JPS58192239A - Non-volatile getter and manufacture thereof - Google Patents

Abstract

PURPOSE:To obtain getter having various gas adsorption modes by means of a simple change of manufacturing conditions by making an intermetal compound showing a getter action due to activation to be ribbon-shaped by means of molten metal quick chilling. CONSTITUTION:A zirconium alloy block containing 24.3wt% of nickel is put into a container 12 made of quartz glass to be molten by high frequency induction heating from outside and said molten metal is supplied on the surface of a rotating steel cooling roll 16 from a nozzle 14 provided with an opening part of 1mm.X8mm. prepared on the bottom of the container 12 made of quartz glass thus to obtain a thin ribbon 17 having the thickness of 20-100mum in the nearly tangential direction to the cooling roll surface, whereon said molten metal falls. Further, the whole equipment is required to be maintained in an argon atmosphere during the period from alloy melting to ribbon making in order to prevent it from being oxidated.

Description

DETAILED DESCRIPTION OF THE INVENTION (Technical Field of the Invention) The present invention relates to a non-vaporizable getter used in electron tubes and lighting tubes 114, and a method for manufacturing the same.

(Technical Background of the Invention and Melting Point) A non-vaporizable getter is used to remove undesirable gas in the tube and prolong its life in electron tubes and blind tubes.

As materials for non-vaporizable getters, there are many pure metals such as zirconium and titanium, and so-@ inter-compounds that are treated as zirconium, are solid crystals, and have a strong getter action, etc. ing. However, these getter materials mainly composed of intermetallic compounds are not molded to 4 kA, but are crushed into powdered form, and this first ice is made into iron #i grade wires, and the iron plate itself is molded. There is. As a result, assembling the earthen plug is messy and takes a long time, leading to an increase in the getter price. Also, in order to fit into the small space inside the electron tube, the bent getter is in use. The cause of the increase is the appearance of the wood, or the excessive leakage of the tube, a decrease in rigid pressure characteristics, and an increase in noise.

In such a situation, Higashine, a getter that can be vaporized, has good getter performance, workability, and handleability, and does not cause any leakage or suppressive properties. 1k rare C
There is.

(Hita of the invention)) The present invention was made in view of the above-mentioned drawbacks, and an object of the present invention is to provide a non-vaporizable getter that has good getter performance, good workability and handling, and does not lower the pressure resistance by -1, and a process for manufacturing the same. purpose.

(Summary of the Invention) The non-vaporizable getter of the present invention is characterized in that it contains a gold-M intercompound that exhibits a getter action upon activation and is ribbon-shaped.

Further, the method for manufacturing a non-vaporizable getter of the present invention is characterized in that the getter is manufactured at the end of 'M1.

(Embodiments of the Invention) (Example 1) A zirconium alloy ingot containing 24.3% nickel was placed in a quartz glass bowl a-type bath, as shown in Fig. 141, with an inner diameter of 8 Iu, and heated from the outside by a zirconium alloy ingot containing 24.3% of nickel. By heating, the molten metal is transferred to the nozzle 0 (which is attached to the cuff of 1 m x 8 u provided at the bottom of the quartz glass container 04) and then to the rotating fII4 cooling roll uF.
By supplying the 5J table improvement, its rb m rl
＋ - I did it ~ The surface of the roll was a jealous line, and I was humiliated 2
A Zhaonai ribbon aT) of 0 to 100 μm was obtained. From the general understanding of alloys, during ribbon production, the entire apparatus was repeatedly air-plowed and filled with pure argon three times to prevent hydrogenation, and was strictly maintained in an argon atmosphere of 400 Torr. The malleable ribbon-like grinding assembly obtained in this manner is set at a gap between the magazine nozzle and the cooling roll of 0.211al to 0.7 magazine rotation, and the continuous rotation of the cooling roll is set at a circumferential speed of 5. The surface morphology shown in Table 1 was obtained by impregnation with four yokes from m/I to 2Q m/8.

Table 1 In addition, the table l1ltI was measured by Ls ET, and the transmittance of the -5-character X-rays (alpha rays) was measured, and the appearance of the curved ribbon was determined. Calculated assuming the fabric length is 100%. Caulk and melt these non-vaporizable getter 9bons onto the surface of a stainless steel cylinder with a diameter of Ion! #! After mounting, it was placed in a vacuum chamber that was completely evacuated, and was heated and partially activated using a one-frequency wave 4ζ2 from the outside. The temperature of this viscosity was measured using a thermocouple and was controlled at 800° C. for 30 seconds. After activation, carbon monoxide was poured into the vacuum container from the outside through a gaseous mold tube. Next, the non-vaporizable getter device was maintained at 350° C., and the pressure deterioration in the vacuum container over time was measured using a Virani Q needle and a 1111:Ill^ empty gauge. the result,
It was found that initially, the gas sorption ability was low in the order of e, B, and A, and after a long period of time, it was in the order of m, B, C, and D.

Based on this result, D is given to equipment with poor initial JL airflow but relatively little risk of gas generation over time, and D to equipment with good initial vacuum but with a risk of deterioration of vacuum due to gas generation over time. A is considered to be suitable for devices such as 42.

