentioned getter alloy st101 (5 to 7 embodiments) and mixed. Comparative examples show the release of mercury after the hermetic action of the glass stock mixture, respectively, by the same material. Similar comparisons for mixtures of Ti ₃ Hg and MM powders are unlikely to cause hypersensitivity to this mixture.

For virtual hermetic action, a mixture of 150 mg of each powder has been accumulated in a ring-like container as in FIG. 1 or on a strip as in FIG. 3 and proceeded in the air according to the next thermal cycle. come.

(1) heating from room temperature to 450 ° C. in about 5 seconds,

(2) maintaining isothermal at 450 ° C. for 60 seconds;

(3) cooling to 450 ° C. to 350 ° C. for about 2 seconds;

(4) maintaining isothermal at 350 ° C. for 30 seconds;

(5) naturally cooling to room temperature for about 2 seconds;

From there, the mercury spinning test is thus conducted by inducing heating at 850 ° C. for 30 seconds on the inner surface of the vacuum chamber and by measuring the mercury remaining in the mercury injection device through titration of the mixture by experiment in the "Volhart". Progress has been made on the treated samples.

The results of the mercury release test are summarized in Table 1, and Table 1 shows the mercury injection compound (A) and the promoted alloy (B) (depending on the composition of the copper-tin-MM alloy as shown in the diagram of FIG. Symbol (i) or (l)) in the eighth and ninth embodiments, the intermetallic compound (A), the promoting alloy (B), and the mercury released on the total capacity of the mercury injection device. The weight ratio of the mercury generation amount as a ratio is shown.

Comparative examples are marked with an asterisk.

TABLE 1

10th-14th Example

Examples 10-14 relate to tests for functionality as residual getter material remaining after mercury release by the inventive mixtures and by some comparative mixtures.

These tests have been generated by the virtual conditions of the glass stock mixture induced during the bending and hermetic action of small circular fluorescent lamps, the virtual conditions being more difficult than those for linear fluorescent lamps. In particular, the mixture of this example has been run according to the following thermal cycles in air.

(1) heating to room temperature to 600 ° C. in about 10 seconds,

(2) forming an isothermal curve at 600 ° C. for 15 seconds,

(3) cooling to room temperature naturally for about 2 minutes.

A mercury release test (activation) has been conducted after a virtual experiment of the hermetic action of the glass stock mixture on the sample. The sample of glass material mixture is injected into a vacuum chamber having a volume of 1 liter, heated under vacuum at 850 ° C. for 10 seconds, and maintained at 850 ° C. for 20 seconds.

The amount of residual getter material that acts as a getter material is measured after the activation step. The measurement is made by injecting an amount of hydrogen into the chamber resulting in a pressure of 0.1 mbar at a temperature of 30 ° C. and by measuring the time required to reduce the pressure in the chamber to 0.01 mbar. The measurement of pressure is taken by volume manometer. The results of these tests are summarized in Table 2, which shows the composition of the sample and the hydrogen absorption rate at 30 ° C. The column "Sample Composition" shows the weight percentage of the constituent materials. Comparative blends are marked with an asterisk.

TABLE 2

It can be seen from the data in Table 1 that the mixtures with the inventive facilitator generate at least 80% mercury during the activation step after the hermetic action of the glass material mixture in air at 450 ° C.

In addition, as shown by the data in Table 2, the residual material remaining after mercury release is getter activity. Indeed, the residual material remaining after mercury release by a single compound of Ti ₃ Hg is not gettered and the sample of Example 13 in which no getter material is added exhibits a clear mercury absorption rate. In addition, the sample 12 has a hydrogen absorption rate comparable to that of the sample of the eleventh embodiment, and the sample of the eleventh embodiment is a mixture of a mercury injection device with a getter material, and has been widely used by a fluorescent lamp manufacturing apparatus.

When the getter material is added to the mixture of the twelfth embodiment, the hydrogen absorption rate is almost doubled to that of the eleventh embodiment having the same proportion of getter material. This stateful nature of the mixtures according to the invention allows the use of very small amounts of added getter material or no added getter material, while achieving the functionality of the apparatus employed.

The inventive mixtures with accelerators provide another important advantage of being able to generate activation even at low temperatures or in a short time compared to those implemented with prior art materials. In fact, in order to have an industrially suitable activation time, a single compound of Ti ₃ Hg requires an activation temperature of about 900 ° C., which can reduce the operating time and the size of the production line of the fluorescent lamp, in both cases Two advantages are degassing for all materials of the present invention to prevent contamination inside the tube and reduce the amount of energy required by the present invention.

Claims (2)

In a mercury injection mixture, the general formula Ti _x Zr _y Hg _z (where x and y are each given between 0 and 13, the sum (x + y) is given between 3 and 13, and z is 1 Or 2) mercury injected intermetallic compound (A) and the following points in a three-dimensional diagram based on the weight percent composition: a) Cu63% -Sn36.5% -MM0.5%, b) Cu63% -Sn10% -MM27%, c) Cu30% -Sn10% -MM60%, d) Cu3% -Sn37% -MM60%, and e) Cu3% -Sn96.5% -MM0.5% Mercury injection mixture, characterized in that consisting of a promoted alloy or an intermetallic compound (B) comprising at least one metal selected from copper, tin, and rare earths. In the method of injecting mercury into the electrode tube, (1) a mercury-injected intermetallic compound (A) comprising mercury and a second metal selected from titanium, zirconium and mixtures thereof, and an accelerated alloy or intermetallic compound comprising at least one metal selected from copper, tin and rare earth metals; And (B) and a getter material (C), wherein the material (A, B) is contained in a metal support having an annular channel shape, and the mixture of the materials (A, B) is strip-shaped. Introducing into an open tube of one of the devices that is rolled on the surface of the support; (2) a method of mercury injection comprising heating the device to a temperature between 600 ° C. and 900 ° C. for a time between 10 seconds and 1 minute after sealing the tube to obtain free crystals of mercury.