JP3359050B2 - Manufacturing method of strip getter - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a getter used for adsorbing a gas in a vacuum vessel, and more particularly to a method for releasing a gas from a substrate with excellent adhesion strength between the substrate and the getter material. We propose a strip getter molded into an easy-to-handle form that exhibits excellent gas adsorption capacity without any problems.

[0002]

2. Description of the Related Art Getters are used by attaching them directly or indirectly to a vacuum vessel such as a vacuum tube or a thermos in order to evacuate the inside thereof. For example,
A getter formed in the shape of a strip is fixed to the inside of a thermos by spot welding and used, or a cylindrical getter material is mounted on the discharge electrode in the lamp and used, or a getter formed in the shape of a tablet is mounted An example of mounting and using inside a thermos via a container is
This is a typical usage.

[0003] Such getters are classified into two types: getters such as barium type getters, which are referred to as "evaporation type", and Zr, Ti type getters, which are referred to as "non-evaporation type". It is used properly according to. Recently, non-evaporable getters that are easy to handle, have excellent adsorption capacity, and do not contaminate the inside of a vacuum vessel are being used.

[0004] As a method of manufacturing the non-evaporable getter, a metal powder or alloy powder of pure Ti, Zr-Ni, Zr-Fe, Zr-V, Ti-W or the like is pressed into a strip or a cylinder. Then, a method of firing if necessary is known.

[0005] As a typical prior art for obtaining a strip getter, a surface of a base material such as iron or stainless steel is plated, and a getter material of a metal powder or an alloy powder is pressed on both sides of the base material. (See U.S. Pat. No. 249,772).

Furthermore, facilities as a method for obtaining an excellent strip getter adhesion strength without performing pretreatment of the plating process and the like for the purpose, a pre-hole opens only treated steel plate such as iron or stainless steel to improve adhesion There is also a technique of using a punched plate as a base material and connecting getter materials pressed to both surfaces of the base material through the holes.

[0007]

However, the strip getters manufactured by the conventional methods as described above use a plate material such as iron or stainless steel as a base material. When performing or heating for activation, there is a problem that the getter material is separated from the substrate due to impact or heat history.

When a getter using such a plate material as a base material is used in an extremely high vacuum region of 10 ^-8 Torr or more, the gas released from the base material lowers the exhaust efficiency, and particularly, H ₂ , When CH ₄ , CO gas, etc. were released, the degree of vacuum was significantly reduced.

Further, in the above-described strip getter, it is necessary to press-bond the getter material while leaving welding margins for performing spot welding or the like at both ends of the base material, and press-bond and fire in such a state. In addition, the difference in the shrinkage ratio between the base material and the getter material caused distortion in the longitudinal direction, which caused defects such as warpage and peeling.

[0010] An object of the present invention is to overcome the above-mentioned problems of the prior art, and in particular, to achieve excellent gas adsorption without releasing gas from the substrate and having excellent adhesion strength between the substrate and the getter material. An object of the present invention is to provide a method capable of stably producing a strip getter exhibiting its ability.

[0011]

As a result of intensive studies for realizing the above-mentioned object, the present inventors have found that the above-mentioned problems are caused by the base material itself. Therefore, as a result of various studies on this base material, the use of a foil material instead of a plate material as a base material has alloyed the getter material and the foil material, thereby advantageously solving the problems of the prior art. The inventors have found that the present invention can be solved, and arrived at the present invention.

That is, the present invention, Ni, comprising any one or more metals or alloys of Cu and Al 10
Zr, V, Fe, on at least one surface of the ~ 50 μm thick foil
A getter material made of a metal powder or an alloy powder made of at least one of Ni, Nb, Ti, Mn and Al is used.
Of part is crimped so as to break through the foil, then,
By firing under vacuum, the foil material and getter material are fused.
Ru manufacturing method der strip getter, characterized in that alloying is engaged.