Also, regarding gas purification equipment, etc., please check whether it is breathable or not.
D is the most chewy fish because it is important that the H side is large. Furthermore, even in the case of A, when the ribbon width is made extremely small and it is made into a single strip, it has properties similar to those of D.

Next, we will briefly discuss examples of these samples and those sent to the X-ray tube.
the&! I will discuss this in the next issue.

A ribbon-shaped getter shrine made with νlj l in ★ and a zirconium ribbon for comparison were incorporated into an X-ray tube as shown in Figure 3. It is housed at the tip of the elm, and the house is fixed inside the glass envelope with the filament Kawa Hiroto #1, and electrically led to the outside. . A ribbon-shaped non-vaporizable getter material was also fixed around the bottom of the pole body by dispersion and vapor resistance contact.

The inside of the envelope □□□ was completely evacuated, baked in an electric furnace, and the components were finally degassed by high-ms induction heating.Finally, the getter part was heated at 800°C for 30 seconds. It is activated and sealed by me.

Using the X@ effect created in this way, '#! Voltage 120rVr rated 100V), tube 1t ft, 24
A forced life test was conducted. Both the getter material of the present invention and the comparative zirconium ribbon incorporated into the X-ray tube had a diameter of 1100 p@10 m. Pure zirconium is X! When producing liI tube sea bream, the surface was already covered with brownish oxidized doves, but in contrast to sample A, which has the composition of a gold-F14 compound called Zr1Aj, the surface was not oxidized and did not lose its metallic luster. Nothing happened. The results of the forced life test showed that the comparative zirconium ribbon tube used as the getter reached J! after about 500 hours. On the other hand, the tube used as the ribbon getter of the product of the present invention showed no abnormal discharge phenomenon even after 700 hours had passed, and was in good condition. A carp ＾
- It showed pressure characteristics. The difference between samples A, B, C, and D is
In this case, I didn't get much credit.

(Example 2) A porous fibrous getter ribbon having a diameter of 101111 and an apparent thickness of 100 μm was produced using a zirconium alloy ingot containing 16% aluminum by a method similar to that shown in Example 41S1. The diameter of one linear fiber is about 10 μm. In the case of this embodiment, it was applicable to high-torque strength radiation cauterization ()iID) which is resistant to electric painting. In this case, a comparison was made with a conventional case in which zirconium powder was applied to the electrode support in the discharge lamp for 4 hours in advance. As in the case of Example 1, the zirconium surface was saponified during the manufacturing process, whereas in the case of the present invention, a gold luster was maintained.

In this case as well, as a result of HID's forced pure life experience, it fully exerts its getter effect on the water threads that greatly affect the sac 4t1,
Until now, Kajohokai, which was caused by the omission of Getta Material Kyoshi, which had been thought to be Itsumugi, was not introduced at all. Zirconium has the disadvantage that it can ignite in the atmosphere at high temperatures, is extremely unstable, does not oxidize, is difficult to handle industrially, and is not suitable for commercial use. is stable at '1i4fkA', and XX &u゛tgMt'! ＞(DX
'46. t,iv*Round example u□iThe fact that it can be treated as a ribbon with wing expansibility is one of the great advantages as well as being a means of actually developing measures to improve pressure resistance properties.

(Deformation meeting) In addition, it corresponds to zirconium-nickel system with the composition of ZrNi, Zr, A/1, etc.
Zirconium-aluminum thread, HfNi, of composition.

By applying Hf, Ni, etc. (2) to hafnium-nickel systems with corresponding compositions, ribbon-shaped getter materials were created and used in tubes, respectively, and were able to improve the getter effect.

(Effect of the explanation) As mentioned above, the non-vaporizable getter of the present invention is a gold-114 compound and has a ribbon shape, and as a result, it is difficult to handle and is saponified during electron tube processing. It has excellent gettering ability.

It is also an excellent getter with good pressure resistance even when applied to tubes that require high voltage resistance such as X-rays and repeated on-off cycles.

In addition, according to the method for producing a non-volatile getter of the present invention, it is possible to form a book made of a gold-kI quaternary compound into a ribbon shape at an extremely high speed, which has not been possible in the past. Rotation speed, melt from nozzle
The surface condition can be reduced by 1#Sv by simple changes in the injection pressure, bath water temperature, distance between the nozzle and the cooling roll, and as a result, a getter with the desired gas yield mode can be obtained. Many effects can be added to the depths.

[Brief explanation of drawings]

! Figure 2 is a diagram explaining the manufacturing method of the non-vaporizable getter of the present invention, and Figure 3 is a diagram of the non-vaporizable getter of the present invention.
It is a schematic lllT1 diagram showing a state in which the wire tube is filled with carbon dioxide. 11.21...Zoku-12,22...Yaramic Valley Equipment
j, 2j...ll1lb Hermit drum-coil 14.24...
Nozzles 16, 26, 28, cooling rolls 17, 29, 36...Non-vaporizable getter 31...Target 33...-Polar structure agent Patent attorney Yu Chika (and 1 other person) Figure 1 Figure 3

Claims (1)

[Claims] ill A non-vaporizable getter characterized by producing a ribbon-shaped non-vaporizable getter which is mainly composed of a gold-intermetal compound that exhibits a viscosity (two-way getter action). E! Manufacturing method.