More specifically, from the upper part of the pair of pressure-bonding rolls, a central part of the gap between the rolls is made of a metal or alloy of at least one of Ni, Cu and Al.
While feeding the m-thick foil continuously, Zr, V, Fe, Ni, Nb, Ti, Mn and metal powder comprising at least one of Al in the gap between the feeding foil and each roll or A getter material consisting of an alloy powder is continuously supplied, and the
Some of the getter material and pressed under pressure to break through the foil and laminate,-out continuously pulling downwardly as a strip-shaped to fit the laminate to the rotation of the rolls, the
After that, by sintering under vacuum, foil material and getter material
It is preferable to use a method for producing a split getter, which is characterized by fusing and alloying .

[0014]

The feature of the present invention is that, instead of a conventionally used plate material such as iron or stainless steel as a base material of a strip getter, a foil made of one or more metals or alloys of Ni, Cu and Al is used. The point is to use.

By the way, in order to eliminate the adverse effects caused by the use of the substrate, a getter that does not use the substrate can be considered. With such a getter, a high vacuum can be maintained without releasing gas, and no defects such as peeling and warping due to the base material are observed. However, in the method without using the base material, since the getter material alone is pressure-formed by a roll or the like, there is a disadvantage that the getter material is cracked or broken during the pressure molding, and there is a new problem to be solved. It will be.

In this regard, according to the present invention, since a foil material is used as a base material instead of a plate material and a getter material is pressed on at least one side of these foils, cracks and breaks during molding can be prevented. In addition, it can also eliminate inconveniences such as warpage and peeling at the time of press bonding, firing and processing.
A getter having excellent gas adsorption ability can be provided.

That is, when a foil material is used as a base material and a getter material is pressed and formed on at least one side of the foil by a roll or the like, as shown in FIG. Effectively improves the adhesion between the foil material and the getter material. Moreover, a molded article can be obtained without cracking or breaking.

Further, when the molded body is fired,
As shown in the figure, since the foil material and the getter material are in an alloyed state, warping does not occur in the getter due to cooling after firing, and bending and cutting of the obtained strip getter are performed. However, the getter material does not peel off from the substrate. In addition, since the foil material itself hardly exists, there is no problem that the gas adsorption ability is deteriorated due to the generation of gas from the base material when the getter is used.

Here, the reason why the material of the foil material is limited to Ni, Cu and Al is that the getter material is press-bonded to a foil made of one or more metals or alloys of Ni, Cu and Al, and then subjected to vacuum. When sintering is performed, these foil materials can be fused with the getter material and alloyed. Therefore, compared with the conventional plate materials such as iron and stainless steel, the adhesion strength between the base material and the getter material is larger, and the foil material itself has getter performance, so-called high gas adsorption capability, It is possible to manufacture a strip getter exhibiting excellent gas adsorption ability without generating gas from the substrate.

The reason why the thickness of the foil is limited to the range of 10 μm to 50 μm is that if the thickness is less than 10 μm, the getter material is uniformly pressed over the entire surface of the foil, particularly when the getter material is pressed by a roll or the like. On the other hand, if it exceeds 50 μm, the foil is not broken by the getter material particles and remains as it is as a metal layer or an alloy layer, and like the base material using the conventional plate material, it causes warpage, cracking and breaking, In addition, this is because the adsorption capacity is also deteriorated due to gas release.

After the getter material is pressed against the foil by a roll or the like and molded, the firing is performed under a vacuum of 10 ^-3 Torr or less.
It is desirable to carry out at a temperature of about 900 to 1200 ° C.

[0022]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS An embodiment of the method of the present invention using the manufacturing apparatus shown in FIG. 1 will be specifically described below. Here, reference numerals 1 and 2 in the figure denote a pressing roll for pressing the getter powder material to the foil 7, and reference numerals 3 and 4 denote the getter powder material and the foil 7 uniformly in the axial direction of the pressing rolls 1 and 2. Is a raw material supply table provided with a vibrator or the like, for example, for supplying a uniform amount of getter powder material into the raw material nozzles 3, 4, and 6 is a raw material cutting device. It is. . First, the Al foil 7 is fed from above into the center of the roll gap between the pressure-bonding rolls 1 and 2 at a rotation speed of 10 rpm, and at the same time, Zr-Al (84 wt% -16 wt%) powder was transferred to the raw material hopper 3 in the gap between the both sides of the Al foil 7 and the rolls 1 and 2 kiss portions.
The mixture was fed at a speed of g / min and compression-molded with a roll to obtain a strip-shaped laminated molded article having a cross-sectional structure as shown in FIG. The pressure applied to the pressure rolls 1 and 2 at this time was maintained at 5 to 6 tons. . Next, the strip-shaped laminated molded body thus obtained was placed in a vacuum sintering furnace, and sintered at a temperature of 1150 ° C. for 1 hour under a vacuum of a pressure of 10 ⁻⁶ Torr or less. Later, Ar
When the inside of the furnace was cooled to room temperature with gas and taken out into the atmosphere, a strip getter having a cross-sectional structure as shown in FIG. 3 was obtained.

With respect to the strip getter thus obtained, this getter was placed in a 1-liter vacuum vessel, and the vacuum getter was performed to check the gas exhaust efficiency. As a result, when the pressure was reduced to 1 Torr, the material was heated and activated at 800 ° C., and further evacuated to 10 ^-8 Torr, and the required time was 16 minutes. For comparison, Zr−
Using a commercially available strip getter (ST101) in which an Al alloy was pressure-bonded to a FeNi substrate, vacuum exhaustion was performed under the same conditions as described above, and it took 20 minutes. From this, it was found that the strip getter manufactured by the method of the present invention did not release gas from the substrate and was excellent in both gas adsorption amount and gas adsorption speed.

Further, using the same strip getter sample as described above, a bending strength test was conducted in which the operation of bending to R25 was repeated 50 times. As a result, the strip getter manufactured by the method of the present invention did not have any breaks or cracks and did not peel off the getter material, whereas the commercial strip getter showed that a part of the getter material peeled off. Was done.

As described above, according to the present invention, the adhesive strength between the substrate and the getter material is excellent, and the gas is removed from the substrate without causing defects such as peeling and warping caused by the substrate. It is possible to stably manufacture a strip getter exhibiting excellent gas adsorption ability without releasing.

[Brief description of the drawings]

FIG. 1 is a diagram showing a manufacturing apparatus suitably used in the method of the present invention.

FIG. 2 is a diagram showing a cross-sectional structure after a getter material is pressure-formed on a foil.

FIG. 3 is a diagram showing a cross-sectional structure of a strip getter obtained by the method of the present invention.

[Explanation of symbols]

 1, 2 Crimping roll 3, 4 Material nozzle 5 Material supply table 6 Material cutting device 7 Al foil

──────────────────────────────────────────────────続 き Continuing on the front page (72) Inventor Nobuo Ito Okinokuchi, Oguni-machi, Nishiokitama-gun, Oguni-machi, Yamagata Pref. -17784 (JP, B1) U.S. Pat. No. 4,977,035 (US, A) (58) Fields investigated (Int. Cl. ⁷ , DB name) H01J 9/39

Claims (2)

(57) [Claims] The present invention relates to a Zr, V, Fe, Ni, Nb, Ti, Mn, and Al film on at least one surface of a foil having a thickness of 10 to 50 μm made of one or more metals or alloys of Ni, Cu, and Al. A getter material made of a metal powder or an alloy powder consisting of any one or more of the above, a part of the getter material is pressure-bonded so as to break the foil, and then the foil material and the getter material are baked under vacuum. A method for producing a strip getter, wherein the strip getter is fused and alloyed. 2. A foil having a thickness of 10 to 50 μm made of one or more metals or alloys of one of Ni, Cu and Al is continuously fed from a top of a pair of pressure rolls to a central portion of a gap between the rolls. In the gap between this feeding foil and each roll
Zr, rodents comprising V, Fe, Ni, Nb, Ti, a metal powder or alloy powder consisting of any one or more of Mn and Al
The getter material is continuously supplied, and the roll
Part is a laminate and pressed under pressure to break through the foil,-out continuously pulling downwardly as a strip-shaped to fit the laminate to the rotation of the roll, then baked under vacuum
By combining foil material and getter material by forming
A method for producing a split getter.